Temperature of synthesis (Ts), polymorphic transition (Ttr), decomposition (Td) and melting (Tm) of some apatite-structured compounds [65].
\\n\\n
Dr. Pletser’s experience includes 30 years of working with the European Space Agency as a Senior Physicist/Engineer and coordinating their parabolic flight campaigns, and he is the Guinness World Record holder for the most number of aircraft flown (12) in parabolas, personally logging more than 7,300 parabolas.
\\n\\nSeeing the 5,000th book published makes us at the same time proud, happy, humble, and grateful. This is a great opportunity to stop and celebrate what we have done so far, but is also an opportunity to engage even more, grow, and succeed. It wouldn't be possible to get here without the synergy of team members’ hard work and authors and editors who devote time and their expertise into Open Access book publishing with us.
\\n\\nOver these years, we have gone from pioneering the scientific Open Access book publishing field to being the world’s largest Open Access book publisher. Nonetheless, our vision has remained the same: to meet the challenges of making relevant knowledge available to the worldwide community under the Open Access model.
\\n\\nWe are excited about the present, and we look forward to sharing many more successes in the future.
\\n\\nThank you all for being part of the journey. 5,000 times thank you!
\\n\\nNow with 5,000 titles available Open Access, which one will you read next?
\\n\\nRead, share and download for free: https://www.intechopen.com/books
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Preparation of Space Experiments edited by international leading expert Dr. Vladimir Pletser, Director of Space Training Operations at Blue Abyss is the 5,000th Open Access book published by IntechOpen and our milestone publication!
\n\n"This book presents some of the current trends in space microgravity research. The eleven chapters introduce various facets of space research in physical sciences, human physiology and technology developed using the microgravity environment not only to improve our fundamental understanding in these domains but also to adapt this new knowledge for application on earth." says the editor. Listen what else Dr. Pletser has to say...
\n\n\n\nDr. Pletser’s experience includes 30 years of working with the European Space Agency as a Senior Physicist/Engineer and coordinating their parabolic flight campaigns, and he is the Guinness World Record holder for the most number of aircraft flown (12) in parabolas, personally logging more than 7,300 parabolas.
\n\nSeeing the 5,000th book published makes us at the same time proud, happy, humble, and grateful. This is a great opportunity to stop and celebrate what we have done so far, but is also an opportunity to engage even more, grow, and succeed. It wouldn't be possible to get here without the synergy of team members’ hard work and authors and editors who devote time and their expertise into Open Access book publishing with us.
\n\nOver these years, we have gone from pioneering the scientific Open Access book publishing field to being the world’s largest Open Access book publisher. Nonetheless, our vision has remained the same: to meet the challenges of making relevant knowledge available to the worldwide community under the Open Access model.
\n\nWe are excited about the present, and we look forward to sharing many more successes in the future.
\n\nThank you all for being part of the journey. 5,000 times thank you!
\n\nNow with 5,000 titles available Open Access, which one will you read next?
\n\nRead, share and download for free: https://www.intechopen.com/books
\n\n\n\n
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The first synthesis of apatite was performed by DAUBRÉE [1], who obtained it in crystals by passing the vapor of phosphorus trichloride (PCl3) over red-hot lime. The synthetic mineral analogues of chlorapatite, fluorapatite, or the mixtures of these phases were prepared by Manross [2] via fusing of sodium phosphate either with calcium chloride, calcium fluoride, or both together. The similar process was also successfully used by Briegleb [3]. Forchhammer [4] prepared chlorapatite by fusing calcium phosphate with sodium chloride. When bone ash or marl was used instead of artificial calcium phosphate, mixed apatite was formed. Similar results were reported by Deville and Caron [5], who fused bone ash with ammonium chloride and either calcium chloride or fluoride, and also by Ditte [6], who repeated Forchhammer’s experiment [7]. Zambonini and Ferrucio [8] found that the fusion of Ca3(PO4)2 with CaCl2 produced apatite with very weak birefringence. Fusing Ca3(PO4)2 with an excess of NaCl gave crystals with the birefringence of 0.0050–0.0058.
\nBy heating calcium phosphate with calcium chloride and water, under the pressure at 250°C, Debray prepared chlorapatite [9]. Weinshenk [10] also prepared chlorapatite by heating calcium chloride, ammonium phosphate and ammonium chloride at the temperature of 150 to 180°C in a sealed tube. The method is described in The separation techniques based on leaching of minerals from a solid by dissolving them in a liquid. Chlorine analog of spodiosite [14]. Calcium chlorspodiosite is colorless crystalline compound structurally related to the mineral wagnerite (Mg2(PO4)F). It was reported by Nacken in his study of the phase relationships which was obtained in the system CaCl2-CaO-P2O5 [12]. The synthesis of the compound by dissolving Ca3(PO4)2 in fused CaCl2 was reported by Klement and Gembruch [13]. Since the mineral was recognized as the mixture of fluorapatite, calcite and serpentine, it was discredited (IMA action 2003-03-B).
The history of synthesis of various apatite compounds and substitution in the apatite structure including the preparation of didymium bearing chlorapatite and chlorspodiosite is described in the work of Zambonini and Ferrucio [17]. The paper describes three of those apatite syntheses using the mixture of Ca3(PO4)2, DiPO4 Didymium (Di) was recognized as the mixture of element of neodymium and praseodymium [18].
Hendricks et al [19] reported the preparation of hydroxylapatite by the hydrolysis of tricalcium phosphate Tricalcium phosphate was prepared by slow addition of Na3PO4 solution to the solution with the excess of Ca(NO3)2. The precipitate was washed with saturated solution of Ca3(PO4)2 until the filtrate was free of nitrates. The salt was then dried at 50°C [19],[18]. Hydroxylapatite is very difficult to dehydrate, even at high temperature (
The phase equilibrium in carbonate-apatite–CaCO3 (a) and carbonate-apatite–CaCO3–Na2CO3 systems (b) [
\nEitel [20] investigated the binary systems Ca3(PO4)2–CaCO3 (Fig. 1(a)) and Ca3(PO4)2–CaCO3–Na2CO3 Introduced as double salt of Na2Ca(CO3)2. Prepared mixtures were heated under the pressure of CO2 in the range from 55 to 100 and from 23 to 54 kg·cm−2 (kg·cm−2 = 98066.5 Pa) for binary and ternary system, respectively [20].
The equilibrium given by the following scheme was predicted- for carbonate-apatite [20]:
\nThe prepared crystals are typically long or short lengths with hexagonal prism {10
The literature on the preparation of synthetic analogues of minerals from the supergroup of apatite In older literature termed as apatite-like substances.
Various alternative names, such as Shake ’n Bake Methods or Beat ’n Heat, are used for the solid state synthesis (reaction) in literature [23].
\nJaffe [18] recognized the precipitation by metathesis and the precipitation by hydrolysis.
Sometimes are included among high-pressure methods [24].
Other methods (
The pressure-temperature ranges of these methods are shown in Fig. 2. Some of the most applied techniques are described in this chapter. The methods for the preparation of single crystals are described separately in the next
Pressure-temperature range for the material preparation [
Solid-phase reactions (syntheses) are usually activated by high-temperature treatment [25]. The preparation of materials in solid-state is rather different form the synthesis of discrete molecules. The process involves the treatment of the whole lattice. Often, the post-synthesis purification of materials is not possible due to low solubility of formed phases. Hence, all effort must be made to avoid the excess of reagents. These methods are usually slow due to entire reaction which occurs in the solid state and requires the diffusion across the points of contact in a mixture [26],[27]. Special techniques can also be used based on the reduction of particle size or on the preparation of precursor in order to reduce the particle size, improve the product homogeneity and lower the temperature of thermal treatment [24].
\nReaction scheme for solid-state synthesis: (a) ceramic method [
The most applied techniques Solid-state synthesis is classified among physical methods (together with vapor phase synthesis, laser ablation, etc.) some of other techniques listed below (sol-gel process, precipitation method, etc.) are considered as chemical methods [28].
Since ceramic can be fabricated by a variety of methods, some of which have their origin in early civilizations, ceramic methods must be distinguished from the ceramic fabrication processes. The consolidation of ceramic powder to produce a
The nucleation of a new phase, the epitactic There is a structural similarity between the substrate and the nucleus that is limited to 2D interface and referred to as epitaxy [23]. There is a structural similarity between the substrate and the nucleus (like for epitaxy15)) that extends to 3D for topotaxy [23]. Phase transformation has usually significant effects on the reaction rate. The reaction rate is strongly increased at the temperatures near the phase transformation because the mobility of atoms is also increased. This phenomenon is termed as Sintering is defined as the bonding of adjacent surfaces in a mass of powder or a compact by heating [29]. In general there are three types of sintering process including Solid-Phase (Dry) Sintering (1), Liquid-Phase Sintering (2) and Reactive (Reaction) Sintering (3) [29]. The process can also be divided according to applied conditions and densification practice to Conventional Sintering (1), Microwave Sintering (2) and Pressure Sintering (3). The stages of the sintering process include: (1) initial stage (formation and growth of necks), (2) intermediate stage (pores reached their equilibrium shapes, continuous porosity), (3) final stage (pores reached their equilibrium shapes, isolated (enclosed) porosity) [30]. The process can also be divided according to the mass transport mechanism to viscous sintering and diffusion sintering (further divided according to dominant type of diffusion to surface diffusion, volume diffusion, intergranular diffusion, grain-boundary diffusion, but gas transport (diffusion) of matter can also occur). Generally, the term
Schematic diagram of hot pressing process [
The method is particularly important for the preparation of dense sample of ceramics with high degree of covalent bonding such as SiC and Si3N4.
\nNormal process of compaction of powder material involves uniaxial pressing in a die followed by sintering for densification. However better densification can be achieved by exerting a uniform pressure from all directions through a fluid medium onto the powder material retained in container (die), i.e. the pressure is generated by heating of medium. The process is termed as isostatic compaction, and as
In the case of Generally, the cavitation can be divided into four types on the basis of the mode of generation of cavitation conditions: (1) acoustic cavitation (sound waves of high frequency 16 kHz–1 MHz), (2) Hydrodynamic cavitation (pressure variation is obtained by changing the geometry of the system), (3) optic cavitation (passing of photons of high intensity) and (4) particle cavitation (produced by the bombardments of other types of elementary particles, e.g. protons) [28].
By The method for the detonation transformation of graphite into diamond was earlier developed at the Institute of Chemical Physics of the Academy of Sciences of the USSR [38].
Mechanochemical synthesis (reaction) of solids in the presence of water can be considered as hydrothermal one [25]. Mechanochemistry is a branch of chemistry which is concerned with chemical and physico-chemical changes of substances of all stages of aggregation due to the influence of mechanical energy (Ostwald [39]). Colloid mills can be classified into three main groups with regard to the mechanism utilized for production of dispersion: beater-type mills (1), the smooth-surface type (2) and the rough-surface type. Beater-type mills include the original Plauson machine and some modified mills [48]. Also intermetallic compounds, i.e. substances composed of two or more metallic elements with given stoichiometry and structure. Different atomic species occupy different lattice sites [44].
The first mechanochemical reactor Constructed by PARKER [
The advanced preparation techniques used for the reduction of particle size, activation of starting material or preparation of nano-scale Nano it the Greek word for dwarf. In the International System of Units (SI) it is the decimal multiple 10−9 used as prefix. Nanoscience refers to the range from one to several hundred manometers and the nanotechnologies are the technologies in which atoms are manipulated in quantities of one to several thousand atoms. Nanoscience probably first gained the attention in 1959 in the lecture of the American Nobel laureate of 1965 in physics R. Feynman, who stated:
Tetrametoxysilane, tetraetoxysilane, tetraethyl orthotitanate, etc. Methyltrimethoxysilane, vinyltrimethodxysilane, etc. This classification [30] does not set aside often used group of semi-alkoxide methods (using the mixture of soluble salt and metal alkoxide), Pechini type polymeric gel methods (liquid mix techniques) as well as modified Pechini methods. The Pechini process usually uses soluble nitrates, acetates, chlorides, carbonates, isopropoxides or other metal compounds which are dissolved in the solution of citric acid (in general in polycarboxylic acids) and ethylene glycol (in general glycol). The polycondensation reaction leads to the polymeric gel accommodating the stable chelates of metal cations [50]:
\n\n
\n\n
\n
Basic flow charts for sol-gel processes using a sol (a) and a solution of alkoxides (b). Schematic diagram of the structure of particulate gel formed from a sol (c) and polymeric gel from a solution (d) [
Starting with a sol, gelled material consists of identifiable colloidal particles which were joined together by the surface forces to form a network Fig. 6(c). When the solution of metal-alkoxides is used ( The first step is the hydrolysis, the equilibrium constant for higher degree of hydrolysis decreases depending on the nature of –OR (increasing length of hydrocarbon chain and its branching). The process is also affected by the temperature, the solvent composition and applied water to alkoxide ratio, the type of catalysis, the application of ultrasound energy, etc. [52]. Due to the formation of ROH molecule is termed as “alcohol producing condensation”, i.e. the reaction between alkoxy (nonhydrolyzed) and hydrolyzed groups. The reaction with two hydrolyzed groups leads to the formation of –M–O–M– bridge and water, i.e. is termed as “water producing condensation”.
Drying of gel leads to xerogel. The process is usually followed by shrinkage and formation of cracks. The thermal treatment of xerogel often involves the pyrolysis and calcination. If monolith is needed (aerogel [51]) the supercritical drying is usually applied.
The precipitation method is used for the preparation of precursor that is further treated by solid-state synthesis. The techniques of direct precipitation of apatite are described in
Therefore often associated with combustion techniques [56]. The process is analogous to the process of frontal polymerization in which localized polymerization reaction zone propagates thorough the mixture of solution of a monomer and initiator due to the heat diffusion and the occurrence of exothermic reaction [59].
Thermal cycle of spray pyrolysis [
The reaction schemes for the solid-state synthesis of apatite structured compounds were published by Knyazev et al [65]:
where
where
where
The temperature effect (Table 1) observed during the synthesis includes [65]:
synthesis;
polymorphic transition;
thermal decomposition; and
melting.
Compound | \n||||
---|---|---|---|---|
[K] | \n||||
Ca5(PO4)3OH | \n310 | \n992 | \n– | \n– | \n
1173 | \n– | \n1523 | \n– | \n|
Ca5(PO4)3Cl | \n1073 | \n953 | \n– | \n>1723 | \n
Ca5(VO4)3Cl | \n1073 | \n794 | \n– | \n>1723 | \n
Ca5(CrO4)3Cl | \n1123 | \n9007 | \n– | \n1616 | \n
Sr5(PO4)3Br | \n1473 | \n– | \n1661 | \n– | \n
Sr5(VO4)3Cl | \n1023 | \n– | \n– | \n>1723 | \n
Sr5(CrO4)3F | \n1373 | \n– | \n– | \n1705 | \n
Ba5(VO4)3Cl | \n1073 | \n– | \n– | \n>1723 | \n
Ba5(MnO4)3F | \n1123 | \n– | \n1163 | \n– | \n
Pb5(PO4)3I | \n973 | \n– | \n– | \n256 | \n
Pb5(VO4)3F | \n923 | \n– | \n1044 | \n– | \n
Temperature of synthesis (Ts), polymorphic transition (Ttr), decomposition (Td) and melting (Tm) of some apatite-structured compounds [65].
The temperatures of these effects for some apatites are listed in Table 1.
\nThe phase transformation and the thermal expansion coefficient of apatite-structured compound with the composition given by the formula
and the monoclinic phases are less anisotropic but have larger thermal expansion coefficients in comparison with the hexagonal phases.
\nThe precipitation method is based on the combination reaction(s) when cations and anions in the solution combine to form insoluble ionic solid, so-called precipitate. The method can be divided to [35]:
Wet techniques of apatite preparation are based on the precipitation from solution at ambient temperature [67]. The preparation techniques based on aqueous precipitation at moderate temperatures often lead to non-stoichiometric apatites [68]. Hydroxylapatite close to the ideal formula, can be precipitated by the addition of Ca(OH)2 to diluted phosphoric acid and complete neutralization at the boiling point [69]
Precipitated hydroxylapatite shows extremely small crystal sizes (hexagonal plates ~200Å sides) and large surface area from 50 to 200 m2·g−1.
\nThe Eh-pH diagrams for the Ca-P-H2O system at 25 and 300°C for 1.67 mol activity of Ca and 1 mol activity of P (
Eh-pH and PaCa-pH diagram of Ca-P-H2O system at 25°C (a) and 300°C (b).
The stability of calcium phosphates at higher temperatures is shown in Fig. 9. The equation numbers refer to the following reactions [21]:
Temperature dependence of free energy of reaction for some calcium phosphates according to
Eh-pH diagram of Ca-P-H2O system at 25°C (a), 100°C (b), 200°C (c) and 300°C (d).
For the purpose of this book the calculation of Eh-pH diagram for the solution where the concentration of ions (Ca2+, PO43− and OH−) is equivalent to the system containing 5·10−3 mol·dm−3 of apatite was performed. The ionic strength (refer to
In this system, The main difference against to the systems on Fig. 8 and Fig. 11 is significantly lower ionic strength.
Eh-pH diagram of Ca-P-H2O system with the concentration 20× higher than for that in
Other difference is a fact, that the field of stability of Ca(OH)2 starts at the pH = 13 for the system with elevated temperature. The formation of CaHPO4·2H2O, Ca2P2O7 and Ca3(PO4)2 was not predicted.
\n\nThe calculation for 20-times higher concentration Fig. 11 than for the system mentioned above shows broadening field of CaHPO4·2H2O. Ca2P2O7 was formed by the thermal condensation of CaHPO4 at temperatures higher than 164°C in acidic environment and Ca3(PO4)2 precipitated from the solution at nearly neutral conditions. Hydroxylapatite again predominates at higher pH and Ca(OH)2 does not appear at higher temperatures and the pH below 14 (the same as for Fig. 8).
\n\nThe phase equilibrium in the system CaO-P2O5-H2O was extensively studied by the solid-state reaction method under the atmospheric pressure of water vapor by Van Wazrer [70] and in aqueous systems at temperatures lower than 100°C by Brown et al [71],[72]. Biggar [73] studied the CaO-P2O5-H2O system in the temperature range from 700 to 950°C and the pressure of 1 kbar. Feng and Rockett [74\n] studied the system CaO-P2O5-H2O at 1000 bar with 50%wt. and 200°C (Fig. 12).
\nPhase diagram of Ca(OH)2-Ca3(PO4)2-H2O system [
The Fused salts are widely used in many industrial processes requiring to free the limitations arising from the use of aqueous solutions. Their thermal stability and generally low vapor pressure enable fast reaction rates and ability to dissolve many inorganic compounds making them useful solvents in electrometallurgy, metal coating, treatment of by-products, and energy conversion. It is recalled that one of the most important chemicals produced worldwide, sulfuric acid, is made by the molten salt catalysis. The electrolysis of molten salt is a technique used by H. Moissan for the isolation of element fluorine from the melt of KF·2HF (Moissan’s method is used for industrial production of fluorine). It was also used by H. Davy to discover several new elements (sodium, potassium, alkali metals) and to prove the chlorine as a new element (originally discovered by C.W. Sheelle who considered it as “
The structure of a molten salt is characterized by an alteration of positively and negatively charged ionic solvation shells around a given ion. This arises from the predominance of Coulombic effects, which results in a strong attraction between oppositely charged species and a strong repulsion otherwise [75].
\nThe utilization of molten salt precipitation method for the synthesis of apatites at “moderate temperatures” in the range from 500 to 700°C was also reported. Based on its principle, the method combines the advantages of thermal hydrolysis (“dry method”) and the precipitation from the solution (“wet method”). As a reaction media, the chloride melt of the equimolar NaCl-KCl (665°C) composition as well as eutectic melt (390°C) in the system Li2CO3 (27)–Na2CO3 (28)–K2CO3 (45% mol.) can be used. The most probable reactions are estimated from the thermodynamic consideration as follows [22]:
The original hydrothermal The term hydrothermal is of purely geological origin. It was first used by British geologist, Sir Roderick Murchison, to describe the action of water at elevated temperature and pressure in bringing about changes in the Earth´s crust, and leading to the formation of various rocks and minerals. Materials scientists popularized the technique, particularly during 1940s. The first hydrothermal synthesis was performed by Schafhautl in Papin’s digester, who obtained quartz crystals upon hydrothermal treatment of freshly precipitated silic acid [21].
Synthesis of new phases or stabilization of new complexes.
Crystal growth of several inorganic compounds.
Preparation of finely divided materials and microcrystallites with well-defined size and morphology for specific applications.
In situ fabrication of materials with desired size, shape and also dispersity in case of nanomaterials.
Leaching of ores in metal extraction.
Decomposition, alteration, corrosion and technique.
Several definitions of hydrothermal synthesis use aqueous solvent under HPHT conditions [21]:
In hydrothermal synthesis the material is subjected to the action of water, at temperatures generally near, though often considerably above the critical temperature The temperature and the pressure at critical point of water are 373.946°C and 22.064 MPa, respectively.
Hydrothermal synthesis is a heterogeneous reaction in aqueous media above 100°C and the pressure higher than 1 bar [78].
Hydrothermal synthesis involves water as a catalyst and occasionally as a component of solid phases in the synthesis at elevated temperature (>100°C) and pressure greater than a few atmospheres [79].
Depending on the type of solvent used in the heterogeneous reaction the glycothermal, alcothermal, ammonothermal, lyothermal, carbothermal, etc., methods are recognized. According to applied solvent and condition, the hydrothermal methods can be further divided as follows [21].
Hydrothermal conditions exist in nature, and numerous minerals including naturally occurring zeolites and gemstones, are formed by this process. The term has been extended to other systems with moderately raised conditions and temperatures lower than those typically used in ceramics and sol-gel syntheses. Lower temperatures used are one of the advantages of the method. Other methods include the preparation of compounds in unusual oxidation states or phases, which are stabilized by raised temperature and pressure [24].
\nTree showing the interdisciplinary nature of hydrothermal technology [
Hydrothermal synthesis was used industrially The first successful commercial application of hydrothermal technology was in mineral extraction or in ore beneficiation. The method was used to leach bauxite by sodium hydroxide by Karl Josef Bayer in 1892. The product of so-called Bayer´s process, aluminum hydroxide, is then converted to Al2O3 and used to produce aluminum metal or in ceramics [21].
Throughout the course of evolution of hydrothermal synthesis from the geoscientific applications to modern technologies, the hydrothermal technique has captured the attention of scientists and technologists from different branches of science. The hydrothermal technique is popularly used by geologists, biologists, physicists, chemists, ceramists, hydro-metallurgists, materials scientists, engineers, etc. Fig. 13 shows different branches of science either emerging out from the hydrothermal technique or closely linked up with the hydrothermal technique. One could firmly say that this family tree will keep expanding its branches and roots in the years to come [21].
\n\nThe hydrothermal techniques for the preparation of compounds with the structure of apatite should be divided to:
low-temperature hydrothermal synthesis (LHS);
high-temperature hydrothermal synthesis.
The hydrothermal synthesis of all three normal apatite end-members was reported by Baumer and Argiolas [80]. They prepared crystallites of sizes from 50 to 500 μm. The synthesis of chlorapatite at 400°C and the pressure <3 kbar proceeds via the reaction:
The synthesis and the stability of carbonate-fluorapatite were examined by Jahnke [81]. The carbonate-apatite phase is stable in solutions relatively rich in carbonate such as sea-water. When exposed to low-carbonate solutions, the carbonate-apatite should lose the CO32− ion [82].
\nDuring the hydrothermal synthesis of HAP whisker, the acetamide was used by Zhang and Darvell [83] as an agent to drive homogeneous precipitation at temperatures below 100°C. Acetamide shows low hydrolysis rate in both acidic and basic conditions, releasing acetate and ammonia:
which do no substitute in HAP lattice. The precipitation of hydroxylapatite from the solution of Ca(NO3)2·4H2O and (NH4)2HPO4 in 0.05 mol·dm−3 (Ca:P = 1.67) treated to the temperature of 180°C for 10–15 hours yielded to large rod-like and well-crystallized particles of hydroxylapatite.
\nThe stoichiometric single crystals of hydroxylapatite nanorods with mono-dispersion and narrow-size distribution in diameter were successfully synthesized by Lin et al [84] via the hydrothermal microemulsion method [85]. The emulsification consists in dispersing of one fluid in another, non-miscible one, via the creation of interface [85]. The name surfactant is a contraction of the term:
The first technique that was used for the production of crystals Fig. 14(a) was described by Verneuil [90],[91],[92],[93] at the turn of the 20th century, \nVerneuil in fact wished to study the properties of ruby and other alumina-based crystals and was aware of very high melting temperatures of these materials, which prevented the use of any crucible material known in that time. This problem was solved- by melting alumina powder in a hydrogen-oxygen flame and solidifying the droplets on a colder seed. Nowadays this technique is used for the production of single crystals of sapphire (single crystal of Al2O3 in The scheme of Verneuil’s growth unit [87],[90],[93]: electromagnet (A, or camshaft) operating the hammer (M), supply chamber of fine Al2O3 powder (P), feeder (C, D), oxygen (O) and hydrogen (H) inlet, growing crystal (R), crystal holder (S) and device for the crystal adjustment (V). Small dimension is necessary to dissipate the latent heat of solidification efficiently and rapidly [87].
Kyropoulos developed the melt growth techniques (Fig. 15) for growing large crystal from the melt using a cooled seed in 1926 [96],[97],[98]. The method was demonstrated via the production of large single crystals of alkali halides [99].
\nScheme of Verneuil’s method42 (a) [
Schematic illustration of Kyropoulos method [
After important growth processes based on capillarity, historically the next development was the Bridgman method [100], aiming at increasing the crystal size and consisting in growing the crystal in crucible. The next method to be invented in 1952 by Phann [101] was the floating zone (FZ) technique. The floating zone is generated by means of water-cooled induction coil fed by radio frequency power in the megahertz range [103]. Marangoni convection, which is caused by the differences in the surface tension over the melt surface, flows along the interface from the surface to a central region of the melt. On the other hand, forced convection, which is caused by the crystal rotation, flows towards the periphery from the center [102].
Since then various modifications of these basic methods have been proposed, such as the pedestal growth, edge-defined film-fed growth (EFG) process, inverted EFG process, micro-pulling down (μ-PD, Fig. 14(c)), etc., all based on the use of capillary force in order to maintain and shape the liquid. Fig. 17 show the classification of these methods based on the presence or absence of the crucible or shaping die in contact with molten material and on the direction of pulling [87],[89],[103],[104].
\nSchematic representation of convection in the molten zone [
Whiskers can be described as long filamentary defect-free single crystals of great mechanical strength, which is attributed to their high structural perfection. The explanation of whisker growth is based on the screw dislocation theory. The dislocation appears only along the whisker axis, while in another two dimensions the faces will stay perfect. Consequently, no growth will occur at an appreciable rate on the side faces of whisker. Due to the presence of axial screw dislocation the whisker grows only along its axis [105]. Apatite whiskers are usually prepared by hydrothermal synthesis [83],[106],[107],[108], molten salt method [109] and also via the precipitation method [110].
\nDendrites The name was derived from the Greek word ”tree like”.
Classification of various crystal growth processes using capillary forces for maintaining or shaping the molten material [
Single crystals of fluorapatite up to 5 cm long and of 1 cm maximum diameter were first prepared via the Kyropoulos method (pulling the crystal from the melt) by Johnson [114]. The Czochralsky method was used by Mazelski et al [114],[115] to grow the crystals up to 30 cm long. The ratio of CaF2 to Ca3(PO4)2 as determined by chemical analysis of crystals depends upon the value of the same ration in the melt. Even if the melt had correct stoichiometric composition, grown fluorapatite would appear to have the deficiency of CaF2 of about 5%. Fluorapatite as well as chlorapatite crystal with the length from 5 to 6 mm were grown by Prener [116] from the solutions of apatite in molten calcium fluoride and chloride, respectively. The analyses of these flux-grown crystals agreed with theoretical values within 0.1% [114],[117].
\nSingle crystals of apatite-type Nd9.33(SiO4)6O2, Pr9.33(SiO4)6O2 and Sm9.33(SiO4)6O2 were prepared by Higuchi et al [102],[118],[119] from the stoichiometric mixture of Nd2O3, Pr6O11 and Sm2O3 with SiO2 (9.33 : 6) via the floating zone method. The crystal growth using the optical floating zone technique (a) was extensively used to grow a variety of bulk crystals, particularly single crystals of metal oxides [120],[121].
\n\nThe pseudobinary phase diagram for the Nd2O3–SiO2 system around the apatite phase is shown in Fig. 19 [118],[122]. With the except of the end-member Nd2O3 and SiO2, the apatite phase (Nd2O3 : SiO2 = 7:9), Nd2SiO5 and Nd2Si2O7 are observed. Both, Nd2SiO5 and Nd2Si2O7 melt incongruently, while the apatite phase melts congruently.
\n\nYoshikawa et al [123] prepared <0001> oriented Ca8La2(PO4)6O2 (CLPA) single crystals with the apatite structure, which were grown by the Czochralsky method. This material can be used as substrate for the growth of <0001> GaN epitaxial layers.
\nSchematic diagram of the furnace with double ellipsoidal mirrors (a) and single grown crystals of Pr9.33(SiO4)6O2 (b), Nd9.33(SiO4)6O2 (c) and Sm9.33(SiO4)6O2 (d) [
Reconstructed pseudobinary phase diagram around the apatite phase Nd9.33(SiO4)6O2 in the Nd2O3-SiO system [
The growth of single crystal of synthetic analogue of vanadinite (lead vanado-chlorapatite, Pb5(VO4)3Cl) using the CsCl flux method was performed by Masaoka and Kyono [124]. No impurity phases were formed from this crystal growth method. Crystals obtained via this method exhibit well-developed hexagonal prismatic form of the size of several millimeters along the [0001] direction. The largest crystals were approximately 6×1×1 mm.
\nThe first hydrothermal growth of single crystals of chlorapatite was reported by Roufosse et al [125]. Crystals grown from the system chlorapatite-HCl-H2O at 50 000 psi and pH = 1 with the growth zone at 465°C and dissolution zone at 360°C were found to be of high stoichiometry.
\nThe synthetic analogue of the mineral hydroxylapatite can by prepared by the reaction [126]:
Aqueous solutions of 0.167 mol·cm−3 of Ca(NO3)2 and 0.100 mol·cm−3 of (NH4)2HPO4 were prepared, and their pH values were adjusted to above 8 by the addition of ammonium hydroxide. (NH4)2HPO4 solution was heated to about 85°C and then slowly dropped into equal volume of vigorously stirred solution of Ca(NO3)2. The temperature of the reaction mixture was kept at 85°C and stirring was maintained for further 3 days. In order to remove CO2, the flow of N2 was introduced to the suspension in reaction vessel. The suspension was then filtered and washed.
\nThe survey of known chemical reactions successfully used for the synthesis of hydroxylapatite was provided by Shojai et al [32]. Depending on applied method (Table 2) and conditions (Fig. 20), different shapes of apatite particles can be prepared.
\nShape of hydroxylapatite particles prepared by given synthesis methods [32].
* Consult with
** Solid-state synthesis (ss), mechanochemical method (mch), conventional chemical precipitation (cc), hydrolysis method (hl), sol-gel method (sg), hydrothermal method (hth), emulsion method (em), sonochemical method (sch), high-temperature processes (ht), synthesis from biogenic sources (bs), combination procedures (cp).
The influence of conditions on the morphology of hydroxylapatite particles is shown in Fig. 20. During hydrothermal synthesis, the particle size of HAP decreases with increasing pH value [32],[127],[128].
\nThe formation and the morphology evolution mechanism of Ca5(PO4)3OH samples with various morphologies based upon different pH values [
Complete replacement of halogen occurs when either fluorapatite or chlorapatite is heated in the steam of H2 or H2O at high temperatures [69]:
In literature various routes for the preparation of synthetic analogues of fluorapatite are described which include solid-state reactions of the type [129]:
At the temperature of 900°C hydroxylapatite reacts with calcium fluoride to give fluorapatite [69]:
Fluorapatite can be also prepared directly by firing a mix of 3Ca3(PO4)2 with CaF2 at 1600°C, or from calcium pyrophosphate and calcium fluoride:
Chlorapatite can be prepared by similar method using calcium chloride. It can also be produced in the reversible reaction according to
Original phase diagram Fig. 21(a) for the section Ca3(PO4)2–CaF2 of the ternary system CaO–P2O5–CaF2 was published by Nacken [130]. The range of compositions was extended by Berak [131] (b), and further refined (Fig. 22) by Berak and T.-Hudina [132]. Important features are congruent melting of Ca10(PO4)3F2 at 1650°C, eutectics with Ca3(PO4)2 at 1620°C and second one with CaF2 at 1203°C. Sufficiently precise phase diagram enables to determine necessary information on the flux growth of fluorapatite, so the crystal with only slight deficiency in fluorine compared to the theoretical one can be prepared. The problem concerning possible stable existence of spodiosite (Ca2(PO4)F) analogous to naturally occurring mineral remains unsettled, but it appears unlikely to be stable at liquidus temperatures [133].
\nPhase diagram of Ca3(PO4)2–CaF2 section by
Phase equilibrium in the system Ca3(PO4)2–CaF2: Ca10(PO4)6F2 (ApA) and Ca7(PO4)4F2 (ApB) [
The implication of the crystal growth of apatite and calcite in the systems Ca3(PO4)2–CaCO3–Ca(OH)2–CaF2 (Fig. 23(a)) and Ca3(PO4)2–Ca(OH)2–CaF2–H2O (
System Ca3(PO4)2–CaCO3–Ca(OH)2–CaF2 (a) and Ca3(PO4)2–Ca(OH)2–CaF2–H2O (b) at the pressure of 1 kbar [
Long and uniform HAP whiskers with high crystallinity, controlled morphology and high aspect ratio were synthesized by Zhang and Darwell [83] via the hydrothermal method using acetamide. Compared to urea as an additive, which is commonly used to raise the pH in order to drive the nucleation and growth of HA crystals [106], acetamide has low hydrolysis rate under required hydrothermal conditions. This allows better and easier control, giving rise to rapid growth of whiskers at low supersaturation. The whisker length and width were in turn given by the solution conditions, including the concentration of Ca and PO4 [83].
\nBarium apatite can be prepared by solid-state reaction [135]:
It possesses typical hexagonal structure with the space group P63/m and
Ba(1) atoms are located in columns on three threefold axes and are coordinated by nine oxygen atoms. The Ba(2) sites form triangles around the F site and are coordinated by six oxygen atoms and one fluoride ion. Fluoride ions are statistically displaced by ∼0.25 Å from the Ba(2) triangles. This displacement of F ions is analogous to the displacement of OH ion in Ca10(PO4)6(OH)2 [138].
\nThe stoichiometric Ca:P ratio in the composition of chlorapatite, the mole ratio of calcium to phosphorous was equal to 1.67 [139]. The reaction of CaCl2 with H3PO4 under hydrothermal conditions including the temperature of 400°C and the pressure < 3 kbar leads to chlorapatite (
The mechanochemical synthesis of chlorapatite in a high energy planetary mill should be described by the reaction [139]:
\nNacken [141] determined the phase diagram for the section Ca3(PO4)2–CaCl2 of the ternary system CaO–P2O5–CaCl2 (Fig. 24). Chlorapatite crystallized from melts of its own composition is highly deficient in Cl, while lower temperatures near 1040°C lead to the crystallization of stoichiometric chlorapatite [133].
\nPhase equilibrium in the system Ca3(PO4)2–CaCl2 by
The mechanosynthesis and the characterization of chlorapatite nanopowders were performed by Fahami et al [139]. The formation of chlorapatite takes place according to the reaction 29. At the beginning of milling, the main products were stoichiometrically deficient chlorapatite and calcium oxide. Eventually, high crystalline CAP nanopowder was obtained after 300 min of milling. By increasing the milling time to 300 min, the lattice strain significantly increased.
\nLarge crystals of Cd5(PO4)3Cl (space group P63/m,
The structure of apatite phase of the composition Ba5(OsO5)3Cl (P63cm,
Projection of the structure of Ba5(OsO5)3Cl along the c-axis [
\nSuzuky and Kibe [148] used the NaCl flux method to prepare barium (Ba5(PO4)3Cl) and strontium chlorapatite (Sr5(PO4)3Cl) crystals and modified. The weight of liquid was measured instead of the weight of crystal. Since measured parameter is force ( The value should be affected by the estimation of value of aspect ratio. First-order hexagonal prism and first-order dipyramid, respectively.
where
It seems now to be generally accepted that CO32− dominantly replaces PO43− in biological apatite (BAP, BAp) [155]. Carbonate-hydroxyl-apatite (Ca10(PO4,CO3)6(OH)2), can be found mainly on islands and in caves, as a part of bird and bat excrements, guano [156].
\nCarbonated hydroxylapatite is the most important mineral in human dental enamel and bone [157],[158],[159],[160],[161],[162],[163],[164]. The presence of highly carbonated apatite was also proposed as a marker of the presence of bacteria (infectious microorganism) in kidney stones From the medical point of view, pathological calcifications refer to a concretion, e.g. a kidney stone, often associated with the tissue alteration. Additionally, normal physiological calcifications such as bone may become pathological through the influence of diseases such as arthrosis or osteoporosis Different chemical phases constitute the pathological calcifications, but calcium phosphate apatites are present in most of them [166]. Biological apatites (BAP) are described in
The crystal structure of type-A carbonate apatite is controversial [172]. There are three different structures: with the space group\n
The atomic configuration of type-A carbonated apatite on the (010) plane (a) and (001) plane (b) according to
where
Two different structural roles of CO32− anion result in characteristic infrared (IR) signatures: type A carbonate having a doublet band at about 1545 and 1450 cm−1 (asymmetric stretching vibration,
Published structural studies [158] of carbonated apatites were performed with the synthetic phases. Ren et al [171] investigated the structure of carbonated apatite using the ab initio simulation (Fig. 27) with the conclusion that the most energetically stable substitutions is type-AB in which two carbonate ions replace one phosphate group and one hydroxyl group respectively. The crystal structure of A-type of carbonated apatite is energetically more favorable than B-type of substitution. The most stable configuration of type-A is carbonate triangular plane almost parallel to the
The model of channel structure for ideal carbonate ion geometry of
The type-A of carbonated apatite in which carbonate ion was completely substituted for the hydroxyl site, was synthesized by heating low crystalline and stoichiometric synthetic analogue of hydroxylapatite powder in the flow of dry carbon dioxide gas at 1000°C for 24 h by Tonegawa et al [172]. The chemical composition of this phase can be described by the formula: Ca10(PO4)6(CO3)0.93±0.06. The crystal structure was determined to be of monoclinic symmetry with the space group Pb in the temperature range from 25 to 500°C.
\nThe synthesis of type-A carbonate apatite can be performed by heating of pure HAP at temperatures from 800 to 1000°C for several hours in dry CO2 atmosphere according to the reaction [176],[179]:
Type-B carbonated apatite powders are generally synthesized from the precipitation reaction in aqueous media [176]. The reaction
The mechanochemical synthesis of B-type carbonated fluorapatite under argon atmosphere using high-energy planetary ball mill was described by N.-Tabrizi and Fahami [180]. The process can be described by the reaction:
Carbonated chlorapatite nanopowders can be synthesized by the mechanochemical process under argon atmosphere using the mixture of calcite (CaCO3), phosphorus pentoxide (P2O5) and calcium chloride (CaCl2) as raw materials [181],[182]:
The substitution degree of PO43− was given by the
The high-pressure (1 GPa) synthesis of sodium-bearing carbonate chlorapatite of type A-B (CCLAP, Ca10−(y+z)Nay[V]z[(PO4)6−(y+2z)(CO3)y+2z][Cl2−2x(CO3)x], where
The structure of carbonate chlorapatite showing one of 12 possible orientations of the type-A carbonate ion in apatite channel: the unit-cell origin is in the center of figure, shaded phosphate polyhedra and Ca(2) atoms are centered at
The structure of Na-bearing CCLAP crystals (Fig. 28(a)) with the contents of Na and A and B-type of carbonate ranges between those of Na-bearing carbonated fluorapatite (CFAP) and carbonated hydroxylapatite (CHAP). The stoichiometric amount of Na and A-type of carbonate is consistent with the near linear (1:1) correlation reported for CHAP and CFAP and provides the evidence of active role of Na in the substitution of carbonate into the apatite channel, even if Na does not appear in usual charge-balanced substitution scheme [169]:
On the other hand, the B : Na ratio is higher than one (approximately 1 : 1.5) and is located between the values determined for CHAP (B : Na = 1) and CFAP (B : Na = 2). The substitutions of B carbonate ion into CCLAP seem to be more complex than those into CHAP, which is expressed by Fig. 28 or by the following charge-balanced substitutions scheme:
There should be additional vacancies including the charge-balancing mechanism:
This leads to the formula of sodium-bearing carbonate chlorapatite mentioned above.
\n\nSimilar profiles of
The synthesis of hydroxyl-chlorapatite solid solution via the precipitation method can be presented as follows [183]:
Also fluorine and chlorine co-substituted hydroxylapatites can be prepared by aqueous precipitation method [184]:
Carbonate can be introduced into the structure of carbonated barium-chlorapatite by stirring apatite in an (NH4)2CO3 solution for 1 week [185]:
The attempts to prepare carbonated barium-chlorapatite in a one-step synthesis results in a mixture of BaCO3 and Ba3(PO4)3. The variations in the manner in which carbonate was added to the reaction mixture, such as co-titrating a carbonate solution along with BaCl2 and NH4H2PO4, pre-mixing it with NH4H2PO4, or adding it first or last did not eliminate the precipitation of simple salts. The inability at 60°C and at the pH of 10 to produce carbonated barium-chlorapatite at any ratio of carbonate to phosphate in the aqueous solution is probably due to close molar solubility of simple salts [185].
\nCalcium bromapatite has typical hexagonal apatite structure with the space group P63/m,
The structure of Ca5(PO4)3Br (perspective view along the c-axis).
The phase can also be prepared via solid-state synthesis reaction [135]:
The synthesis of
The structure of lead bromapatite identifying the channel polyhedron (broken lines) formed by Pb(2) cations in apatite channel wall: open Pb(2) circles are at the height z = 1/4 and closed circles are at z = 3/4; triangles are PO4 tetrahedra centered at z = 1/4 (open) and z = ¾ (shaded); numbers (1, 2, 3) identify oxygen atoms forming the corners of tetrahedra [
\nLiu et al [190] prepared synthetic lead bromapatite via solid-state reaction at pressure up to 1 GPa. In the structure of this phase (Fig. 30), isolated PO4 tetrahedra centered at z = 1/4, 3/4 are linked by Pb(1) in nine-fold (6 + 3) coordination and Pb(2) in an irregular sevenfold (6 + 1) coordination. A prominent feature is large c-axis channel which is defined by tri-clusters of M(2) cations at z = 1/4, ¾ and accommodates a variety of anion components.
\n\nStrontium bromapatite (strontium bromoapatite) can be prepared via solid-state reaction (
Since the precipitate contains Na+ ions, it must be washed thoroughly to obtain pure product. A small amount of hydroxylapatite may also be present.
\nStrontium bromapatite forms softer crystal than fluorapatite or strontium chlorapatite. Since it is not stable under the mercury-vapor discharge in fluorescent lamp (
Other bromapatites are Cd5(PO4)3Br (
Since, the apatite structure is capable of accommodating monovalent anions, strontium iodoapatites were investigated as a potential waste form to immobilize radioactive iodine [135],[192].
\nCalcium iodoapatite (Ca5(PO4)3I) does not exist as a separate phase but as oxoapatite. Iodo-oxyapatite (pentadecacalcium iodide oxide nanophosphate, Ca15(PO4)9(I,O)) was synthesized by the flux method (
Strontium iodoapatite (strontium iodoapatite, strontium iodine-apatite) is of academic interest due to large size of I− ions compared to other halide ions. However, the thermodynamic functions determined for the alkaline earth apatite series preclude the formation of stable iodoapatite because the cationic size of Sr2+ or Ba2+ is too small relating to that of iodide ion which must fit upon the
The preparation of lead vanado-iodoapatite (Pb10(VO4)6I2) by hot pressing (HP), isostatic hot pressing (HIP) and sealed-tube method (
Facile low temperature solid-state synthesis of iodoapatite by high-energy ball milling of PbI2, PbO and V2O5 was described by Lu et al [195]. As-milled iodoapatite is in the form of amorphous matrix embedded with nanocrystals and can be readily crystallized by subsequent thermal annealing at low temperature of 200°C with minimal iodine loss.
\nSynthetic cadmium apatites containing iodine such as Cd5(VO4)3I (space group P63/m,
Radium iodoapatite, if could be formed, would have the formula Ra5(PO4)3I but it has not been prepared yet. This salt would be probably best prepared by solid-stare reaction [135]:
Whether this compound can be formed remains speculative. In human body radium behaves in a similar way as calcium. When ingested, it is readily adsorbed in bone where it may directly irradiate the bone and other tissues. This exposition may result in fatal disease as the tragic story of “
The preparation and the structure of chalcogenide phosphate apatites of the composition Ca10(PO4)6S (calcium sulfoapatite), Sr10(PO4)6S (strontium sulfoapatite), Ba10(PO4)6S (barium sulfoapatite) and Ca10(PO4)6Se (calcium selenoapatite) was reported by Henning et al [196]. These apatite phases are isostructural and crystallize in the trigonal space group\n
The apatitic structure can accommodate a great variety of other substituent’s and vacancies in anionic sites (
Polyhedral view in the ab-plane of the crystal structure of NaCaPb3(PO4)3 showing the tunnels [
Lead in apatite is of great interest from two points of view. First, lead is known as a “bone seeker” as it accumulates in bones and teeth, second, it may contribute to the deviation from the general formula of apatites. Moreover a new voltammetric sensor for the quantification of mercury based on NaCaPb3(PO4)3 modified carbon paste electrode can be prepared. Because of the importance of these types of lacunar apatites and the problems which they may cause in biomaterial applications, particular attention has been paid during past few years to synthesize new lacunar anionic apatites [198],[199].
\nSilver lead apatite (Ag2Pb8(PO4)6, P63/m,
The unit cell contains eight divalent Pb2+cations, two monovalent cations (Na+ or Ag+) and six [PO4]3− ions. The triangle sites, 6
The structure of this phase was also investigated by Koumiri et al [201]:
Pb2(II) cations with stereochemically inactive lone 6
Pb1(II) is engaged in a Pb(1)–O bond with more covalent character, where its lone 6
The correlation chart for PO43− fundamental modes under free-ion, site-group and factor group analyses in Pb8M2(PO4)6 where M = Ag and Na [
All [PO4]3− groups are crystallographically equivalent in the cell and have
where
\nNaddari et al [202] performed the solid-state synthesis of colorless calcium-lithium lead apatite (Pb6Li2Ca2(PO4)6, LCPbAp, P63/m,
Perspective view of Pb6Ca2Li2(PO4)6 structure (a) and Pb(II)-Pb(II) stacking in Pb6Ca2Li2(PO4)6 showing possible arrangement of electron lone pairs [
Lithium ions occupy preferentially site (I) and this structure is anionic lacunary apatite stabilized by the interaction of Pb(II) electron lone pair. The electrical conductivity as a function of temperature can be interpreted assuming a hopping mechanism of Li ions in the tunnels [202].
\nTricationic lacunar apatites Na1−xKxPb4(AsO4)3 (0 ≤
It was found that Pb(II) ions in the solid solutions preferentially occupied the M(1) and M(2) sites in the lacunar anionic apatite structure. The structure contains the channels running along the
The factor group analysis [198] of the hexagonal structure (P63/m) shows that the normal modes of vibration can be classified among the irreducible representations of C6h as follows:
where the internal mode contribution of (AsO4) groups to the IR- and Raman-active vibrations is:
where
The syntheses of apatites, Na1−xKxCaPb3(PO4)3 (0 ≤ x ≤ 1), with anion vacancy were carried out using the solid-state reactions at 700°C for 48 h [199]:
The lattice constants of the solid solutions varied linearly with x. It was found that Pb ions in the solid solutions occupied M(1) and M(2) sites in the lacunar apatite structure. The structure was described as built up from [PO4]3− tetrahedra and Pb2+ of six-fold coordination cavities (
The factor group analysis of the hexagonal structure (P63/m) shows that the normal modes of vibration can be classified among the irreducible representations of C6h by
These minerals were usually prepared in order to elucidate the structure of naturally occurring minerals or due to its potential applications in immobilization of nuclear and toxic waste (
Synthetic cesanite as an analogue of mineral with the composition Na3Ca2(SO4)3(OH) (
The projection of the crystal structure of synthetic cesanite parallel to (001) (1) and the arrangement of cations and sulfate tetrahedra around the 63 and the 6̅ axes, respectively (2): phosphate apatite (a) and synthetic cesanite (b) [
Small spread in the S-O distances and O-S-O angles indicates only minor deviations from ideal tetrahedral symmetry. The sub-structure of the array of sulfate tetrahedra shows a distinct pseudo-symmetry, closely mimicking P63/m. Maximal deviations from this symmetry occur at O(4) atom, which is shifted by 0.16 Å (synthetic) and 0.02 (natural) from its position in P63/m. Na and Ca cations are distributed either by six O atoms and one hydroxyl ion or water molecule (M(1) and M(2)) or by nine O atoms (M(3) and M(4) [205].
\nSynthetic analogues of minerals cesanite Halide sulfates have general formula [206]:
where Z = OH, F and Cl. Klement [207] synthesized sodium-calcium sulfatapatite, Na6Ca4(SO4)6F2, by full substitution of S6+ for P5+ through the substitution scheme [208]:
where the hydroxyl equivalent is the equivalent to mineral cesanite, Na6Ca4(SO4)6(OH)2. Kreidler and Hummel [209] also synthesized Na6Ca4(SO4)6F2 and Na6Pb4(SO4)6F2 apatite-like phases. Knyazev et al [206] prepared the compounds of the composition of Na3Ca2(SO4)3F, Na3Cd2(SO4)3Cl, and Na3Pb2(SO4)3Cl with the structure of apatite via the solid-state reactions:
from the stoichiometric reaction mixture in a porcelain crucible. The mixtures of components were calcined in several steps at the temperatures of 570, 770 and 1020 K for 10 h, with intermediate grindings in agate mortar every 2 h [206].
\nThe Na3Ca2(SO4)3F:Ce3+ phosphor was prepared by Nikhare et al [210] via the solid-state method according to the following reaction:
The pigment shows a single high intensity emission peak at 307 nm when excited by UV light of the wavelength of 278 nm
\nThe compound having the formula: K3Ca2(SO4)3F, was identified in coatings of heat recovery cyclones of Portland clinker kiln. The structure of this phase (noncentrosymmetric, space group Pn21a,
The structure of K3Ca2(SO4)3F according to
The activation by Eu or Ce leads to the phosphor: K3Ca2(SO4)3F:Ce, Eu, which was prepared by Poddar et al [213] via the precipitation method. The K3Ca2(SO4)3F:Ce luminescent pigment shows the emission at 334 nm when excited at 278 nm due to the 5
The synthesis, the characterization and ionic conductivity of Ca8−xSrxBi2(PO4)6O2 phase where
New bismuth calcium silicon oxide Ca4Bi4.3(SiO4)(HSiO4)5O0.95, with the apatite structure was synthesized by Uvarov et al [215]. The structure was refined from the powder X-ray diffraction data. The refinement revealed that the phase had the P63/m space group with the unit cell parameters
Also the structure of bismuth calcium vanadium oxide (BiCa4V3O13, BiCa4(VO4)3O) was reported by Huang and Sleight [216] as apatite without an inversion center. The phase crystallizes in hexagonal system with the space group P63,
The hexagonal channel in the structure of apatite can accommodate infinite linear chains of [-Me-O-]nn−, where Me = Cu, Zn, Ni, Co… (Fig. 36). The incorporation of
Crystal structure fragments of doped apatite showing the atomic arrangement at the hexagonal channel where 3-d metal atoms are located [
Depiction of the structure in hexagonal channels (along the c-axis) in the lattice of copper-containing apatite: hydroxylapatite (a), hydroxylapatite with OH partially replaced by Cl and hydroxylapatite with OH partially replaced by F (c). The planes passing through Ca atoms depict the channel walls.
Doping of Sr5(PO4)3OH with ZnO, NiO and CoO at 1400°C in air resulted in the incorporation of 3d-ions entering the hexagonal channels of the apatite structure, formally substituting for protons in the OH groups. The structure of apatite channels in the phases with the composition of Sr5(PO4)3Zn0.15O0.3(OH)0.7 (white and shade of green), Sr5(PO4)3Ni0.2 O0.4(OH)0.6 (green) and Sr5(PO4)3Co0.2O0.5(OH)0.4 (dark-violet) contains O-Me-O fragments separated by OH groups. Co atoms were localized in the position shifted by 0.5 Å from the center of channel. Their coordination can be described as distorted from linear O-Co-O probably by additional coordination to phosphate oxygen atoms [217].
\n\nIn other work of Kazim et al [218], the synthesis and the properties of three compounds possessing the apatite structure with the composition of Ca5(PO4)3CuyOy+δ(OH)0.5−y−dX0.5, where the parameter
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In the context of this chapter, a satellite is a spacecraft (SC) that orbits around a celestial body such as the earth. A spacecraft has several design constraints placed upon it before it can be placed in an orbit around the intended celestial body. First, satellite designs are limited in their mass and volume to fit on the launch vehicle that places them into orbit. Secondly, the mass and volume limits affect the size of the power system on the spacecraft; therefore, the amount of power available to the satellite is also limited. In addition, the space environment (thermal, radiation, atomic oxygen, space debris, micrometeoroids, etc.) imposes constraints on the design such as parts and material selection.
A spacecraft is consisted of two parts: the spacecraft bus and the payload (PL) [1, 2]. The spacecraft bus provides control of the satellite and support services to the mission payload, while the mission payload provides the mission part of the satellite including payload control, mission data processing, and mission data downlink dissemination. Examples of mission payloads (or payloads or PLs) are: scientific instruments, remote sensing instruments, navigation service transmitters, or communications equipment. A satellite may have one type of PL or a combination of payload types to accomplish its mission such as navigation, remote sensing, and communications. Shown below in Figure 1 is a typical imaging satellite used for the remote sensing mission. Note the clear separation between the spacecraft bus that provides solar power and maneuvering capability via thruster, while the payload consisting of the camera and supporting communication devices such as antennas and guidance devices such as star trackers.
A typical satellite with bus and payload separation.
Regardless of the mission type1 and the payload that a spacecraft carries, a subsystem that must exist in all satellites is the communication subsystem that enables the spacecraft to communicate with the ground stations that control the satellite and to deliver the data that the mission requires. This chapter focuses on architecture and functionalities of the communications subsystem that usually resides on the satellite.
There are three specific segments shown in Figure 2 below that must work together for the larger overall system to provide communication, navigation, or any other type of missions:
The space segment consisting of all satellites and associated equipment required for the mission applications and the launch vehicles used to deliver those satellites to orbit.
The satellite control (or control) segment consisting of all the personnel, facilities, and equipment that are used to monitor and control all the assets in space. Practically, the control segment is also referred to as satellite ground segment because it is usually located on the ground.
The user segment consisting of all the individuals and groups who use and benefit from the data and services provided by the payloads of the satellite and the equipment that allows this use.
The three main segments for satellite system.
In general, the space mission dictates the type of orbit2, satellite design and its expected life cycle, and its operational scenarios. The PL design includes dimensions, interfaces, weight, physical characteristics, and basic utility needs (e.g., power consumption), which usually influences spacecraft (SC) bus design. The PL is often a unique and one-of-a-kind design tailored to meet specific mission requirements, frequently relying heavily on newer technology, while the satellite bus has the supporting function, and as such relies largely on existing or modified hardware such as batteries, inertial devices, and star trackers. Since PLs and their missions vary widely, so is this satellite bus supporting role.
Traditionally, the PL is considered a subsystem of the satellite bus that is designed to generally satisfy the corresponding mission requirements. The PL operational requirements sometimes impose specific requirements on the satellite bus that must be satisfied for the PL to accomplish its mission. This interdependence between satellite bus and PL subsystems has historically resulted in many nonstandard interfaces developed and implemented by the incumbent spacecraft builders. As a result, the aerospace industry has been moving toward a more standardized and commodity satellite bus framework that can potentially result in a tremendous cost saving approach.
As shown in Figure 3 below, a satellite bus typically consists of the following subsystems: command and data handling subsystem (C&DHS); communications subsystem (CS); electrical power subsystem (EPS); propulsion subsystem (PS); thermal control subsystem (TCS); attitude control subsystem (ACS) also known as guidance, navigation and control (GNC) subsystem; structures and mechanics subsystem (S&MS); and life support subsystem for manned missions if required. The C&DHS will be described in detail below. The CS provides the satellite bus with the necessary communication functionalities to connect the user and ground segments to different satellite subsystems. The EPS provides the electrical power generation and distribution for various spacecraft subsystems. The PS provides maneuvers necessary for altitude, inclination adjustment, and momentum management adjustments. The TCS provides active thermal control from electrical heaters and actuators to control temperature ranges of equipment within specific ranges. The ACS provides proper pointing directions for the satellite subsystems, such as sun pointing for EPS to the solar arrays and earth pointing for CS. The S&MS provides the necessary mechanical structure to withstand launch loads by the launch vehicle, during orbital maneuvers, as well as loads imparted by entry into the atmosphere of earth or another planetary body.
A typical satellite bus and payload subsystem.
On the other hand, a PL is tailored to a specific mission type. For example, a remote sensing satellite can have as its payload an electro-optical (EO) camera to take day-time pictures of the earth and then convert them to electrical signals that can be captured. Alternatively, the camera may also have infra-red (IR) sensors that enable the PL to see the earth at night, or microwave sensors that will let the PL “see” radio frequency (RF) signals from the earth at several radio frequencies (RFs). These sensors can be classified as passive or active, and each of them can be further classified as imaging or sounding3. Figure 4 below illustrates a generic imaging PL that will convert the sensor analog data into electrical signals that can be captured and transmitted to a ground station. Note the existence of a communication subsystem as part of this imaging payload.
A typical and generic sensor payload.
In this section, the different typical modules of a satellite communication subsystem are discussed. In addition, the command and data handling subsystem, and command, telemetry and mission data processing subsystem will also be described in detail.
At the physical layer, the communications subsystem starts with an antenna and the RF front-end transceiver. The antenna is the most important component of the communications subsystem where the electromagnetic (EM) signals are originated or received. The RF front-end/back-end is where the EM signal is being down/up-converted to baseband/RF signal to be demodulated/modulated for baseband signal recovery or downlink transmission, respectively. Figure 5 below depicts a typical transmitter and receiver (transceiver) chain with the modulation and demodulation (MODEM), followed by the RF front-end and the antennas. The baseband communications function is carried out by the MODEM, whereas the RF portion is handled in the transceiver, RF front-end, and antenna sections.
Typical RF front-end chain.
Modulation is the name given to the process of impressing the wanted signal to be transported onto a radio frequency (RF) carrier, which is then conveyed over the satellite link and demodulated at the receiving terminal to extract the wanted signal from the carrier. Thus, modulation translates a baseband spectrum (at zero frequency) to a carrier spectrum (at RF range) and demodulation is the process of recovering the data at the receiver end of the link. Thus, the process requires a modulator and a demodulator, collectively known as a MODEM. The input to the modulator may require some initial processing such as filtering and amplitude limiting.
Before the RF signal is sent to the antenna, a traveling wave tube amplifier (TWTA) or solid-state power amplifier (SSPA) is needed to amplify the RF signal to a desired level for transmission. Conversely, after the RF signal is received by the antenna, a low noise amplifier (LNA) is needed to ensure that the received signal is brought up to the desired signal level with minimum noise before demodulation.
In addition to being lighter than TWTA, the achievable power efficiency for SSPAs is a major factor to support transmit phased arrays. Currently, the tube-based TWTA implementations are still the most cost-effective design, even though both options might be viable for lower power systems.
In increasing technical maturation over the years, the following types of spacecraft antennas have been used for satellite communications:
Low-gain omni and squinted-beam antennas for large earth coverage.
Increased gain types of satellite antennas (horn type and helix antennas) for medium earth coverage.
Parabolic reflectors, including multi-beam antennas with multiple feed systems for multiple user and small area coverage.
Deployable antennas, particularly to achieve more highly focused beams and support much high-gain multi-beam antennas.
Phased array feed and phased array antennas for scanning and hopping beams.
Optical communications systems, which have been used for intersatellite links and interplanetary communications, and increasingly being considered for earth-to-space systems.
In general, there are many different types of antennas, but the one most commonly associated with satellite communications is the parabolic dish antenna. These dish antennas have a narrow beam width, concentrating the energy of the radiated main beam into a smaller solid angle. This means more of the radiated energy reaches, or “illuminates,” the satellite when using a dish antenna as compared to an omnidirectional, or “omni” for short, antenna. An example of dish antenna used on satellite is shown below in Figure 6 for a Ku-band space to ground antenna (SGANT) mounted on the external stowage platform of the International Space Station (ISS).
Example of a satellite dish antenna.
There are several factors driving the design and development of satellite antennas. These include the need to reuse frequency bands because of limited spectrum allocations; the need to have antennas that can operate at higher frequencies with higher bandwidth; and the desire to deploy higher gain antennas at the same time minimizing the required size, weight, and power (SWAP) constrains. In practice, there are substantially more SWAP constrains for satellite antennas than on the ground stations, and this results in several design trade-offs between the space and control/user segments.
For example, the GEO orbit allows a high gain antenna to be pointed at a satellite with a minimum of tracking. Thus, a large dish can be used and remain virtually stationary without tracking a satellite as it moves around in its orbit. On the other hand, a low earth orbit (LEO) satellite that can cross from horizon to horizon in a few seconds can result in ground antenna installations that can be quite complex and expensive. Consequently, trade-offs need to be made to support the mission parameters of the whole satellite network.
The term “command and data handling subsystem” (C&DHS) was referred to as “On-board Computer” (OBC), which is a legacy of the past in which many satellite functions were performed by analog circuits with the help of an OBC. With the current shift toward the digital domain, the term OBC does not fully cover the topic anymore thus C&DHS is being used instead. An appropriate analogy to describe the C&DHS subsystem is to regard it as the brain and nervous system of the spacecraft.
The function of a C&DHS subsystem is to perform onboard processing and operations and internal communication [3, 4]. The task of managing the operations of the spacecraft subsystems is nowadays performed mostly by software in an autonomous manner and is generally categorized as onboard operations. The software is also responsible for preparing the data to be downlinked and handling any commands that are received from satellite operators on the ground. Lastly, the C&DHS facilitates and controls all internal communications (consisting of commands, telemetry, and tracking data) between the different satellite subsystems. The basic functions of the C&DHS can be summarized below:
Receives commands from the command or user segment through the telemetry, tracking, and control (TT&C) subsystem.
Decodes, executes, and/or distributes those commands to/from the onboard computer.
Collects and formats telemetry data from all space vehicle (SV) units.
Distributes telemetry for downlinking. Provides a platform for bus flight software (FSW).
Additional functions include ranging processing for satellite tracking purpose, satellite timekeeping, computer health monitoring (watchdog), and security interfaces.
An overview of the architecture of C&DHS in a typical satellite is provided in Figure 7 below. In this figure, all components are connected to each other via a common low-speed data bus in red color, typically compliant with MIL-STD 1553 or other standards. Also shown is the data connection in blue from the C&DHS to other components, which is more customized and high-speed in nature depending on the design.
Block diagram of a typical command and data handling subsystem.
The heart of the system is the C&DHS’ onboard computer (or OBC) that runs the software responsible for managing the onboard operations. The OBC is tightly linked to the electrical power subsystem (EPS). The main reason is the importance of the available and consumed power for managing onboard spacecraft operations. For instance, by continuously querying the EPS on the available power, the OBC can decide to turn off non-critical subsystems to prevent vital systems from shutting down from lack of power. Secondly, the OBC must be able to command the EPS to disable or enable different subsystems throughout the various phases of the mission. Since the amount of transmitted data between these two subsystems is small, a low-speed data link is sufficient, although there is a new trend to incorporate high-speed standard link such as SpaceWire4 to satisfy increasing demand for data volume.
The OBC is also responsible for receiving, interpreting, and executing commands from ground operators via the radio receiver. Using low-speed radio transmitters, the OBC also sends packets of housekeeping data, or telemetry, to the ground station. The purpose of the housekeeping data is to give the operators on the ground an overview of the spacecraft health and its general condition.
Some small satellites only have a single low-speed transmitter, so the housekeeping and payload data are combined over the same link. For larger satellites with payloads capable of producing vast amounts of data, a dedicated high-speed data link is used to store the data on an onboard storage system. When the satellites pass over a ground station, the OBC commands the high-speed radio transmitter to retrieve and transmit the previously stored payload data through another dedicated high-speed link from the onboard storage system. This approach frees the OBC from having to process large amounts of data and allows it to devote its internal resources for time critical operations and communicates with the PL and all other subsystems through the low-speed data links. This would include the requirements to retrieve information on the health, perform critical interventions as well as to command these subsystems to perform various actions according to the operational arrangement of the mission.
The telemetry, tracking, and control (TT&C) subsystem of a satellite provides a connection between the satellite (space segment) and the ground facilities (control or user segment). The purpose of the TT&C function is to ensure the satellite performs correctly. As part of the satellite bus, the TT&C subsystem is required for all satellites regardless of the mission type. The TT&C subsystem has three specific tasks that must be performed to ensure a successful mission:
Telemetry: the collection, processing of health, and status data of all spacecraft subsystems, and the transmission of these data to the control segment on the ground. This requires not only a telemetry system on the spacecraft but also a global network of ground stations around the world, unless the satellite space network includes intersatellite links that can relay the data to designated satellite and downlink to the appropriate ground station. Figure 8 below illustrates the processing of telemetry data by the C&DHS. Here the different health information and status information sent from various subsystems are collected by the telemetry input interface, fed to the C&DHS processor, buffered, encrypted, and sent down to the ground station.
Tracking: the determination of the satellite’s exact location by the control segment and where it is going via the reception, processing, and transmitting of ranging signals. This requires a ranging system on the spacecraft and a data collection ground network for this tracking function to work.
Command and control: the reception and processing of commands for continuous operation of the satellite. Usually a ground system is required, although advanced spacecraft designs have evolved toward “autonomous operations” so that many of the control functions can be automated onboard and do not require ground intervention except under emergency conditions. A typical command processing scenario is illustrated in Figure 9 where serial command bit stream from the command receiver is received by the command input interface, where the relevant commands are extracted and sent to the appropriate subsystems via a serial or parallel interface.
Telemetry processing by C&DHS.
Command and control message processing by C&DHS.
For communications payload, the onboard switching systems are designed to make more efficient use of a satellite communication network, especially those that employ multi-beam technology that entails onboard switching to interconnect uplink and downlink beams with a high degree of efficiency.
Figure 10 below summarizes the functional block diagram of a channelized transponder processor assuming a digital implementation of the channelized transponder filtering and switching function. Any signal within the receiver bandwidth is down-converted to an intermediate frequency (IF) or baseband and digitally sampled. These samples are digitally filtered, stored, and routed to the switch port corresponding to the desired downlink beam. This routing is achieved by a simple readdressing of the stored digital samples within a common output buffer memory or by a more traditional digital switch implementation.
Channelized processor for communications payload.
For most sensing payload and as shown in Figure 4 above, the sensor analog data are collected onboard, digitized, buffered if necessary, and transmitted down to ground station for processing. This is due to the complexity of sensing mission data processing and the lack of onboard computational power to accomplish these tasks. An example of onboard PL processing for passive electro-optical (EO) remote sensing is shown in Figure 11 below, where the reflected light from earth is passing through a combination of optical lenses and charge coupled device5 (CCD) whose output is an analog signal that would be conditioned by analog filters before being digitized, compressed, and sent down via a mission data downlink to the ground station for processing. There, the data are decompressed, and image is enhanced by appropriate algorithms and displayed for users.
Onboard image processing for an EO application.
Typical data volume collected by sensing payload is large, and peak rates can produce data at much higher speeds than TT&C; thus, a separate downlink for mission data is needed. Depending on the system, this mission data downlink to a ground station can either be performed using a dedicated mission direct downlink, or indirectly via a relay broadband communications satellite. Sensing satellite can be positioned in GEO, MEO, or LEO orbits, and can have many possible mission data downlink architectures based on mission requirements. For example, a LEO sensing satellite can either buffer its mission data until within view of a dedicated ground station for downlink, or it can forward its mission data to a relay satellite that can ensure that the mission data can be downlinked to a designated ground station.
Another example of active remote sensing is a synthetic aperture radar (SAR) mission, where returned radar signals are collected onboard and sent to the ground to be correlated and form an image of the ground surface. This type of remote sensing does not heavily depend on sun light and other weather affects. Applications for SAR include agriculture, geology, geohazards, ice, oil spills, and flood monitoring. Several emerging applications such as forestry, ship detection, and others are possible [1]. An example of a SAR mission is the NASA-ISRO Synthetic Aperture Radar (NISAR) [5], which is a collaborative earth-science mission between NASA and the Indian Space Research Organization (ISRO). The sensing payload features an L-band SAR instrument and an S-band SAR instrument. The simultaneous dual-frequency radar system at peak rates will produce data at gigabit-per second speeds, which drives the data-volume requirements at a minimum of 35 Terabits per day of radar science data to the ground. This is a direct mission downlink system with three designated ground stations. The payload communication system uses a 70-cm high-gain antenna with two synchronized transmitters in a dual-polarization configuration with each transmitter providing 2.4 Gbps of coded data with an aggregate rate of 4.8 Gbps.
Traditional communications systems are designed for and constrained to a specific waveform(s) operating over predetermined frequencies, bandwidths, and signal modulation types. This paradigm works well when the requirements and constraints of the communication link and network protocol are well understood prior to design.
As a result, most radios in today’s world have very dedicated uses. A car key fob is designed only to unlock or lock your car door, while a smart phone radio connects to the Internet through various wireless communication protocols. Although these examples vary in complexity of the hardware, they both cannot operate outside the confines of their physical layer implementation. Consequently, RF hardware with a narrow focus is not suitable for applications with a broader communication scope.
A single software defined radio (SDR) with a flexible RF front-end combined with modern computing power can be used for the above applications plus more. In addition, a radio with a flexible hardware and software architecture can also lead to more innovation in the communications industry. Because of the rapid development nature of software, an engineer or researcher can experiment with novel ideas and SDR waveforms that would not be achievable with a traditional radio.
SDR in the satellite communications industry has become a growing trend, particularly in the commercial and defense industries. In the following section, an overview of SDR will be given and applications of SDR in satellite communications will be discussed.
Before going into SDR basics, some of the SDR advantages are [6]:
Interoperability: an SDR can seamlessly communicate with incompatible radios, or work as a bridge between them. For example, different branches of the military and law enforcement can use many incompatible radios, thus hindering communications during joint operations. A single multichannel SDR can work with all these different radios and provide interoperability.
Efficient use of resources under varying conditions: for example, a low-power waveform can be selected if the radio is running low on battery, while a high-throughput waveform can be used to quickly download a file. This flexibility is one of the first reasons why SDR became popular.
Opportunistic frequency reuse in SDR using cognitive radio6 (CR) technology: if the “owner” (or primary user) of a spectrum band is not using it, an SDR-CR can “borrow” the spectrum until the owner comes back. This technique has the potential to dramatically increase efficient use of radio frequency spectrum.
Reduced obsolescence: an SDR can be field upgraded to support the latest communications standards. This capability is especially important to radio with long life cycles such as those in satellite communications.
Lower cost: a single SDR can be adapted for use in multiple markets and for multiple applications. For example, a single radio can be sold to cell phone and automobile manufacturers to significantly reduce cost.
Research and development: SDR can be used to implement many different advanced waveforms, e.g., code division multiplexing access (CDMA) or orthogonal frequency division multiplexing (OFDM), for real-time performance analysis. Performance studies can be conducted much faster and often with higher fidelity than simulations.
On the other hand, some of the disadvantages for SDR are:
Cost is the most common argument against SDR. A single key fob is based on a very inexpensive ASIC7; however SDR is heavily reliant on FPGA,8 which is much more expensive. This is even more significant for high-volume, low-margin consumer products.
The second most common argument against SDR is increased power consumption with increased DSP complexity and higher mixed-signal/RF bandwidth. Power consumption in an FPGA or GPP for flexible signal processing can easily be 10 times higher than in ASIC. Also, wideband analog-to-digital converters (ADCs), digital-to-analog converters (DACs), and RF front-ends consume more power than their narrowband equivalents.
Increased time and cost to implement the radio: it can take much more engineering effort to develop software/firmware for multiple waveforms than for one, especially if it must be compliant with a military standard such as JTRS9.
Changing specifications and requirements: this usually happens when the SDR design must support not only a set of baseline waveforms but also anticipate additional waveforms.
Increased schedule risks: since SDR is still a relatively new technology, it is more difficult to anticipate schedule problems. Also, it is difficult to thoroughly test the radio in all the supported and anticipated modes.
Limited technical scope: SDR only addresses the physical layer and will require cooperation from upper layers for throughput improvements.
The general definition for a SDR is
A radio can be categorically separated into receivers and transmitters. For this section, the receiver implementation will be considered as it is generally more interesting and complex. A block diagram of an SDR receiver is shown below in Figure 12. The following sections will present the anatomy of the SDR that differentiates it from a traditionally designed radio.
A block diagram of an SDR.
The purpose of the RF front-end (RFFE) is to isolate the desired signal received by the antenna from interference signals. To achieve this, the signal of interest must be brought down to lower frequency for digital conversion while mitigating the side effects from filtering during the frequency conversion process. A flexible RFFE for SDR must be designed so that the frequency and bandwidth are controllable by software. Depending on the system requirements and the available RF component specifications, there are several ways to achieve this.
One of the most common RFFE designs for analog radios is the heterodyne receiver. A heterodyne receiver, shown in Figure 13 below, works by mixing down the received signal from its carrier frequency to a lower intermediate frequency (IF). The signal at IF can now be more conveniently filtered, amplified, and processed. A super-heterodyne receiver uses a fixed IF that is lower than the carrier frequency but higher than the signal bandwidth and often uses two stages of down conversion to reduce the filtering requirements at each stage.
Heterodyne receiver.
Another popular RF front-end architecture generally used for low-power applications is called zero-IF. A zero-IF receiver, shown in Figure 14 below, uses a single mixing stage with the local oscillator (LO) set directly to the desired carrier frequency to convert directly to baseband in-phase and quadrature signals. Because mixers tend to have high power consumption and only low-pass filters are required, the simpler zero-IF provides improved power efficiency over a heterodyne architecture. However, the zero-IF implementation is more susceptible to IQ imbalances of the in-phase and quadrature oscillators, which will produce anomalies in the signal constellation. LO leakage may also self-mix through the RF ports creating a large DC bias. Both issues can be corrected using digital signal processing.
Zero-IF receiver.
The analog-to-digital converter (ADC) is responsible for converting a continuous-time signal to a discrete-time one. To translate signals from the analog to digital domain, an ADC must perform two fundamental steps: sampling and quantization. Sampling is the process of reading voltages at discrete-time intervals. Quantization is the process of converting these voltage readings into binary outputs. ADC performance can be evaluated based on various parameters, such as: signal-to-noise ratio (SNR), dynamic range, bit resolution, sampling rate, and power dissipation. The ADC dictates the DSP limitations of the SDR. Generally, the sampling rate should be at least twice the desired bandwidth of your signal. The ADC should be chosen to match the capability of your processor and specifications of the signals of interest.
The two main functions of a digital front-end are sample rate conversion (SRC) and channelization. Once a signal has become digitally converted, the samples need to be further primed for digital processing. Operating the ADC at a fixed rate simplifies its clock generation; however, it may be necessary to convert the sampling rate to match the sampling rate required to demodulate certain waveforms. Most wireless signals generally operate with specific symbol or chip rates that are specified by their respective standard. Depending on the RFFE design and signal type, channelization may be required to select the channel of interest.
SRC represents a classic sampling theorem problem. Converting sampling rates can introduce undesirable effects such as aliasing, an effect that causes frequency components to overlap. SRC can be achieved digitally through the processes of decimation and interpolation. To mitigate aliasing, decimation is performed by using an anti-aliasing filter followed by subsampling, which is essentially removing samples at certain intervals. Interpolation is a method of calculating values to add values in between samples. Channelization works by using digital down conversion, the process of digitally mixing down a signal to baseband with a numerically controlled oscillator.
SDRs have an array of devices to choose from for the required DSP application, each with their own strengths and weaknesses. An SDR may integrate multiple processor types and partition the signal processing chain to optimize each processor. The following criteria should be considered when evaluating the various processor types: flexibility, modularity, and performance. The three digital hardware choices this section will consider are the general-purpose processor (GPP), digital signal processor (DSP), and the field programmable gate array (FPGA).
A GPP is the typical microprocessor designed to handle a wide variety of generic tasks that can be found in your everyday personal computer. They are generally designed to have large instruction sets and highly capable of implementing and performing complex arithmetic tasks such as modulation/demodulation, filtering, fixed/floating point math, and encoding/decoding. Some commonly used GPP architectures are x86/64 and Advanced RISC Machine (ARM). The advantage of using a GPP is the wide availability, flexibility, and ease of programmability. Several GPP-based SDRs, such as Universal Software Radio Peripheral (USRP) and the LimeSDR, operate by digitizing the baseband signal and performing the required digital signal processing on computers. These types of SDRs are popular among university researchers and hobbyists due to the relative ease of obtaining and developing their applications.
Because the GPP was designed with such a broad focus, latency, speed, and power efficiency may be a limiting factor depending on the application. Many wireless communication standards have strict real-time and large processing bandwidth requirements that most modern CPUs cannot meet due to processor architecture and operating system design. .
A DSP is a microprocessor optimized for digital signal processing applications with the ability to be programmed with high-level languages. Although a GPP can contain much of the same functionality, the DSP performs the same digital signal processing operations more quickly and efficiently due to its reduced instruction set computer (RISC) architecture and parallel processing. The reduced instruction set limits the essentials but contains optimizations for common DSP operations such as multiply accumulate (MAC), filtering, matrix operations, and fast Fourier transform (FFT). DSPs are commonly sold in two variants: optimized for power efficiency and optimized for performance; and are used in applications such as base stations and edge devices. Power consumption is also minimized by reducing the silicon footprint that would be in GPPs sophisticated cache and peripheral subsystems.
Although DSPs have been commonly deployed in the past decades, they serve as a middle ground between GPPs and FPGAs with regard to flexibility, performance and efficiency. Field-programmable gate array (FPGA) offers more parallelism, higher data rates, and better power efficiency than DSP, but is not well suited for control applications, such as implementing the network/protocol stack. This is due to the limited amount of memory in FPGA and for this reason it is often paired with GPP.
A FPGA is an array of programmable hardware logic blocks, such as general logic, memory, and multiplier blocks, that are wired together via a reconfigurable interconnect to generate an integrated circuit for several designs with the ability to quickly switch between configurations. FPGA configurations are programmed using hardware description language (HDL), which is also used for ASIC. Because a FPGA functionality is defined at the hardware level and can be implemented using parallelism, it can perform DSP algorithms at much higher rates than DSPs and GPPs. FPGA consumes more power and requires more space than ASICs but provides more programmability and flexibility than ASIC. A big consideration for using FPGAs for SDR is the domain knowledge requirement for developers. Developing on FPGAs can be time consuming and require an extensive understanding of the target hardware architecture.
When the system requirements exceed the capabilities of a singular processor type, a comprehensive solution may include a combination of the above processor types. A common processing architecture in the defense industry comprises of a FPGA, DSP, and GPP. In this paradigm, the FPGA is responsible for high data rate signal processing tasks, such as sampling and filtering, the DSP handles demodulation and protocol, and the GPP performs control-related tasks, such as the user interface and algorithmic processing. Implementing such a system can become a complex management task to coordinate the processing flow; however, the system can benefit greatly by optimizing overall performance based on the strength of each processor.
For space applications, SDR has unique challenges such as extreme radiation and temperature environment, autonomous operational requirements, limitations on size, weight and power (SWAP), and the need for reduced development time and increased reliability in agile prototyping. In this section, recent applications of software defined radio to satellite, as well as the current status of radiation-hardened SDR components, are presented.
Recognizing early on that a standard and open architecture is needed to encourage reuse and portability of software, NASA developed an open architecture specification for space and ground SDRs called the Space Telecommunications Radio System (STRS) [9]. From this standard, several compliant systems have been built and demonstrated in radios on the International Space Station (ISS) and several ground stations. It was also the intention of NASA that the STRS architecture should be used as baseline for many future NASA space communications technologies.
In a nutshell, the STRS standard consists of hardware, configurable hardware design, and software architectures with accompanying description, guidance, and requirements. The three main hardware functionalities are connected by the Hardware Interface Description10 (HID) and described and shown in Figure 15 below:
General processing module (GPM) consists of the general-purpose processor; appropriate memory; spacecraft bus (e.g., MILSTD-1553, Space Wire); interconnection bus (e.g., PCI); and the components to support the configuration of the radio.
Signal processing module (SPM) where signal processing is used to handle the transformation of digital signals into data packets. Its components include ASICs, FPGAs, DSPs, memory, and connection fabric/bus (e.g., PCI, flex-fabric).
RF module (RFM) handles the RF functionality to transmit/receive the appropriate digital signal. Its components include RF switches, digital-to-analog converter (DAC), analog-to-digital converter (ADC), diplexer, filters, low-noise amplifiers (LNAs), and power amplifiers (PAs).
NASA STRS’ three main hardware functionalities.
In STRS terminology, software includes source code, object code, executables, etc. implemented on a processor. As shown in Figure 16, the STRS software architecture uses three primary interfaces: the STRS APIs, STRS hardware abstraction layer11 (HAL) specification, and the Portable Operating System Interface12 (POSIX®). The STRS APIs provide the interfaces that allow applications to be instantiated and use platform services.
STRS software architecture layers.
Configurable hardware designs are the items and designs, such as hardware description language (HDL) source, loadable files, data tables, etc., implemented in a configurable hardware device such as a FPGA.
STRS encourages the development of applications that are modular, portable, reconfigurable, and reusable. The STRS software, configurable hardware design, metadata, documentation for STRS applications, STRS devices, and operating environments (OEs) are submitted to NASA STRS Application Repository to allow applications to be reused in the future with appropriate release agreements.
CubeSats13 are increasingly popular spacecraft platforms for mission-oriented experiments that can be accomplished via quick prototyping and launches [10, 11, 12]. This short development timeline is due to the use of commercial-off-the-shelf (COTS) technology that typically has limited resilience to the space environment. Therefore, CubeSat usage has largely been limited to experiments or applications where high availability is not the main objective.
In general, SDR technology will allow for on-orbit flexibility via reconfigurability of data management, protocols, multiple access methods, waveforms, and data protection. SDR processing requirements are inherently scaled to the application. The availability of modular, high-performance sequential and parallel processors that are resilient to radiation upsets allows the tailoring of hardware architectures to the application and to the CubeSat platform. This is especially suitable for missions that require the flexibility to support multiple TT&C and mission data from multiple satellites and ground stations [13, 14, 15].
Given the provided mission flexibility, implementing an SDR on a CubeSat could significantly increase the required processing capacity and thus the size, weight, power and cost (SWAP-C) of the SDR implementation. Consequently, most current CubeSat SDR design and implementation are still customized depending on the mission requirements. In [16], some of the current COTS SDR hardware and software platforms such as GomSpace, Ettus Research USRP, EPIQ Solutions, Lime Microsystems, FunCube, and RTL SDR are described and categorized in decreasing cost and mass to illustrate the heterogeneous nature of SDR in CubeSat applications. Also described are a number of space and ground segment systems built to be (or have been) launched using these COTS SDRs or components thereof. What would be needed is a standard for CubeSat SDR similar to NASA STRS to ensure that hardware and software reuse can be incorporated into future CubeSat developments.
A pioneering commercial application of SDR in space is the HawkEye 360 (HE360) system [17] that was launched on 3 December 2018. HE360 system consists of three identical spacecrafts and their primary payload is a SDR with custom RF front-end along with VHF Ku-band antennas. This Pathfinder mission14 was to enable onboard reception and geolocation of different types of terrestrial RF signals using signal processing technique to combine received data from all three payloads15.
One commercial application of this mission is the detection and geolocation of a maritime vessel’s automatic identification system (AIS), which broadcasts the locations generated by GPS-enabled receiver. The locations generated by AIS can be disabled or spoofed, therefore not reliable. Another application would be to allow regulators, telecommunications companies, and broadcasters to globally monitor spectrum usage and identify areas of interference. The system can also be used to help large area search and rescue operations by quickly locating activated emergency beacons.
The SDR developed for the Pathfinder payload consists of an embedded processor system and three baseband processors. The baseband processor was built around the Analog Devices 9361 (AD9361) System on Chip (SoC) product, which is a highly integrated RF transceiver that combines high-speed ADCs and DACs, RF amplifiers, filtering, switching plus more. The HE360 payload supported up to three receiver channels (one AD9361 per channel) that can be simultaneously processed on separate frequencies. In addition, the signal processing subsystem takes advantage of open-source software and firmware code to allow system development to proceed without knowing the final space hardware. GNURadio16 was selected for being a free and open-source toolkit for SDR and widely used in small space projects for ground software processing.
In space, most semiconductor electronic components are susceptible to radiation damage, thus radiation-hardened (or rad-hard) components are required and normally developed based on their COTS equivalents with variations in design and manufacturing17 to reduce the susceptibility to radiation. Consequently, rad-hard components tend to lag behind most recent COTS developments. Depending on mission requirements, rad-hard products are typically selected and tested using popular metrics such as total ionizing dose18 (TID), and single event effects19 (SEEs).
Per US DoD MIL-PRF-38535 J standard [18], an ideal integrated circuit for space applications is the qualified manufacturing line20 (QML) Class V with radiation hardness assurance21 (RHA) level identified in the part specification. From the perspective of payload designer and developer, only Class V is space quality and should be the main factor for selecting SDR hardware components.
The FPGA is perhaps the most important component of an SDR and has a long history for manufactured QML class V parts where rad-hard Xilinx and Actel (now Microsemi) FPGAs were studied [19]. Currently, Xilinx is the major player for space-qualified QML level V products used in actual payloads with many more devices under development. The rad-hard DSP products also follow the QML process, with Texas Instrument (TI) currently taking the lead for in-flight payloads with many offerings in space-qualified RF components in addition to DSP. Similarly, space-qualified GPP follows the same QML path as FPGA and DSP, and the current on-flight rad-hard GPPs based on the following architecture are [20].
RISC PowerPC: RAD750, RAD5500.
RISC MIPS: RH-32, Mongoose-V, KOMDIV-32.
Motorola 68,000 Series: Coldfire M5208
ARM Microcontroller: Vorago VA10820
In the first section of this chapter, an overview of the satellite bus and payload subsystems are presented for command and data handling subsystem (C&DHS); communications subsystem (CS); electrical power subsystem (EPS); propulsion subsystem (PS); thermal control subsystem (TCS); attitude control subsystem (ACS) also known as guidance, navigation and control (GNC) subsystem; and structures and mechanics subsystem (S&MS). A significant portion is spent on describing the C&DHS and CS with much details on how they are related to other satellite subsystems for continuous operation.
There are distinctive functional separations between the satellite bus and payload that are discussed at a high level with some examples given; however, there are currently no existing standard on their interfaces due to legacy satellite design and development. Examples were given for mission-specific sensing and communications payloads, showing that pretty much all mission payloads are very customized in design in legacy systems.
The second section of this chapter covers software defined radio (SDR) as a new technology with an overview and how SDR is being applied to satellite design and development in both space and ground segments. There has been a NASA standard for SDR that has been used for traditional and large satellites and shown to have some advantages over non-SDR approach.
However, recent rapid developments of Small Satellites (SmallSats), which CubeSat is a subset of, have resulted in an explosion of SDR applications to build Pathfinder missions that can lead to successful follow-on projects. There remains to be a standard to be defined for SDR for this CubeSat application. Regardless, SDR is providing a path forward to a common framework that may enable a more generic building block for a future concept called Software Defined Satellite that will change missions based on a software upload.
Since SDR is becoming an important part of a satellite, radiation hardening of the relevant SDR components is described in some detail. The area is evolving slowly despite fast changing technology due to the additional design and manufacturing steps taken to ensure minimum effects of radiation on microelectronics. The selection of the appropriate rad-hard FPGA, DSP, and GPP components should be an important factor in design trade-offs when SDR is being considered for future missions.
The first author, Dr. Hung H. Nguyen, would like to express bountiful appreciation for his wife, Thuy Le Nguyen, for her constant support during this effort.
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