Band gap energy (Eg) for PZTN, determined using the diffuse reflectance principle (Kubelka-Munk expression). Error Eg= ± 0.003 eV. ED values obtained with the Eg and more intense emission band at around 2.56 eV.
\\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
\n'}],latestNews:[{slug:"intechopen-partners-with-ehs-for-digital-advertising-representation-20210416",title:"IntechOpen Partners with EHS for Digital Advertising Representation"},{slug:"intechopen-signs-new-contract-with-cepiec-china-for-distribution-of-open-access-books-20210319",title:"IntechOpen Signs New Contract with CEPIEC, China for Distribution of Open Access Books"},{slug:"150-million-downloads-and-counting-20210316",title:"150 Million Downloads and Counting"},{slug:"intechopen-secures-indefinite-content-preservation-with-clockss-20210309",title:"IntechOpen Secures Indefinite Content Preservation with CLOCKSS"},{slug:"intechopen-expands-to-all-global-amazon-channels-with-full-catalog-of-books-20210308",title:"IntechOpen Expands to All Global Amazon Channels with Full Catalog of Books"},{slug:"stanford-university-identifies-top-2-scientists-over-1-000-are-intechopen-authors-and-editors-20210122",title:"Stanford University Identifies Top 2% Scientists, Over 1,000 are IntechOpen Authors and Editors"},{slug:"intechopen-authors-included-in-the-highly-cited-researchers-list-for-2020-20210121",title:"IntechOpen Authors Included in the Highly Cited Researchers List for 2020"},{slug:"intechopen-maintains-position-as-the-world-s-largest-oa-book-publisher-20201218",title:"IntechOpen Maintains Position as the World’s Largest OA Book Publisher"}]},book:{item:{type:"book",id:"2874",leadTitle:null,fullTitle:"Hydrogenation",title:"Hydrogenation",subtitle:null,reviewType:"peer-reviewed",abstract:"The domain of catalytic hydrogenation continues to grow fast, reflecting the wide range of chemical applications that can be enhanced by the easy use of molecular hydrogen. The advances in characterization techniques and their application have improved our understanding of the catalytic processes and mechanisms occurring in both homogeneous and heterogeneous catalysis.\r\nThe aim of this volume, although not exhaustive, is to provide a general overview of new progress of the hydrogenation reactions.\r\nThis volume comprises a series of various contributions, as reviews or original articles, treating heterogeneously and homogeneously catalyzed hydrogenation reactions. It is composed of three parts: hydrogenation reactions in fine organic chemistry, hydrogenation reactions in environmental chemistry and renewable energy, and special topics in hydrogenation.",isbn:null,printIsbn:"978-953-51-0785-9",pdfIsbn:"978-953-51-4272-0",doi:"10.5772/3208",price:139,priceEur:155,priceUsd:179,slug:"hydrogenation",numberOfPages:340,isOpenForSubmission:!1,isInWos:1,hash:"737b7439c2b3372d6c4b34ce28a37fe4",bookSignature:"Iyad Karamé",publishedDate:"October 10th 2012",coverURL:"https://cdn.intechopen.com/books/images_new/2874.jpg",numberOfDownloads:68435,numberOfWosCitations:179,numberOfCrossrefCitations:47,numberOfDimensionsCitations:122,hasAltmetrics:1,numberOfTotalCitations:348,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"November 29th 2011",dateEndSecondStepPublish:"December 20th 2011",dateEndThirdStepPublish:"March 25th 2012",dateEndFourthStepPublish:"June 23rd 2012",dateEndFifthStepPublish:"July 23rd 2012",currentStepOfPublishingProcess:5,indexedIn:"1,2,3,4,5,6,7,8",editedByType:"Edited by",kuFlag:!1,editors:[{id:"145512",title:"Prof.",name:"Iyad",middleName:null,surname:"Karamé",slug:"iyad-karame",fullName:"Iyad Karamé",profilePictureURL:"https://mts.intechopen.com/storage/users/145512/images/3352_n.jpg",biography:"Iyad Karamé, PhD.\nHe is a professor at the Faculty of sciences in the Lebanese University in Beirut. Director of the Organometallic Catalysis and Materials Laboratory, in the department of Chemistry. He got his PhD degree from Claude Bernard-Lyon 1 university in France in January 2004. He was an assistant professor and researcher (ATER) at the Ecole Normale Supérieure de Lyon, France, for one year (2004-2005). A researcher at the Leibniz Institut für Katalyse in Rostock (Germany) (2005-2006) and then at the Laboratory of Organometallic Chemistry of surface, CPE-Lyon till 2008. 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The photoluminescence (PL) it is a non thermal origin process, in that a chemical compound absorbs the photons (of the electromagnetic radiation), jumping to an electronic state of more energy, the inverse process happens and so call recombination (when passing to inferior energy level) and the materials radiating photons. The period between absorption and emission occur is in order to 10 nanoseconds. But under special circumstances, this period can extend in minutes or hours. The transition energy is determined by quantum mechanics rules. Different imperfection presents in the materials study will alter the recombination time or frequency.
\n\t\t\tSimpler PL processes are resonant radiations, in that a photon of a particular longitude wave is absorbed and an equivalent photon is emitted immediately. This process doesn\'t involve any transition in forbidden energy band and it is extremely quick (10 ns). The most interesting processes happen when the desexcitation energy transition is not direct at the basic level. The most common effect is the fluorescence that is also typically a quick process, but in that the original energy it is dissipated so that the slight photons emitted are of the lower energy that those absorbed. This phenomenon can happen for the isolated atoms, molecules or atoms and molecules in interaction excitement.
\n\t\t\tThe isolated atom excitement (making notice that a very rarefied gas can be considered as a group of isolated atoms) it drives to a spectrum of lines. The atom only absorb the frequency of the incident ray that corresponds to the allowed transitions (Figure 1). So all the isolated atoms can be luminescent.
\n\t\t\t\tThat happens for the isolated atoms is also valid for the isolated molecules, but the laws are more complicated due to the vibrations and rotations molecular than they introduce supplementary energy levels as the sample the following diagram of figure 2.
\n\t\t\t\tThe pressure of a gas it increases and a new transitions of excitement energy appear by collision, for the appearance of kinetic energy and metastable states. The return to the basic state is with a reduction of the yield of the luminescence and an expansion of the spectrum of the transmission. Then appears spectrum of band. The return to the fundamental state it doesn\'t always happen with light emission (transitions without radiation).
\n\t\t\t\tThree possible luminiscence types of an isolated atom: 1) direct transition, this is a resonance phenomenon; 2) indirect transition, distributing the energy in several photons hν1 and hν2, 3) indirect transition by a metastable state (M) following by interatomic collision (not very probable).
The luminescence of the crystalline bodies is due to the transmission centers (the activators). These centers are:
\n\t\t\t\tphysical imperfections in crystalline structure (vacancies, interstitial atoms, dislocations), this is intrinsic luminiscence.
Energy levels that appear in a molecule.
chemical imperfections (impurity atoms) in interstitial or substitution position, this is extrinsic luminiscence.
The mechanism of crystalline luminiscence it is explained with the help of energy bands diagram (Figure 3).
\n\t\t\t\tConsidering that in the perfect crystal any level doesn\'t exist in forbidden band, the presence of imperfection in the cystal introduces some levels allowed in the forbidden or in the allowed bands. These energy levels they can be:
\n\t\t\t\trecombinations levels (h/e -)
metastable levels: the traps of e- (Pe) or h (Pt)
fundamental (F) and excited levels (E) of isolated centers
The spectra of crystalline luminiscence differ notably of the atomic spectra for two fundamental aspects.:
\n\t\t\t\tbands are observed and
the emitted radiation appears toward the longitude of big waves, this can made a mistake with the absorbed radiation.
These two aspects are due to the interaction between the emission center and the crystalline lattice.
\n\t\t\t\tAccording to the type of imperfections there are the transitions way and therefore the energy of the transition.
\n\t\t\t\tA first transition consists on an electron that leaves a donor level and go toward the valency band. The energy of this transition is given for: E=Egap-Ed
\n\t\t\t\tAlso, can be observed where an electron leaves to the conduction band to pass at aceptor level. In this case, the energy of the transition is given for: E=Egap-EA
\n\t\t\t\tTypes of transitions among bands.
It is known that the energy ED and EA differ according to the chemical nature of the impurity. For this reason is allows to use the photoluminiscence experiments to confirm the presence of a specific type of impurity in a material.
\n\t\t\t\tIn many cases, the theory of the effective mass is a first valid approach, it predicts the value of the energy ED and EA for a given semiconductor.
\n\t\t\t\tIn general
Broad bands are observed for many optical transitions in the partly filled d-shell of transition metal ions (d - d transitions), but also for transitions between the 5d shell and the 4f shell of rare-earth ions (d - f transitions) and for emission on s2 ions (these ions possess a ‘‘lone pair’’ of s electrons), like Tl+, Pb2+, or Sb3+. Sharp emission bands are characteristic of optical transitions between electronic states with chemical bonding character (almost) the same for ground and excited state, and for the same reason also of optical transitions between electronic states that hardly participate in the chemical bonding (e.g., f - f transitions on rare-earth ions).
\n\t\t\t\tIn the case of optical processes involving electronic states which participate in the chemical bonding, the nature of the bonding (covalent, ionic) and the symmetry of the site at which the emitting ion is incorporated play a very important role. This is generally described by the ligand field theory, which we do not treat here.
\n\t\t\t\tThe emission generated reflects how the optical properties of the ion depend on its chemical environment. This luminescent material can be applied as green phosphor in very high-quality fluorescent lamps and also in plasma display (Ronda, 2008).
\n\t\t\tThe width of luminescent band usually observed at room temperatures in crystals of perovskite type it is associated with the presence of imperfections or defects (Haertling, 1999; Anicete-Santosaet al., 2007), be already oxygen or lead vacancies. But other author explain apparition of PL to order-disorder presence in the structure (Chen et al., 1989; Suárez-Gómez et al., 2009; Shannigrahi, 2007) distortion of oxygen octahedral fundamentally.
\n\t\t\tUndoped PZT ceramics are seldom used. They are usually substituted in the A or B-sites of the perovskite structure ABO3 in order to improve dielectric, piezoelectric and mechanical properties. For example La3+ and Nb5+ are used satisfactorily (Durruthy et al., 1999, 2002; Bharadwaja et al., 2002). The excess of positive charge in (La/Nb) doped PZT is compensated by lead vacancies and the typical Kröger-Vink notation to describe the electroneutrality, have been reported in many papers previously (Eyraud et al, 2006; Jaffe et al., 1954).
\n\t\t\tThe defects caused by the small dopant concentrations in A or B places of the structure could generate a combination of blue, green and red emission of light which is of great importance for optical devices applied in optoelectronics includes flat-screen, full-colour displays and compact laser devices operating in the blue region (Nakajima et al., 2004; Yang et al., 2008).
\n\t\t\tRecently M.S. Silva et. al., 2005, reported a theoretical and experimental result, and presents an alternative method to process PL in PZT and aim to explain why this phenomenon depends on the crystalline structure of the material. The wide bands at 2.1 and 2.67 eV respectively in PL emission in perovskite ceramics are associated to the oxygen vacancies provoked during the sintering process (Lines & Glass, 2001) or related to ensure electroneutrality process.
\n\t\t\tWhat happens with luminescence effect with A, B or A+B doped PZT?
\n\t\t\tWe will try to respond this question with several examples.
\n\t\t\tAll samples that show were prepared by a conventional processing method using mixed oxide powders. The photoluminescence (PL) spectra were obtained using a Jobin Yvon Horiba Fluoromax-3 spectrometer using the excitation band at 373 nm. The absorption spectra were acquired with an UV-vis Ocean Optics Spectrometer QE650000 using diffuse reflectance measurements the data was processed by using the Kubelka-Munk function:
\n\t\t\tR∞ = (I/I0) is diffuse reflectance at one wavelength from an opaque sample with infinite thickness (> 2 μm), 0< R∞<1, α is the absorbance in cm-1 and S is the scattering factor which is assumed to be independent of the wavelength for grain sizes greater than the wavelength of the light (Wendlandt & Hecht, 1966; Kottim, 1969).
\n\t\t\tCrystalline structure (Figure 4), like we will see later, influences in the shift energy of PL in the samples. For this reason it is advisable to carry out this study previously to PL analysis. All samples firth were identify by X-ray diffraction (XRD). The XRD patterns of the polycrystalline samples show the tetragonal (Zr/Ti = 20/80, 40/60) and rhombohedral (Zr/Ti = 60/40, 80/20) PZT phases, and both phase together for Zr/Ti = 53/47. This is a classical behavior for this material and has been reported by some authors (Jaffe et al., 1971; Noheda, 2000, 2001).
\n\t\t\tPhases diagram of PZT, appear the existence range of each phase (tetragonal and rhombohedral), the morfotrópica phase boundary (MPB) according to
In our samples doped the compensation of charge provokes in all cases oxygen vacancies that should increase with the dopant concentration or saturates in a composition that denotes a limit of solubility. However, oxygen vacancies are easily induced during the sintering process because the PbO has low volatile temperature of about 880ºC. This phenomenon takes place in all samples and also promotes lead and oxygen vacancies, which are quenched defects at low temperatures. Lead vacancies can only become mobile at high temperatures with high activation energy greater than oxygen mechanism values.
\n\t\t\tAccording to Eyraud et. al. (2006) singly and doubly ionized lead and oxygen vacancies coexist in the PZT ceramic, then they may constitute donor and acceptor sites which are able to exchange electrons according to the following reactions:
\n\t\t\tin our case at least three types of defects coexist\n\t\t\t\t\t
The results of first-principle calculation reported by Ghasemifard et al., (2009) show that the PZT polycrystalline has a direct band gap between the X and Γ points of 3.03 eV (Baedi et al., 2008), then by assuming a direct band gap we can calculate the values of the energy gap (Eg) for all the samples. In general calculating the absorption coefficients of the synthesized powder in the strong absorption region needs both, the transmission and reflection spectra. In our case, we obtained the absorption spectra by diffuse reflectance measurements, and by using the Kubelka-Munk equation for all samples the band gap energy Eg was determined.
\n\t\t\tThe substitution for La3+ in the A site of perovskite structure it’s traditional. It is one of the classic sustituyentes in this system.
\n\t\t\t\tThe emission spectra (PL) at 273, 325, 373, 413 and 457 nm were characterized to present different bands for PLZT 1-x/x/y (Figure 5), prevailing blue-violet band presence (2.4-2.75 eV), it’s appears at bigger intensity for 413 nm. This evidences that PL effect has the same origin in all cases.
\n\t\t\t\tAs it has been expressed previously, the energy of the spectra of PL demonstrates the presence of levels in the forbidden band. The calculations of first principles (Longo et al., 2007) have been demonstrated that disorder in perovskite structure and the defects in the same one, they cause states in the forbidden band. On the other hand the experimental evidence of the presence of defects exists (oxygen vacancies) (Mansimenko et al., 1998) starting from mensurations of resonance electronic paramagnética (RPE) in the system PLZT.
\n\t\t\t\tIf we consider to our materials as semiconductors of big gap, the presence of states in the forbidden band, what causes a contraction of the gap, is the causing of a well-known Burstein-Moss shift of emission spectrum (Yu & Cardona, 1996). It can associate to presence of picks around 2.65 eV to the presence of bands inside of forbiden band in the material, being more intensity when it’s excited with λ= 413 nm.
\n\t\t\t\tAnalyzing the results associating them with the colors corresponding of the wave longitudes, we see that emissions exist (although of different intensity) in almost the whole visible spectrum, from the red one until the ultra violet, but the bands of very high intensity correspond to the bands of the blue-violet and ultraviolet.
\n\t\t\t\tThe motive that causes this effect are similar when you doped these materials in B site, this will be explained in the next section.
\n\t\t\tIn perovskita structure (ABO3) N5+ substitute B site, occupied by Zr4+ and Ti4+ ion. The high volatility of lead oxide at elevated temperatures during the powder calcinations and the
\n\t\t\t\tPL spectra at room temperature, fixing the excitation band at 273, 325, 373, 413 and 457 nm in PLZT ferroelectric ceramics. Appear result for two point of PZT phase diagram doped at different La3+ concentration.
sintering stages in the PZT system is known, which provides both fully-ionized cationic lead \n\t\t\t\t\t\t
\n\t\t\t\t\tFigure 6 shows the PL spectra of PZTN samples for compositions 80/20, 60/40, 53/47, 40/60 and 20/80 which have diverse dopant concentrations. The emission bands (PL response) when fixing the excitation bands (EB) at 373, 457 and 325 nm were observed in three regions: one is at around 1.72 eV (lowest energy region); the second is at around 2.56 – 2.61 eV which shows a higher intensity, and the third is at around 3.35 – 3.45 eV (highest energy region) respectively. The band at 2.56 eV is the most intense and narrow, and the band at 3.35 eV shows greater broadening. The band at 1.72 eV did not show any notable shift in the maximum position peaks for different compositions or dopant concentrations. Nevertheless, the bands at 2.56 and 3.35 eV show a shift in the maximum peak position which depending if the phase is rhombohedral or tetragonal will shift to 2.61 and 3.45 eV, respectively.
\n\t\t\t\tRoom temperature PL for PZTN note the dispersion for non doped materials. For PLZT 1-x/x/1.0 practically all the curves coincide for the same energy 1.72 and 3.36 for λ= 373 and 325 respectively.
Note that in the PZT polycrystalline samples without Nb, the three well resolved emission bands were also shown, in contrast with other reports (Longo et al., 2008; Chang et al., 2001) where the emission for polycrystalline PZT is very low and broad or absent. For these materials (PZTN) the emission is bigger in 1 or 2 order than PLZT. The PLE spectra for samples doped and without doped they present same character, appearing the same line, for what they have the same origin in both cases (Figure 7).
\n\t\t\t\tThe Eg (in PZTN) values for tetragonal samples 20/80 and 40/60 are between 2.80 to 2.98 eV, the composition 53/47 are near the morphotropic phase boundary which shows a higher variation in Eg, values as a function of the dopant concentration from 2.70 to 3.19 eV. For this composition and rhombohedral phases 60/40 and 80/20 the behavior of Eg values as a function of Nb concentration shows a minimum at 0.8% with values of approximately 2.67 to 2.70 eV. In our case, experimentally it is observed a transition (EPL) at 2.56 eV for samples PZTN 80/20/0.0.
\n\t\t\t\tSintering stages in the PZT system is known, which provides both fully-ionized cationic lead \n\t\t\t\t\t\t
Room temperature excitation spectra PLE for PZTN for an emission at 475 and 715 nm respectively.
The ED values reported in Table 2 were calculated using Eg and EPL obtained by excitation at EB=457 nm. Even the origins of these luminescence bands are not clearly understood. Figure 8 shows a schematic diagram to represent the recombination process for the three emission bands. The PL at a high energy region of approximately 3.35-3.45 eV, that overcomes the Eg, which is obtained when the excitation is at 3.81 eV.
\n\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t|||||||||
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t||||||
Eg | \n\t\t\t\t\t\t\tED\n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tEg | \n\t\t\t\t\t\t\tED\n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tEg | \n\t\t\t\t\t\t\tED\n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tEg | \n\t\t\t\t\t\t\tED\n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tEg | \n\t\t\t\t\t\t\tED\n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t|
0.0 | \n\t\t\t\t\t\t\t2.80 | \n\t\t\t\t\t\t\t0.19 | \n\t\t\t\t\t\t\t2.92 | \n\t\t\t\t\t\t\t0.31 | \n\t\t\t\t\t\t\t3.19 | \n\t\t\t\t\t\t\t0.63 | \n\t\t\t\t\t\t\t3.04 | \n\t\t\t\t\t\t\t0.48 | \n\t\t\t\t\t\t\t3.09 | \n\t\t\t\t\t\t\t0.53 | \n\t\t\t\t\t\t
0.2 | \n\t\t\t\t\t\t\t2.84 | \n\t\t\t\t\t\t\t0.23 | \n\t\t\t\t\t\t\t2.86 | \n\t\t\t\t\t\t\t0.25 | \n\t\t\t\t\t\t\t2.93 | \n\t\t\t\t\t\t\t0.37 | \n\t\t\t\t\t\t\t3.04 | \n\t\t\t\t\t\t\t0.48 | \n\t\t\t\t\t\t\t3.04 | \n\t\t\t\t\t\t\t0.48 | \n\t\t\t\t\t\t
0.4 | \n\t\t\t\t\t\t\t2.84 | \n\t\t\t\t\t\t\t0.23 | \n\t\t\t\t\t\t\t2.84 | \n\t\t\t\t\t\t\t0.23 | \n\t\t\t\t\t\t\t2.90 | \n\t\t\t\t\t\t\t0.34 | \n\t\t\t\t\t\t\t2.92 | \n\t\t\t\t\t\t\t0.36 | \n\t\t\t\t\t\t\t2.96 | \n\t\t\t\t\t\t\t0.40 | \n\t\t\t\t\t\t
0.6 | \n\t\t\t\t\t\t\t2.82 | \n\t\t\t\t\t\t\t0.21 | \n\t\t\t\t\t\t\t2.86 | \n\t\t\t\t\t\t\t0.25 | \n\t\t\t\t\t\t\t2.85 | \n\t\t\t\t\t\t\t0.29 | \n\t\t\t\t\t\t\t2.85 | \n\t\t\t\t\t\t\t0.29 | \n\t\t\t\t\t\t\t2.85 | \n\t\t\t\t\t\t\t0.29 | \n\t\t\t\t\t\t
0.8 | \n\t\t\t\t\t\t\t2.87 | \n\t\t\t\t\t\t\t0.26 | \n\t\t\t\t\t\t\t2.80 | \n\t\t\t\t\t\t\t0.19 | \n\t\t\t\t\t\t\t2.70 | \n\t\t\t\t\t\t\t0.14 | \n\t\t\t\t\t\t\t2.67 | \n\t\t\t\t\t\t\t0.11 | \n\t\t\t\t\t\t\t2.67 | \n\t\t\t\t\t\t\t0.11 | \n\t\t\t\t\t\t
1.0 | \n\t\t\t\t\t\t\t2.90 | \n\t\t\t\t\t\t\t0.29 | \n\t\t\t\t\t\t\t2.98 | \n\t\t\t\t\t\t\t0.37 | \n\t\t\t\t\t\t\t3.00 | \n\t\t\t\t\t\t\t0.44 | \n\t\t\t\t\t\t\t2.95 | \n\t\t\t\t\t\t\t0.39 | \n\t\t\t\t\t\t\t2.94 | \n\t\t\t\t\t\t\t0.38 | \n\t\t\t\t\t\t
Band gap energy (Eg) for PZTN, determined using the diffuse reflectance principle (Kubelka-Munk expression). Error Eg= ± 0.003 eV. ED values obtained with the Eg and more intense emission band at around 2.56 eV.
This corresponds to transitions between higher energy states in the conduction band to the valence band (hot luminescence), and the emission intensity shows a strong dependence on the Nb concentration.
\n\t\t\t\tThe PL at 1.73 eV, the lowest energy region which is obtained with excitation energy of 3.32 eV, it could be follows a recombination mechanism:
\n\t\t\t\tfrom the localized states due to oxygen vacancies below the conduction band (\n\t\t\t\t\t\t\t\t
by recombination from band conduction to the localized states above the valence band due to lead vacancies (\n\t\t\t\t\t\t\t\t
The intensity emission of this band also shows a strong dependence on Nb concentration, and is present in all compositions indicating common defect types related to a deep level inside the band gap. In general, the incorporation of Nb5+ increases the PL intensity in this region due to the compensation of charge and induced defects (\n\t\t\t\t\t\t
In this case the simultaneous disorder of lead and oxygen vacancies should be created during the sintering process. The PL at 2.56 eV, which shows the highest intensity in all PZTN compositions and is associated to a transition between a shallow defect in the band gap and the valence band, see Figure 8. These levels are associated to oxygen vacancies, with simple or double ionization which is in accordance with the classification of Longo et al., (2008), vacancies bonded to clusters of TiO5 in disordered regions. In principle, the incorporation of Nb5+ in PZT samples would be producing more lead vacancies than oxygen vacancies. However, the higher intensities observed for peaks at 2.56 eV rather than peaks at around 1.73 eV is an indication that the oxygen vacancy concentration is higher than lead vacancies.
\n\t\t\t\tSchematic diagram of recombination process associated with the emission bands in PZTN ceramics, for excitation energy 3.79, 3.31 and 2.71 eV.
We will present results of double substitution in place A and B for “hard” and “soft” well-known ceramic. For “hard” ceramics present Sr2+ + Cr3+ doped PZT ceramics and for “soft” ceramics present La3+ + Nb5+ doped PZT ceramic.
\n\t\t\t\tWe will only present the behavior in the PZT morphotropic phase boundary region of phase diagram (Zr/Ti=53/47).
\n\t\t\t\tIn both type of samples (hard and soft) only appear two regions of emission bands, one at around 1.86 eV and other with higher intensity at around 3.00 eV when fixing the excitation band at 373 nm (3.4 eV) (Figure 9). Also, it is possible to observe emission band around 2.5-2.7, to a lot of smaller intensity. When fixing the excitation band at 412 nm (3.01 eV) only appear one signal wide at 3.28-3.31 eV (Figure 10).
\n\t\t\t\tPL show in the high energy region, the maximum position is around 3.00 eV for all composition, but the emission band is a broad band composed by two bands, at 2.98eV (414nm) and 3.03eV (408 nm) (Figure 9). PL lower energy region for PSZTC and PLZTN samples show the band at 1.87 eV (659 nm), additionally is observed that band at 1.74 eV is not present in all compositions and its intensity is reduced appreciably with the incorporation of Cr (Durruthy et al, 2010a,b, 2011).
\n\t\t\t\tThe general effect of the Cr doping is a decrement the PL intensity in both region bands with the increase of dopant. It is noted that the PL of doped La3+ and Nb5+ is larger than of undoped samples and increased with the composition of both ions at least one order of magnitude for PSZTC, but is two and three order to PZTN and PLZT respectively.
\n\t\t\t\tIt was of waiting that doped La3+ and Nb5+ increase PL intensity in 1.87 eV (659 nm) in PL, it is well known that is associated with lead vacancies, due to the compensation of charge, in this case the disorder or lead vacancy should be associated to the substitution of La3+ by Pb2+ in the host structure and the typical presence of lead vacancy due to the sintering route (Calderón-Piñar et al, 2007; Silva et al., 2005). The presence of the peak at 1.87 eV, in PSZTC 0.2-0.5 mol % and PLZTN 1 mol% indicates a common defect related with a deep level inside the band gap. As we saw in the region of high energy (3.00 eV) results are similar to showed above previously.
\n\t\t\t\tThe peaks that appear in zone (2.65) was associated with oxygen vacancies, simple or double ionized. In the sample PLZTN evidently that ED will be ≥ 0.54 eV, and EPL is lower 2.43-2.74. This is because ED is not exactly one unique value because there are a distribution defects in the structure.
\n\t\t\t\tThe analysis of the peak at 1.86 eV could be associated to the simultaneous presence of oxygen and lead vacancies (Guiffard et al, 2005; Durruthy et al, 2010a\n\t\t\t\t\t, b, 2011). The PL response in the donor-acceptor mechanism in this case between the levels associated to the oxygen near and below conduction band and the level of lead vacancies above the valence band. Analogously the theoretical quantum mechanical calculation reported by de Lazaro et al. (2007) justify that the presence of disorder associated to the substitution of Zr/Ti or displacement of the ions in the B sites produce an amorphous zone in the ceramic with a direct band gap with a separation near to 1.87eV. Beside this, we are detecting some small peaks whose energy is around of 2.00-2.80 eV which belong to the visible energy spectra too (Figure 9).
\n\t\t\t\tThe calculated results of the band gap values for the PSZTC samples sintered at 1250 ºC are summarized in Table 2. The figure 11 allows us to affirm that the dependence with Zr/Ti ratio is very strong, and has a maximum in the morphotropic phase boundary and the lowest values are for the composition 80/20, this behavior coincides with the calculations carried out by J. Baedi et al. (2008). Figure 12 shows the way that would be materialize recombination in the PSZTC and PLZTN samples. We supposed that the main way was 1, 5 and 6 for the experimental results obtained, in this work.
\n\t\t\t\tRoom temperature PL emission spectra for PSZTC and PLZTN ceramics at different dopant concentration, fixing exited band at 373 nm.
PL emission spectra at room temperature for PSZTC fixing exciting at 412 nm.
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t||
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tEgap\n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t\tEgap\n\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
0.0 | \n\t\t\t\t\t\t\t3.25 | \n\t\t\t\t\t\t\t0.0 | \n\t\t\t\t\t\t\t3.15 | \n\t\t\t\t\t\t
0.1 | \n\t\t\t\t\t\t\t3.33 | \n\t\t\t\t\t\t\t0.2 | \n\t\t\t\t\t\t\t- | \n\t\t\t\t\t\t
0.2 | \n\t\t\t\t\t\t\t3.35 | \n\t\t\t\t\t\t\t0.4 | \n\t\t\t\t\t\t\t2.88 | \n\t\t\t\t\t\t
0.3 | \n\t\t\t\t\t\t\t3.36 | \n\t\t\t\t\t\t\t0.6 | \n\t\t\t\t\t\t\t2.91 | \n\t\t\t\t\t\t
0.4 | \n\t\t\t\t\t\t\t3.36 | \n\t\t\t\t\t\t\t0.8 | \n\t\t\t\t\t\t\t3.07 | \n\t\t\t\t\t\t
0.5 | \n\t\t\t\t\t\t\t3.32 | \n\t\t\t\t\t\t\t1.0 | \n\t\t\t\t\t\t\t2.50 | \n\t\t\t\t\t\t
Band gap energy (Eg) for PZT soft and hard, determined using the diffuse reflectance principle (Kubelka-Munk expression). Error Eg= ± 0.003 eV. For EPL supposed ED=0.54.
Behavior of the forbidden band energy for PSZTC and PZTN ceramics, which agrees with the results obtained for J.
Possible energetic process that will be happen in PZT ceramics. 3.4 eV is excitation energy (373 nm), 1-6 there are the possible recombination way (PL). We consider that occurred the way 1, 5 and 6 mainly.
Another characteristics of these materials that they are very affected by the presence of oxygen vacancies there are dielectric (ε) and loss (tan δ), for this we present some results in different substitution type in ABO3 perovskite structure.
\n\t\t\tThe dielectric curves reveal anomalies in the neighbor at transition temperatures corresponding to FR(HT) – PC (TC) and FT – PC (TF-P) phase transitions. Strong influence of dopant La, Nb and La+Nb on the phase transition temperature (TC) is confirmed. The comparison of ε(T) curves, obtained for the ceramic samples is shown in Figure 13, dielectric measurement shows a decreasing TC and TF-P when increasing the dopant concentration. The dielectric permittivity decreases for dopant concentration larger than 0.8 mol% (Figure 13), in particularity in Nb-doped ceramics permittivity decreases for concentrations up to about 0.8 mol %, and then it increases slightly, as the grain size behaves. The same as in PL, the permittivity is more intense for substitutions in B and A+B, in this case it is 4 times.
\n\t\t\tThere is good agreement between the transition temperatures obtained from ε and tgδ, respectively, considering the range of measurement error (δt ~ 5 °C), for almost every sample. Those compositions with 0.6 and 1.0 % La have T tgδmax at 50 kHz differing 7.3-8.2 oC from the value obtained at 1 kHz. A possible cause of such differs is the presence of inhomogeneities as a result of compositional fluctuations (Gupta & Viehland, 1998; Garcia et al., 2001).
\n\t\t\tIn those samples doped with La+Nb, there is not a sum of the separate effects of La and Nb. Note that temperatures are not as low as those for Nb, but compared to those for La they are 50 °C below.
\n\t\t\tPermitivity as a function of temperature, measured at various frequencies, for PZT 53/47 ceramics showing La2O3, Nb2O5, and Nb2O5+La2O3 content.
Grain size decrement implies domain size decrement (Figure 14). Thus, the domain walls become more movable, so the mechanical friction is small, and then the samples doped with Nb and La+Nb are more compositionally homogenous (the evidence is given by narrow plots of dielectric permittivity vs. temperature, that is, increasing permittivity). On the other hand, grain size increment contributes to higher values of the dielectric constant, as a measurement of the number of polarized unitary cells. The amount of polarization of such cells is related to the presence of Nb5+ and La3+ inside the cristalline structure and contributes to the orientation of the domain walls. An increasing dopant concentration produces the increment of the number of lead vacancies and so the dielectric permittivity grows. The values of ε for PZTN samples are higher and attributed to the higher compositional homogeneity and the existence of only one phase in this composition. But is not the same for PLZTN and PLZT, XRD patterns of samples show the tetragonal and rhombohedral PZT phases together. (Figure 15) in all doped samples, with concentration near to MPB (53/47).
\n\t\t\tDecrements of Tc might be attributed to the integration of dopants into the cristalline structure.
\n\t\t\tSEM results for 0.6, 0.8 and 1.0 mol % dopant in study for samples near to MPB. In every case, the decrement of grain size as the dopant concentration increases is observed.
Room temperature DRX patterns for PZT, PLZT, PZTN and PLZTN 53/47/1.0 sinter ceramics. Note for PZTN there are more tetragonal phase, observe better resolution of 002/200 plane.
To determine the factor most influential in dielectric permittivity behaviour with the dopant concentration, the influence of porosity was analyzed. As it was seen in Table 3 it varies in an appreciable way (~ 14%) in the studied composition interval.
\n\t\t\tAmong the models proposed to evaluate the properties of porous materials, applicable to systems with inferior porosity values at 0.6, it (the model) stands out the Bruggeman model. This model offers a satisfactory description of the properties of piezoelectric porous ceramic, in particular those based on PZT. A detailed explanation can it turns in works from Wersing et al (1986).
\n\t\t\tThe model establishes a peculiar relationship between experimental permittivity [ε(p0)] and the theoretical [εpo=0], through of porosity fraction (p0) given by the equation (5), considering connectivity (3-0).
\n\t\t\t\n\t\t\t\tTable 3 shows the results for the dielectric permittivity theoretical and experimental at room temperature. A marked difference exists among both, being bigger for the Nb and the La+Nb, what indicates the influence of this impurity in the evolution of the porosity, also Δε to diminish with the frequency
\n\t\t\tNiobio | \n\t\t\t\t\t||||||
Frecuencia kHz | \n\t\t\t\t\t\t0,2 | \n\t\t\t\t\t\t1,0 | \n\t\t\t\t\t||||
ε(Po) | \n\t\t\t\t\t\tεPo=0\n\t\t\t\t\t\t | \n\t\t\t\t\t\tΔε | \n\t\t\t\t\t\tε(Po) | \n\t\t\t\t\t\tεPo=0\n\t\t\t\t\t\t | \n\t\t\t\t\t\tΔε | \n\t\t\t\t\t|
0,5 | \n\t\t\t\t\t\t830 | \n\t\t\t\t\t\t1249 | \n\t\t\t\t\t\t419 | \n\t\t\t\t\t\t1373 | \n\t\t\t\t\t\t1669 | \n\t\t\t\t\t\t296 | \n\t\t\t\t\t
1 | \n\t\t\t\t\t\t635 | \n\t\t\t\t\t\t955 | \n\t\t\t\t\t\t320 | \n\t\t\t\t\t\t1335 | \n\t\t\t\t\t\t1646 | \n\t\t\t\t\t\t292 | \n\t\t\t\t\t
5 | \n\t\t\t\t\t\t587 | \n\t\t\t\t\t\t883 | \n\t\t\t\t\t\t296 | \n\t\t\t\t\t\t1307 | \n\t\t\t\t\t\t1589 | \n\t\t\t\t\t\t282 | \n\t\t\t\t\t
10 | \n\t\t\t\t\t\t482 | \n\t\t\t\t\t\t725 | \n\t\t\t\t\t\t243 | \n\t\t\t\t\t\t1297 | \n\t\t\t\t\t\t1577 | \n\t\t\t\t\t\t280 | \n\t\t\t\t\t
25 | \n\t\t\t\t\t\t251 | \n\t\t\t\t\t\t378 | \n\t\t\t\t\t\t127 | \n\t\t\t\t\t\t1269 | \n\t\t\t\t\t\t1543 | \n\t\t\t\t\t\t274 | \n\t\t\t\t\t
Lantano | \n\t\t\t\t\t||||||
\n\t\t\t\t\t\t | 0,6 | \n\t\t\t\t\t\t1,0 | \n\t\t\t\t\t||||
0,5 | \n\t\t\t\t\t\t343 | \n\t\t\t\t\t\t395 | \n\t\t\t\t\t\t52 | \n\t\t\t\t\t\t566 | \n\t\t\t\t\t\t658 | \n\t\t\t\t\t\t92 | \n\t\t\t\t\t
1 | \n\t\t\t\t\t\t286 | \n\t\t\t\t\t\t329 | \n\t\t\t\t\t\t43 | \n\t\t\t\t\t\t549 | \n\t\t\t\t\t\t638 | \n\t\t\t\t\t\t89 | \n\t\t\t\t\t
5 | \n\t\t\t\t\t\t155 | \n\t\t\t\t\t\t180 | \n\t\t\t\t\t\t25 | \n\t\t\t\t\t\t425 | \n\t\t\t\t\t\t494 | \n\t\t\t\t\t\t69 | \n\t\t\t\t\t
10 | \n\t\t\t\t\t\t128 | \n\t\t\t\t\t\t148 | \n\t\t\t\t\t\t20 | \n\t\t\t\t\t\t304 | \n\t\t\t\t\t\t354 | \n\t\t\t\t\t\t50 | \n\t\t\t\t\t
25 | \n\t\t\t\t\t\t109 | \n\t\t\t\t\t\t126 | \n\t\t\t\t\t\t17 | \n\t\t\t\t\t\t160 | \n\t\t\t\t\t\t186 | \n\t\t\t\t\t\t26 | \n\t\t\t\t\t
Lantano+Niobio | \n\t\t\t\t\t||||||
\n\t\t\t\t\t\t | 0,4 | \n\t\t\t\t\t\t1,0 | \n\t\t\t\t\t||||
0,5 | \n\t\t\t\t\t\t343 | \n\t\t\t\t\t\t588 | \n\t\t\t\t\t\t245 | \n\t\t\t\t\t\t784 | \n\t\t\t\t\t\t1035 | \n\t\t\t\t\t\t251 | \n\t\t\t\t\t
1 | \n\t\t\t\t\t\t286 | \n\t\t\t\t\t\t491 | \n\t\t\t\t\t\t205 | \n\t\t\t\t\t\t768 | \n\t\t\t\t\t\t1015 | \n\t\t\t\t\t\t247 | \n\t\t\t\t\t
5 | \n\t\t\t\t\t\t155 | \n\t\t\t\t\t\t204 | \n\t\t\t\t\t\t49 | \n\t\t\t\t\t\t734 | \n\t\t\t\t\t\t970 | \n\t\t\t\t\t\t236 | \n\t\t\t\t\t
10 | \n\t\t\t\t\t\t128 | \n\t\t\t\t\t\t220 | \n\t\t\t\t\t\t92 | \n\t\t\t\t\t\t710 | \n\t\t\t\t\t\t934 | \n\t\t\t\t\t\t224 | \n\t\t\t\t\t
25 | \n\t\t\t\t\t\t109 | \n\t\t\t\t\t\t187 | \n\t\t\t\t\t\t78 | \n\t\t\t\t\t\t654 | \n\t\t\t\t\t\t864 | \n\t\t\t\t\t\t210 | \n\t\t\t\t\t
Theoretical and experimental permittivity and their difference at room temperature for 5 frequencies, for PZTN, PLZT and PLZTN 53/47/y ceramic, based on the Bruggeman model.
It is important to make notice that this model considers a materials as a not homogeneous médium and it start with two components: material and pores. In the material component there are all that is not pore, that doesn\'t have to be necessarily homogeneous, due to the procedure method.
\n\t\t\tThe porosity is not the only factor that determines the permittivity variation with dopant concentration. The analysis for dopant type shows that to smaller concentration bigger porosity, but also bigger grain size, therefore is this last one the most influential in the variations of the dielectric parameter. For example, 0.6% of Nb, the smallest difference exists among the theoretical and experimental results, and the porosity has the fundamental rol, for this concentration "po" it is minimized; in the other concentrations exists a cooperative effect of the porosity and the grain size (Sundar et al. 1996), noted how for 1.0% "po" slightly increases the grain size and Δε (Table 3). In La3+ case, Δε diminishes with the frequency and increases with dopant concentration (Table 3), but ε is increasing with grain size decrement, therefore both factors will contribute in a cooperative way in the relative permittivity (Figure 16). The samples doped with La+Nb have a grain size between 1 and 2 microns, in addition the contribution of the porosity is strong in the behavior of dielectric permittivity, being greater even for the composition 0.8. The factors that determined the variation of the permittivity with increasing dopant concentration are the grain size (Cancarevic et al., 2006) and porosity, fundamentally.
\n\t\t\tBehavior at room temperature of dielectric constant () and porosity (po) as function of the grain size.
The used of PL and diffuse reflectance measurement in polycrystalline ceramics to determine the band gap and the mechanism of the recombination in samples is possible. The experimental results agree with those calculated.
\n\t\t\tAll system present show mainly two region of emission bands around 1.8 and 3 eV, the presence of broad band (1.8 eV) at the band gap can be associated to the vacancy defect common in all (containing lead) ceramics sintered at high temperatures, the emission at around 3eV correspond to direct recombination from CB to VB.
\n\t\t\tThe emission at 2.56 eV, this present but it is not very intense in all the analyzed materials. Shows the highest intensity and a shift to higher energies in the tetragonal phases. The Nb concentration produces appreciably intensity changes and is associated to a transition from oxygen vacancy levels to valence band. PZTN presents the biggest intensity in this band, what indicates that the oxygen vacancy concentration is higher than lead vacancies.
\n\t\t\tBut not all the dopant has same behavior, in all zone of PL spectra Cr diminish PL intensity with increase concentration, while La3+, Nb5+ and La3++Nb5+ increase PL intensity with the increase dopant concentration.
\n\t\t\tAnother interesting aspect is that A+B doped produces an increment to 2-3 order in PL intensity, principally for “soft” doped.
\n\t\t\tOn the other hand, a strong influence of dopants on the decrement of grain size as concentration grows is observed. The substitution in the A place and the simultaneous substitutions in the A and B places provokes mixture of (tetragonal and rombohedral) phases, while substitution in the B place the structure is tetragonal at least in 95 %. A texture effect is also noticed, as it grows with the dopant concentration.
\n\t\t\tXRD results are confirmed by the obtained dielectric characteristics. In the PLZT, PLZTN and PSZTC samples which present phase mixture, two peaks in the 1/ε curves are observed and associated to Ferro-Ferro (rombohedral-tetragonal) and Ferro-Para (tetragonal-cubic) phase transitions. Substitutions in the B place contribute more significantly to the Curie temperature drop, with a minimum for PZTN 0.8 %.
\n\t\tThis work was supported by project PNCB 10/04, Cuba, Sabbatical program CONACYT, Mexico. The author appreciate work of Ing. M. Hernandez, Ing. F. Melgarejo, Ing. M. Landaverde and Ing. E. Urbina. And to Cybernetic, Mathematical and Physics Instituted.
\n\t\tGlycerine, also called glycerol (propane-1,2,3-triol, C3H8O3), occurs as the backbone in triglycerides which are the main constituents of all vegetable and animal fats and oils. It is colorless and odorless, has sweet taste, and is very viscous and hygroscopic [1, 2]. Glycerol is a key ingredient in personal care product due to its property of acting as humectants, solvents, moisturizer, as well as an additive to make coatings. Glycerol is currently produced from biodiesel transesterification, saponification, and hydrolysis processes in fatty acid and soap production [3]. Among these, biodiesel transesterification is the biggest crude glycerol generation sector, contributing up to 67% of the total crude glycerol production, followed by high pressure splitting (17%) and soap production (<10%) [4].
Due to the growing biodiesel demand as substitution to petroleum-based diesel, the production of crude glycerol as by-product from this process is also increased. For every 1 ton of biodiesel produced, approximately 100 kg of glycerol will be generated [5]. The crude glycerol generated contains many impurities such as methanol, organic and inorganic salts, water, unreacted triglycerides, soap, fatty acid, etc. Hence, for large-scale biodiesel manufacturers, the plants are normally equipped with crude glycerol refining facilities to produce glycerol with purities up to 95.5 and 99% [3].
Generally, there are three types of glycerol, namely, crude glycerine, technical grade glycerine, and refined glycerine. The process of refining glycerine is a complex process which involves distillation, bleaching, acidification, and several intermediate steps. In the distillation step, refined glycerine is obtained from the side draw of the distillation column and then subsequently bleached and deodorized to achieve the refined grade. Technical grade glycerine, also called yellow glycerine, is obtained from the top of the column with some impurities such as water, fatty acids, soap, etc. [2]. Figure 1 shows the general process flow of glycerine refining.
General process flow of glycerine refining.
According to MarketWatch 2018, the global glycerine market is expected to reach approximately 6200 metric tons by 2024 from 3550 metric tons in 2016, resulted from the growth in bio-renewable chemicals, biodiesel production, and wide range of applications. However, with regard to the market price, technical grade glycerine is cheaper than the refined glycerine which are approximately RM4400 and RM5400 per metric ton, respectively, as reported by Oleoline (2017).
Furthermore, glycerol can be used as a starting material for the synthesis of value-added chemicals via catalytic conversion such as hydrogenolysis to propanediol and ethylene glycol, dehydration to acrolein, fermentation to propane-1,3-diol, thermal reduction into syngas, etherification to fuel oxygenates, conversion into glycerol carbonate, and synthesis of epichlorohydrin [6]. Among these, the etherification of glycerol into polyglycerols particularly diglycerol (DG) and triglycerol (TG) is gaining more interest in the recent research due to their possibility in controlling the hydrophilic–lipophilic balance (HLB) which is highly important as additive to food and pharmaceutical industries, lubricants, stabilizers, dispersants, plasticizers, etc. [6]. According to Grand View Research in polyglycerol market size, the demand for diglycerol and triglycerol is expected to grow by 50% from 2012 to 2022. The global diglycerol demand is expected to grow at a CAGR of 5.3% due its extensive use in various industries, thus validating the importance and value addition of producing diglycerol.
Due to the volatility of refined glycerine market price and increasing demand of polyglycerol especially the shortest chain oligomer which is diglycerol, research has been conducted to upgrade glycerol via various processes such as pyrolysis, epichlorohydrin, and catalytic etherification to produce polyglycerols. Etherification is a single-step process of catalytic conversion of glycerol into polyglycerols, involving the condensation of two glycerol molecules to form the simplest oligomer which is diglycerol with linear, branched, or cyclic isomers. Further reaction yields tri-, tetra-, and higher oligomers. Short-chain oligomers are preferred. Therefore, the etherification of glycerol under controlled conditions is required [7]. The etherification method has potential to replace the conventional epichlorohydrin route of producing polyglycerols which is relatively complex and involves in the production of toxic intermediate. Polyglycerols can be produced from different raw materials such as crude glycerine, yellow glycerine, as well as pure glycerine [7, 8, 9]. Hence, the economical production of glycerol derivatives is directly related with the quality of glycerine feedstocks and prices.
With regard to the heating method, microwave irradiation has been increasingly popular as a heating method for organic reaction. It had been proven to be more effective than the conventional water bath heating [10]. Various benefits of microwave irradiation included internal rapid heating that reduced the reaction time which compensates its higher power consumption. Besides, efficient and uniform heating that enables good temperature control can be achieved via microwave heating.
On small scale, pure diglycerol is produced via direct synthesis methods in which diallyl ether is used as a primary reactant [1]. Diallyl ether is accessible by the reaction between allyl chloride and allyl alcohol in inert solvents under hydrogen chloride release. Direct hydroxylation of this product can be performed with peroxyformic acid, CH2O3, or permanganate at 40°C under safety precautions for 4.5 hours. However, several additional steps are needed for neutralization, filtration, derivatization, and fractional distillation which are required for the isolation of diglycerol and triglycerol. The isolation of diglycerol can be done using neutralization with barium hydroxide solution, centrifugation to separate the solid, digestion of the product in absolute ethanol, and fractional distillation under reduced pressure.
The thermal reaction for glycerol oligomerization is conducted at a certain temperature under inert protecting reactor condition [1]. For selective reaction, pure glycerol up to 99% purity should be used. Commonly, before the use of the oligomeric products for further reactions, a distillation is needed to remove unconverted glycerol. Reaction temperature, basicity, and organic impurities would affect the glycerol oligomerization. For pure thermal conversion of glycerol without the addition of catalyst, temperature is normally set above 200°C. However, at reaction temperature higher than 290°C, side products with strong smelling are formed. At 180°C (low temperature) with the addition of alkali catalyst, the formation of diglycerol from glycerol is observed but at low conversion of glycerol.
The epichlorohydrin method of producing polyglycerol is commonly applied. It involves basic hydrolysis by sodium hydroxide, led to the formation of intermediate product, namely, glycidol and glycerol, and it will react with unconverted epichlorohydrin or glycerol to diglycerol [6]. Further separation and purification of products are required. Residue glycerol will be separated, and then water has to be removed from the raw diglycerol, and, finally, the product has to be subjected to a fine distillation. The reaction of glycidol or epichlorohydrin with glycerol has in common that the coupling OH groups are not confined to the terminal positions but also the middle OH groups of glycerol can be involved as well. This leads to the formation of primary or secondary dimer of glycerol.
The etherification reaction of glycerol to produce value-added diglycerol has been extensively studied either using homogeneous or heterogenous alkali or acid catalysts. The etherification reaction is normally conducted under solvent-free condition for economical and environmental reasons [7]. Etherification is a condensation process whereby two glycerol molecules will react to form ether bond in between the molecules by removing water molecule. This reaction is also called etherification since the final product is in ether form as shown in Figure 2. Glycerol oligomers can be in linear, branched, or cyclic form [11]. The formation of different isomers is affected by the reaction conditions such as temperature, time, catalyst type, catalyst loading as well as the starting raw material for diglycerol synthesis. Diglycerols are mostly obtained from the oligomerization of glycerol catalyzed by acid or based catalysts.
Etherification of glycerol to polyglycerols.
The reaction by homogeneous acid catalyst is promoted by the protonation of one of the glycerol hydroxyl groups: a mechanism of SN1 as shown in Figure 3. A carbocation is formed by splitting off a water molecule, followed by nucleophilic attack of a hydroxyl group of another glycerol molecule. Then, the formed ether is deprotonated, yielding the respective diglycerol [1]. Acid-catalyst oligomerization used sulfuric acid at 280°C in 2 hours giving more than 90% conversion of glycerol, and the main oligomers were triglycerol and tetraglycerol which only make the 20% of overall component, showing other side products were dominant in the reaction which were hardly identified [6].
SN1-type mechanism for glycerol oligomerization in acid-catalyzed homogeneous reaction.
Reported studies suggest that homogeneous acid-catalyzed reaction is generally fast but not selective for diglycerol. This could be due to the dehydration or oxidation of glycerol as secondary reactions to other undesired products. These secondary reactions may also result in the deterioration of the main product quality by changing its color, making the final product darker in appearance.
The reaction with glycerol conversion under basic homogeneous catalyst is proposed to follow an SN2 mechanism as shown in Figure 4. In SN2, the interaction of the base OH with glycerol weakens one of the glycerol OH bonds and enhances nucleophilic character of the hydroxyl oxygen. The attack of this polarized glycerol to a carbon of a second glycerol with simultaneous split off water results in diglycerol.
SN2-type mechanism for glycerol oligomerization in base-catalyzed homogeneous reaction.
Several homogeneous bases have also been studied as catalysts in glycerol etherification. Depending on their basicity and solubility in glycerol, the following order of activity was reported under reaction temperature of 260°C at 4 hours with 2.5 mol% of catalyst:
Based on solubility measurements, the higher activity of carbonates than that of hydroxides was indeed ascribed to a better solubility of the former in glycerol and in the polyglycerol mixture at elevated temperature [6]. However, there are several studies presented that contradict the results from the proposed theory on solubility. A study conducted by [9] of glycerol conversion using Cs2CO3, CsOH, and CsHCO3 showed 20% glycerol conversion and 100% diglycerol selectivity; hence, different anions did not alter the reaction characteristics. From the research carried out by [7], their studies reflected that the pH of the mixture of catalyst with glycerol which increased in the order LiOH, NaOH, KOH, and Na2CO3 was the main factor of high glycerol conversion and diglycerol selectivity. One hundred percent glycerol conversion was achieved for LiOH and NaOH catalysis system with 21 and 18% diglycerol selectivity, respectively. This could be resulted from the nature of lithium metal as the most active metal due to highest alkalinity, smallest ionic size, and highest atomic electronegativity [7].
Raw material choice on polyglycerol production is also very crucial in polyglycerol generation. A study done by [8] argued that polyglycerol production can be carried by the self-polymerization of crude glycerol which contained different amounts of soap (as homogeneous-based catalyst) which was originally presented in the crude glycerol samples. The experiment was carried out at 260°C under microwave heating; within 1 hour, the sample of soap with a highest soap content of 12.5% gave the highest conversion (94.94%) with 47.99% diglycerol. This study supported the claim by [7], whereby the higher the pH, the higher is the conversion and diglycerol selectivity. Besides, they also found that the processes with different feedstocks affected the amount of soap contained in the crude glycerol, preferably the refined, bleached, deodorized palm oil (RBDPO) which generated the highest amount of soap, creating a favorable condition for self-polymerization.
The shortcomings from homogeneous catalysis system include low selectivity to small-size polyglycerols which is the desired product of polyglycerols; uncontrollable oligomerization of glycerol which produces larger polyglycerols together with smaller polyglycerols would result in separation issue.
Recently, the main focus on catalytic etherification is on the implementation of heterogeneous catalyst in the etherification reaction to overcome the shortcomings of using homogeneous catalyst whereby the reactions are performed on solid materials of limited solubility [1]. Mesoporous solids modified by cesium impregnation or exchange lead to the best selectivity and yield to diglycerol in which 100% of diglycerol was produced after 10 hours reaction time [12]. The etherification activity was improved by the impregnation of LiOH with acid-treated montmorillonite K-10 (clay MK-10) [13]. Researchers reported that the clay Li/MK-10 catalyst gave a favorable result in selectively producing diglycerol which yielded 53% with high glycerol conversion of about 98%. However, the drawbacks of using heterogeneous catalyst are the leaching of metal from solid support into the liquid mixtures and instability of the solid support, resulting in dropping in efficiency to cater the reaction.
Microwaves are electromagnetic waves which consist of both electric and magnetic fields that fall within 0.3–300 GHz on electromagnetic spectrum with wavelengths ranging from 0.01 to 1 m. Within the specific frequency range, the microwave transmits energy between 1.24 × 10−6 and 1.24 × 10−3 eV. Table 1 shows the energy of different chemical bonds and microwaves [14]. With the energy lower than the Brownian motion, microwave will not be able to induce chemical reactions through bond breaking.
Bonding and microwave | Energy (eV) |
---|---|
Brownian motion at 37°C | 2.7 × 10−3 |
Biological compound | 13.6 |
Covalent bond | 5 |
Hydrogen bond | 2 |
Van der Waals intermolecular interactions | <2 |
Microwave at 0.3 GHz | 1.24 × 10−6 |
Microwave at 2.45 GHz (domestic oven) | 1 × 10−5 |
Microwave at 300 GHz | 1.24 × 10−3 |
Energy of different bonds and microwaves.
Microwave heating is a direct heating method which is highly dependent on the properties of materials to convert electromagnetic to heat energy. The two ways of inducing heat into a systems via microwave are dielectric heating and magnetic loss heating; however, based on the publications, researchers are mainly focus on studying the dielectric heating effects and mechanisms because this heating effect is more significant. Dielectric heating occurs due to the dielectric properties on the reacting medium. For example, materials with high dielectric constant tend to absorb microwave; however, poor dielectric property compounds are poor electromagnetic wave absorber. Hence, microwave is highly applied in organic reactions.
In conventional heating, heat is transferred through conduction and convection in which the heat is transferred from the sides/surface of a substance, then only travel to the center of targeted heating medium. This heating method is dependent on the heating flask properties such as thermal conductivity, specific heat capacity, density, etc. Hence, the portion of heat will be loss to the environment during heating. When compared to microwave heating, the heating duration using microwave to achieve the same temperature could be dramatically reduced. Figure 5 shows the heating mechanism for both conventional heating and microwave heating.
Heating mechanisms for (a) conventional heating and (b) microwave heating.
Microwave radiation serves as an alternative to conventional heating especially in organic synthesis. The advantages of microwave heating over conventional heating are accelerating chemical reactions and promoting higher conversion and selectivity and low energy consumption as reported by [14] with respect to the same operating conditions under microwave heating. Plenty of studies have been carried out on the application of microwave in organic synthesis, for example, reactions in solvent-free condition, polymer synthesis, homogeneous and heterogeneous catalysis, medicinal and pharmaceutical chemistry, etc. [15].
Theories that are applied to explain the effect of microwave in enhancing a reaction are based on thermal and nonthermal effects as presented by [14] in Table 2.
Thermal effects | Nonthermal effects |
---|---|
Dipolar polarization | K = A exp.(−Ea/RT) |
Ionic conduction | Enhancement in collision probabilities |
Uniform heat distribution | Decrease in activation energy |
Specificity for polar molecule | Hot spots |
Effect increase with polarity | High localized microscopic temperatures |
Microwave heating mechanisms via thermal and nonthermal effects.
Most of the studies on microwave effects describe the presence of hot spots or localized heating which enhances the chemical reactions due to direct adsorption of radiation by the polar molecules. Microwave energy is transferred through the relaxation of polar molecules, thus promoting molecular friction and collision [10]. As reported by [15], the hot spot will possess higher energy at the active sites, promoting the activities of the species adsorbed on the catalyst surface, whereas [16] presented that the conversion of hydrogen sulfide is higher than the theoretical equilibrium conversion; however, the results from conventional heating are similar to the theoretical value. They claimed that the reaction temperature at some site in the catalyst bed was much higher than the average temperature measured. However, studies by [14] illustrated that the occurrence of hot spot on catalyst surface is more likely to lower the catalytic activities, hence reducing the productivity. For an exothermic reaction, for example, the desulfurization, both microwave and conventional, provides similar conversion at the same operating conditions. Further increment in temperature in microwave system would cause the conversion to drop (lower than conventional heating), due to the shifting of equilibrium to less favorable reactions [16].
Besides localized heating effects, decreasing in the activation energy and improving the pre-exponential factor are the two main factors in enhancing microwave-assisted organic synthesis. When inducing microwave, a portion of the radiation heats up the system due to microwave thermal effects; another portion directly interacts with chemical or catalytic reaction system to reduce the activation energy, changing the interior energy level of molecules. The increment in the pre-exponential factor is due to the effective collision between molecules assisted by electromagnetic wave which change the movement of the molecules from disordered motion to ordered motion [17].
Even though in most cases microwave heating enhances the reactions, in the reaction with high sensitivity to the temperature change especially in a strong exothermic reaction, conventional heating would be preferred. The study in Fischer glycosidation showed a higher conversion under conventional heating which may be due to the higher overall reaction time, and the reaction temperature is reached smoothly. The reaction under conventional heating does not present localized overheating which can be found in microwave heating. Localized overheating in microwave was observed from the temperature overshoot above the desired temperature, causing glucose decomposition [18].
For the etherification reaction, most of the researches were conducted by conventional heating, and typical reaction times were longer than 8 hours. Microwave radiation is proven to be a more effective heating method in the etherification of glycerol. The required reaction time to produce targeted polyglycerols facilitated by the microwave irradiation was much shorter than the etherification carried out by conventional heating which required at least 6 hours, whereas it took only 1 hour for microwave heating.
Microwave irradiation-assisted heating found to be a cost-efficient technology to be applied for the biodiesel conversion into polyglycerol. The application of modified heterogenous base catalyst could minimize the waste besides being compatible for the reaction of biodiesel waste into polyglycerol. Besides, it has provided insight on the oligomerization reaction of glycerol to maximize the yield of the valuable di-, tri-, and tetraglycerol oligomers for numerous applications with current industrial demand.
The authors would like to thank the Yayasan Universiti Teknologi PETRONAS with research grant FRGS 0153AB-L63 for providing financial support for this study.
IntechOpen publishes different types of publications
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