Subgroups of clay minerals.
\\n\\n
More than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\\n\\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\\n\\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\\n\\nAdditionally, each book published by IntechOpen contains original content and research findings.
\\n\\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Simba Information has released its Open Access Book Publishing 2020 - 2024 report and has again identified IntechOpen as the world’s largest Open Access book publisher by title count.
\n\nSimba Information is a leading provider for market intelligence and forecasts in the media and publishing industry. The report, published every year, provides an overview and financial outlook for the global professional e-book publishing market.
\n\nIntechOpen, De Gruyter, and Frontiers are the largest OA book publishers by title count, with IntechOpen coming in at first place with 5,101 OA books published, a good 1,782 titles ahead of the nearest competitor.
\n\nSince the first Open Access Book Publishing report published in 2016, IntechOpen has held the top stop each year.
\n\n\n\nMore than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\n\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\n\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\n\nAdditionally, each book published by IntechOpen contains original content and research findings.
\n\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\n\n\n\n
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\r\n\tLiquid atomization, sprays, and fuel injection are at the heart of many chemical-reaction based propulsion and electric energy production such as internal combustion reciprocation, gas turbine and liquid rocket engines. It is known that both performance and emission of pollutants from such systems are heavily influenced by details of the fuel sprays generated from the fuel nozzles or injectors. For these reasons there has been an increasing number of R&D works targeted towards generation of fuel sprays with a desired characteristics to “match” the environment into which they are injected and subsequently burned. Such research efforts span from injector designs to spray characterization and dynamics using both experimental and modeling/simulation approaches. Therefore, the main goal of this book is to cover important advances in this field for the past fifteen years.
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From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. 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In particular, single-walled carbon nanotube (SWCNT) network films have been intensively studied for the development of alternative transparent conductive electrodes due to their excellent electrical properties, the flexibility of SWCNT networks, and their solution processability under ambient conditions (Wu et al., 2004; Kaempgen et al., 2005; Zhou et al., 2006). For such applications, the optoelectronic properties of SWCNT-based TCFs should optimally be controlled by the material properties of the nanotubes, including purity, diameter, chirality, defects, metallicity, and doping level (Geng et al., 2007). Organic materials, such as conjugated polymers, block copolymers, polyelectrolytes, pyrenes, DNA, and so on, may also be used in applications because CNTs display good dispersion and stabilization in a variety of solvent media and polymer matrices. To maintain good electrical and mechanical properties, as well as environmental stability (e.g., thermal and hydrothermal stability), SWCNTs must be hybridized or top-coated with binder materials, such as cross-linkable polymers, ceramic sols, or metal oxide sols. The electrical properties of SWCNT/binder hybrid thin films are sensitive to their surroundings and to the interfacial structure of the network film, and the interfacial interactions or interfacial tension among nanotubes, binder materials, and substrates can affect the optoelectronic and environmental properties of SWCNT-based TCFs.(Han et al. 2009)
Despite these attractive features, fundamental studies and several advances are needed for the practical application of high-performance CNT films. This chapter describes some of the research conducted over the past 3 years that addresses these and other challenges, with an emphasis on our own efforts. We begin with critical properties of binders in CNT/binder hybrid thin films and then describe the various binder materials that yield high-performance CNT-based films via molecular or interfacial engineering at the interface between CNTs and binder materials. We conclude with some discussion of future directions and the remaining challenges in CNT/binder hybrid thin film technologies.
To fabricate CNT/binder hybrid thin films by spraying or spin-coating, CNTs must first be well-dispersed in an organic solvent, and the dispersion stability should be maintained after mixing with the binder materials or additives. The wettability of the components in the CNT/binder mixture solution with respect to the target substrate should be considered. Here, interfacial engineering concepts may be applied to balance the interactions at the interfaces between the CNTs, solvent, additives, binder materials, and substrates (Fig. 1).
Interfacial engineering in high-performance transparent conductive CNT/binder hybrid films.
The conductivity,
Here,
The changes in CNT film sheet resistance after hybridization with binder materials may be understood in terms of the quantity of binder material and the interfacial tension of the components (nanotubes and binder materials). The critical surface tension of a CNT sample falls within the interval 40–80 mN/m, and the cutoff value corresponding to cos
This section presents four methods for modulating the optoelectronic and environmental properties of CNT/binder hybrid films based on interfacial and molecular engineering. The first method uses the concept of a critical binder content to optimize the amount of binder material present with respect to the mechanical and electrical properties of the films. The second method uses molecular engineering to minimize or decrease the sheet resistance of the films or to fabricate multi-functional films by adding insulating binder materials or metal oxides. The last method uses a strategy to control the optoelectronic properties of films by matching the wettability of the coating solution on the substrates.
Transmittance vs. sheet resistance for SWCNT/MTMS hybrid films containing various amounts of MTMS binder. FE-SEM images of SWCNT/MTMS hybrid films containing various amounts of CNTs: (a) 100 wt%, (b) 75 wt%, (c) 50 wt%, and (d) 25 wt%. (
The transmittance and sheet resistance of spray-coated CNT/binder films depend on the quantity of deposited CNTs and binder material, and on the ratio between CNT and binder. A plot of the sheet resistance as a function of binder content shows that above a critical binder content (Xc), the sheet resistance increases dramatically (Han et al., 2009). The strength of the interactions between the nanotubes and binder materials is also an important parameter that determines Xc, thereby influencing the junction structure. Figure 2 shows a plot of the transmittance vs. sheet resistance of the SWCNT/binder hybrid films with various binder contents. In this experiment, a methyltrimethoxy silane (MTMS) sol with a moderate surface tension was used as a model binder material. Here, the sheet resistance increased dramatically at a critical binder content. In this system, the critical binder content, Xc, was approximately 50 wt%. Above Xc, the CNTs were fully covered with the binder material, as illustrated in the scanning electron microscopy image (Fig. 2), which increased the contact resistance between the CNT network and the probe and decreased tunneling between CNTs through the insulating binder layer between the CNT bundles.
Increasing the interaction strength between a binder material and CNT surfaces is expected to increase the distance between nanotubes in a network film due to penetration of the binder material into network junctions. To investigate this interfacial interaction effect, model binder materials are required. A silane sol was used in this study to take advantage of the significant benefits associated with using sol-gel chemistry to modify the properties of a gel using functionalized silane precursors (Brinker & Scherer, 1990). The intermolecular interactions between the nanotube surfaces were controlled using a series of model binder materials: tetraethoxysilane (TEOS), methyltrimethoxysilane (MTMS), vinyltrimethoxysilane (VTMS), and phenyltrimethoxysilane (PTMS), as shown in Fig. 3.
A schematic diagram of the intermolecular interactions between SWCNTs and model binder materials: tetraorthosilicate (TEOS), methyltrimethoxysilane (MTMS), vinyltrimethoxysilane (VTMS), phenyltrimethoxysilane (PTMS). (
The unpaired electrons of the silanol groups of the TEOS sol did not significantly polarize the negative charges on the nanotube surface and did not form favorable interactions. Hydrophobic interactions can arise between the methyl groups in the MTMS sol and the nanotube surface (Gavalas et al. 2001). The vinyl groups in VTMS and the phenyl groups in PTMS can interact with SWCNT surfaces via π-π interactions (LeMieux et al., 2008). The phenyl rings of PTMS may provide the best interfacial surface for CNTs due to strong π-π interactions. Moreover, the surface tension of the MTMS/VTMS/PTMS sol was less than 30 mN/m (Tillman et al., 1998), and that of the TEOS sol was around 170 mN/m (Ulatowska-jara et al., 2009). Therefore, the intertube or interbundle distances in the SWCNT/binder hybrid films could be modulated using these binder materials. This property was directly correlated with the electrical properties of the SWCNT/binder film because the sheet resistance of the film resulted from the intrinsic resistance of the SWCNTs and the contact resistance at the junctions between nanotubes. The binder materials penetrated into the SWCNTs or the SWCNT bundles to increase the junction resistance. From this perspective, we expected the sheet resistance of the SWCNT/PTMS films to be the highest among all films tested because the PTMS increased the junction resistance in the network films.
AFM images of SWCNT/silane hybrid films: (a) SWCNT/TEOS, (b) SWCNT/MTMS, (c) SWCNT/VTMS, and (d) SWCNT/PTMS films. (
As expected, the sheet resistances of the films gradually increased in the order of SWCNT/TEOS < SWCNT/MTMS < SWCNT/VTMS films. However, the sheet resistance of the SWCNT/PTMS film was lower than that of the SWCNT/MTMS film, even though the CNTs appeared to be well-distributed and covered with the binder material (Fig. 4d). Aromatic molecules, such as the phenyl-terminated silane used here, have been reported to interact and bind selectively to metallic SWCNTs because the polarizability of this silane is larger than that of the semiconducting nanotubes (LeMieux et al., 2008). Therefore, Rs of the SWCNT/PTMS was lower than that of SWCNT/VTMS possibly due to interconnections between the nanotubes or nanotube bundles and the phenyl-functionalized silane sol via strong π-π interactions, which decreased the junction contact resistance. Raman spectral data provided evidence of bridging between the nanotubes and the PTMS sol. In a strongly aggregated state, for example a CNT network film without binder materials, van der Waals interactions between bundles dominated, whereas in a CNT/binder thin film, interactions between bundles and the functional groups of the binder materials influenced the Raman features. Binder materials with functional groups, such as nitro, amino, and chlorine groups, provided chemical doping effects via a charge transfer mechanism that influenced the conductivity of the nanotube films (Rao et al., 1997). However, in this system, doping effects were excluded, and the G+ band was only slightly downshifted upon addition of the silane binder materials. This indicated that the functional groups acted as very weak electron-donating groups (CH3, vinyl, phenyl) and the sheet resistances of the SWCNT/silane films were not significantly affected by charge transfer effects. Therefore, the dispersion state or the distance between nanotube bundles in the thin films appeared to dominate the conductivity in the CNT network films. The linewidth of the G+ band and the intensity ratio of the D and G bands were indicative of the degree of aggregation or bundling among the nanotubes. The enhanced resonance processes in the Raman scattering G band may have been due to exfoliation of the nanotubes, which decreased the D/G ratio of the G band. In addition, the relationship between the ratios ID/IRBM and ID/IG for laser excitation at 2.41 eV probed the aggregated state or the interbundle distances of bundles in the thin film network, assuming that the disorder defects were constant after hybridization (Liu et al., 2007). The high ratios of ID/IRBM and ID/IG indicated that the bundles were closely packed (Fig. 5d). The FWHM of the G+ band of the films exhibited a similar trend in the D/G ratio. The sheet resistances of the various silane binders followed a trend opposite that of the D/G ratio and the G+ band FWHM. These results, therefore, provide strong evidence that the average interbundle distance in the SWCNT/PTMS sol hybrid films did not differ from that in the pristine and SWCNT/TEOS sol hybrid films. The SWCNT bundles were presumably bridged by the strong interactions between the CNTs and the phenyl groups of PTMS, which contributed to the enhanced conductivity of the SWCNT networks, even though the CNTs were fully covered with insulating material, as determined by the top-view image. Such precise control over the optoelectronic properties of the SWCNT/binder films may be useful for fabricating high-performance conductive thin films, with ramifications for understanding the fundamental intermolecular interactions in carbon material science.
a) The correlations between the Raman spectral band at 1.96 eV (D/G ratio, FWHM of the G+ band) and the Rs (with an optical transmittance of 85%) for pristine SWCNTs and SWCNT/silane films. (b) Metallic components extracted from the G-band and G-band shift at 1.96 eV. (c) An illustration of the possible interactions between the SWCNTs and PTMS. (d) Correlation between the ratios
If the wettability of conductive CNT films with high transmittance could be controlled via a superhydrophobicity (with a contact angle (CA)> 150°)-to-superhydrophilicity (CA< 5°) transition, this technology could potentially meet the needs of a wide range of applications that require multifunctional coatings (e.g., in optoelectronic devices, structural coatings, etc.). Many authors have focused on the fabrication and understanding of superhydrophobic surfaces, particularly those based on CNTs. However, most studies have not considered the optical properties of such CNT-based superhydrophobic surfaces. For applications in optical devices, transparency is one of the most important characteristics.
In nature, the leaves of many plants exhibit super water repellency (super-hydrophobicity) and are cleaned completely during a rain shower via the rolling of surface water droplets, which remove dirt and debris (self-cleaning) (Barthlott & Neinhuis, 1997). The unusual wetting characteristics of superhydrophobic surfaces are governed by both the chemical composition and the geometric microstructure of that surface. Wettability can be decreased or increased by creating a local structure that has a large geometric surface area in three dimensions relative to the projected two-dimensional area (Wenzel, 1936; Cassie & Baxter, 1944). Control over the wettability and optical properties may be achieved using mixed solutions containing CNTs and silane sols to produce multifunctional coatings. CNT networks control the nanostructure of the films, and silane compounds introduce a variety of chemical moieties on the top surface to provide particular mechanical properties. Recently, we presented, for the first time, a facile method for creating transparent, conductive, superhydrophobic (or superhydrophilic) films from a one-component CNT/silane sol solution (Fig. 6). The stable CNT/silane sol solution relied on the intermolecular interactions between the hydroxyl groups of the H2O2-treated CNTs and the silanol groups of the silane sol. Moreover, the superhydrophobicity of the transparent (T > 90%) conductive films was enhanced by introducing nanoparticles into the coating solution
A) Schematic diagram of the hydrogen bond-driven stabilization of a CNT solution. (B) Image of a stabilized CNT/silane sol solution. (C) FE-SEM image of a spray-coated CNT/silane hybrid film. (D) Water droplets on this film. (
(Fig. 7). The combination of the transparency and conductivity of CNTs with the chemical functionality of the silane binder would be beneficial to a wide range of CNT-based film applications, for example, development of self-cleaning optoelectronic coatings, transparent film heaters, electrostatic discharge coatings, and EMI shielding.
Water CA (triangles) and sheet resistance (Rs) (circles) versus transmittance of CNT/silane hybrid films (silane content = 70 wt%) without (red) or with (blue) silica nanoparticles. The upper image shows water droplets on transparent conductive films (the numbers shown in this image correspond to those in the plot). (
CNTs have been used to prepare a variety of hybrid materials that enhance the stability and functionality of CNT-based films by incorporating organic materials or inorganic oxides, such as SiO2, TiO2, SnO2, and ZnO. A successful strategy for fabricating the SWCNT/metal oxide films should employ a reliable means for forming stable solutions of SWCNTs and the metal oxide sol. The dispersion stability of SWCNTs functionalized with carboxylate groups (SWCNT-COOH) strongly depends on the ionic strength and pH of the solution.(Zhao et al. 2002) At pH < 3.0, SWCNTs are protonated, and they aggregate due to van der Waals forces and hydrogen bonding between protonated carboxylic acid groups. At pH > 3.0, mutual repulsion between tubes with charged carboxylic groups stabilizes the SWCNT dispersion. Organic or inorganic materials that contain amine groups can promote aggregation of the SWCNTs-COOH through hydrogen-bonded network formation.
In particular, titania layers provide efficient shielding to prevent penetration of oxygen or moisture into the electronically active layer.(Lee et al. 2007) Uniform titania coatings on CNT films constitute a potentially useful approach to enhancing the thermal and thermo-hydrostatic stabilities of CNT network films. Titania also acts as an electron transport material due to its high n-type carrier density and high electron mobility, which minimize junction resistance within the film network after hybridization to a binder material. Until now, titania coatings on CNT surfaces have been applied using highly functionalized multiwalled carbon nanotubes (Salzmann et al. 2007 & Gomathi et al. 2005) or benzyl alcohol (BA)-assisted noncovalent methods (Eder et al. 2008). However, functionalization by acid treatment decreases the conductivity of films. The BA method is not suitable for preparing TCF coating solutions because BA does not disperse SWCNTs in organic solvents and cannot stabilize titania sols during the coating process.
We recently reported that a complex formed between acetylacetone (acac, stabilizer of titania sol) and titanium in a titania precursor sol could be used to form a uniform titania layer on nanotube surfaces via hydrophobic interactions (Fig. 8). The thickness of the titania sol layer was controlled by varying the quantity of titania sol used in the solution. TEM images demonstrated formation of a uniform titania layer coating several nanometers thick on the surfaces of the SWCNTs. However, in the absence of acac, irregular titania formed because titanium atoms interacted selectively with carboxyl groups on the nanotube surfaces and amorphous carbon. The titania layer dramatically enhanced the thermal stability of the SWCNT films. The SWCNTs were easily oxidized at temperatures above 350°C, and the network in the SWCNT films was found to be disconnected (Fig. 9d). In contrast, the SWCNTs wrapped with a titania layer were stable under heating, as shown in Fig. 9c. Moreover, the titania layer provided positive effects on the electrical properties of the films via doping effects that operated under a charge transfer mechanism. Titania withdrew electrons from the nanotube surfaces, resulting in enhanced conductivity of the nanotubes. The D-band in the Raman spectra of functionalized SWCNT samples usually contains a broad peak upon which
Mechanism for the noncovalent coating of SWCNTs with a titania layer, followed by removal of acetylacetone molecules by thermal treatment. (
SEM images of (a), (c) SWCNT/titania sol with acac and (b), (d) SWCNT/titania sol without acac containing 50 wt% titania sol; (a), (b) cured at 150°C, and (c), (d) baked at 350°C for 1 h. Right inset images in (a) and (b) show TEM images. Left bottom images in (b) show the chemical environment of the nanotube surface without acetylacetone. (
is superimposed a sharper peak. The broad feature arises from amorphous carbon, and the sharper feature arises from carbon nanotubes. The narrowing of the D-band of titania-wrapped SWCNT (SWCNT@titania) films and the decrease of the carboxyl C1s peak in XPS after heating at 300°C indicated the removal of amorphous carbon without oxidation of the functionalized SWCNTs. The removal of amorphous carbon also decreased the sheet resistance of the SWCNT@titania films. Moreover, the ultrathin titania layer on the SWCNTs protected against water molecule absorption.
Transparent conductive coatings based on CNTs are currently made using membrane filtration or spraying techniques. Spray application over a large irregular area is advantageous for high-throughput fabrication. Here, the wettability of the CNT/binder coating solutions on the substrates should be controlled during fabrication of highly transparent conductive thin films, because the film thickness is optimally smaller than several hundred nanometers. In this respect, the surface free energy of the substrate affects the surface properties and interfacial interactions, such as adsorption, wetting, and adhesion. Control over the wettability and optical properties may be achieved using a mixture of CNTs and silane sol, which is a promising candidate for producing multifunctional coatings. Sol-gel chemistry offers several advantages when used to modify the properties of a gel with functionalized silane precursors. Recently, we studied the surface energy effects on the optoelectronic properties of CNT/binder hybrid films on glass substrates modified with silane layers containing various end functionalities. The CAs of silane-modified glasses were 67° for an NH2-functionalized surface, 96.5° for a CH3-functionalized surface, and 112° for a CF3-functionalized surface (Fig. 10).
The sheet resistances gradually decreased with increasing wettability of the coating solution on the substrates. Although the transmittance of the films changed very weakly (T changed from 92.3% to 91.2% in moving from a CF3-functionalized to an OH-functionalized surface), the sheet resistance of the film on the OH surface was an order of magnitude smaller than the counterparts prepared on a CF3-functionalized surface, giving a very low surface energy. This result is significant because the sheet resistance can change dramatically for high transmittance films. SEM images of the CNT/MTMS sol hybrid films clearly showed that the hydrophilic surfaces were more homogeneous than the hydrophobic surfaces. A decreased surface energy increased the heterogeneity of the surface morphology. In particular, the most hydrophobic surfaces (containing CF3 groups) clearly showed a dewetted pattern after spray-coating, which may explain the slightly higher transmittance of the film. Nevertheless, the sheet resistance of this film was sufficient for transparent ESD films. The CNTs were macroscopically connected with a fractal dimension of 1.77 for the film surface. The dark regions in the SEM images indicate the low-CNT-density areas (mostly binder materials), as shown in Fig. 11. The low sheet resistance and high transmittance of the film prepared on a CF3-functionalized surface was explained in terms of the submicrometer-scale disconnect between CNTs, as shown in Fig. 15d. These results indicated that the sheet resistances of highly transparent CNT/binder hybrid films were easily modulated by controlling the wettability of the CNT/binder mixture solutions on the substrate. Previous studies by Kim et al. also attempted to improve the transparency of CNT films by adjusting the CNT network density using a two-dimensional colloidal crystal template. (Kim et al. 2008)
Schematic representation of the spray coating of FWCNT/silane solutions on surface-modified model substrates. (
These results have important implications for the fabrication of highly transparent conductive films from CNTs and binder solutions. Although we used a polar solvent and a hydrophilic binder material in this study, our method is applicable to a variety of coating solutions prepared using other solvents and binder materials on various substrates, such as poly(ethylene terephthalate), polyether sulfone, and polycarbonate. Moreover, we suggest that the transparency of CNT/binder films can be improved by manipulating the CNT density in the film, which can be achieved by adjusting the wettability of the coating solution or by forming dewetted areas with different surface energies, because the conductivity and transparency of a film depend primarily on the CNT density.
Scanning electron microscopy images of CNT/MTMS thin films on various substrates; the surface functionalities are: (a) OH, (b) NH2, (c) CH3, and (d) CF3. (
Research into CNT/binder hybrid thin films over the last few years has yielded significant progress in controlling the optoelectronic properties of the films by modulating the balance of interactions at the interfaces among the components: CNTs, solvent, additives, binder materials, and substrates. A critical binder content was identified, above which the sheet resistance increased dramatically, and this value was found to depend on the interfacial tension between the CNTs and binder materials. At the same time, effective methods were developed for minimizing or decreasing the sheet resistance by adding insulating binder materials. The transparent, conductive, superhydrophobic coating technology relies upon controlling the surface nanostructure and chemical state of the surface. The thermal and environmental stability of the SWCNT films were enhanced by noncovalent wrapping by a titania layer. The optoelectronic properties of the CNT/binder hybrid films were modulated by controlling the wettability of the coating solutions on the substrate.
Significant challenges to this technology remain. First, strategies for minimizing the junction resistance in a random network structure must be developed for applications such as high-performance CNT-based TCFs. Second, improved hybridization methods using various ceramic oxides or metal oxides are needed to use these films in multifunctional electronic devices, such as sensors, actuators, and thin film heaters.
Clays are inorganic, natural, earthy, and fine-grained materials that acquire plasticity when mixed with water [1]. For sedimentologists, a clay is a raw material whose grain size is less than 2 μm. Like clays, in turn, there are rocks made up of clay minerals and may contain other minerals such as quartz, feldspar, mica, calcite, hematite, and organic matter as accessories [2]. A clay, once ground and mixed with water, in addition to presenting excellent workability in the fresh state, after drying, becomes extremely rigid. After burning normally above 800°C, it acquires great resistance [3]. Clays are used worldwide in the ceramic industry, especially in bricks, coatings, and others. However, clays are formed from the weathering of explosion and can be contaminated with several minerals among them or carbonate, which can alter the shape that causes the following burns. Limestone may be present in colloidal form, or coarse particles. However, in all cases it is impossible to separate or calculate this. Some researchers have tried to reduce the size of the variations to improve the chemical changes. According to Barba et al. [4], calcium carbonate and magnesium carbonate are the main constituents of carbonate sedimentary rocks. Anionic carbonate groups are strongly activated units and share oxygen with each other. They are responsible for the properties of these minerals. The most important anhydrous carbonates belong to three isostructural groups: the calcite group, the aragonite group, and the dolomite group. Among these, the minerals most used in the ceramic industry are calcite and dolomite, as they are low-cost raw materials, in addition to having favorable physical and chemical properties and available deposits. Second, Padoa [5] adds that when CaCO3 is small, a decomposition can be complete and the calcium oxide reaches later with other mass components forming calcium silicates and silicon aluminates (wollastonite, anortite, gehlenite etc.) during sintering. Barba et al. [4] mentioned that the raw materials of clay when burned at high temperatures produce crystal phases that influence the properties of ceramic products. Calcite exerts a bleaching action on burnt products when added to a formulated mass of clays (in proportions above 5% and less than 30%) and at the same time decreases its expansion by legislation, as it forms crystalline and liquid phases, including cycles temperature and firing adopted. Calcite and dolomite are the most important representatives of carbonates in the ceramic industry. They are used as main components in the manufacture of ceramic tiles with high water absorption. These coatings include “porous coatings” or “tiles.” These products are designed or used on walls and are not suitable for application on floors, as they have undesirable technical characteristics, such as mechanical resistance, incompatibility with use. According to Amorós [6], properties of parts of a ceramic product are registered by crystalline phases formed based on calcium and magnesium as ghelenite (SiO2⋅Al2O3⋅2CaO) and anortite (2SiO2⋅Al2O3⋅CaO). To achieve these phases, use the dolomite calcium oxide and/or magnesium reaction with a remaining clay structure proven by its thermal decomposition.
The calculation in general can affect the ceramic product in two ways: low percentages (up to 3%) and high temperature (above 1180°C) result in flow agents, that is, materials that contribute to reduce water absorption and increase the resistance of ceramic products. Above 3%, they can act as a foundation at temperatures above 1170°C [7].
In this chapter, we will highlight properties of limestone clays and their application in the ceramic industry.
Clays are hydrated aluminum silicates with crystalline structure arranged in layers, consisting of continuous sheets of SiO4 tetrahedrons, ordered in a hexagonal shape, condensed with octahedral sheets of di and trivalent metal hydroxides, usually below 2 μm. They are materials that in contact with water become plastic, a fundamental characteristic for conformation of ceramic products because it provides mechanical resistance in the pressing, extrusion, or gluing process. Clays are mixtures of various clay minerals such as kaolinite, illite, and montmorillonite, which may or may not contain impurities [3, 8].
The kaolinite with structural formula Al2O3⋅2SiO2⋅2H2O has a dioctahedral structure, which consists of a tetrahedral layer linked by an octahedral layer. Pure kaolinites usually have low plasticity, see Figure 1.
Kaolinite structure. (a) Si▬O tetrahedra on the bottom half of the layer and Al▬O,OH octahedra on the top half. (b) Dioctahedral structure.
Montmorillonites are a set of family of clay minerals, composed of dioctahedral and trioctahedral silicate sheets, see Figure 2(a) and (b). The most outstanding feature of these minerals is their ability to absorb water molecules [8, 9]. It has 80% of exchangeable cations in the galleries and 20% on the lateral surfaces. The modification of montmorillonite clays has aroused scientific and technological interest for providing significant improvements when incorporated into pure polymeric materials and conventional composites. The clay modification process occurs preferably through the ionic exchange of the exchangeable cations of its crystalline structure.
Crystalline structure of a montmorillonite. (a) Montmorillonite structure, composed of Si, Al, and O. (b) Sheets of dioctahedral and trioctahedral silicates.
The basic structural unit of the illites is the same as that of the montmorillonites except that in illites, the silicon atoms in the silica layers are partially replaced by aluminum. Therefore, there are free valences in the boundary layers of the structural units, which are neutralized by K cations, arranged between the overlapping units. The structural scheme of the illites is shown in Figure 3. The K cation is the one that best adapts to the hexagonal meshes of the oxygen planes of the layers of silica tetrahedron and is not displaced by other cations. The water adsorption and cation exchange capacity is due only to the broken connections at the ends of the layers. The average diameter of the illites varies between 0.1 and 0.3 μm. When the replacement of silicon in the tetrahedron layers by aluminum in the illites is small, the connections between the structural units provided by the K cations may be deficient and will allow water to enter. When this occurs, the properties of the illites are close to the properties of montmorillonites [3].
Crystalline structure of an illite. (a) Silicon atoms in the silica layers partially replaced by aluminum in the illites. (b) Structural scheme of illites.
Chlorites are minerals made up of four hydrated aluminum and magnesium silicate layers, containing Fe (II) and Fe (III) as shown in Figure 4.
Crystalline structure of chlorite [
The most common clay minerals are interstratified, characteristic of mixtures of clay minerals, classified by subgroup and mineralogical species, see most common classification in Table 1. Clay minerals are divided into several classes. A large majority of clays do not have in just one crystalline phase. Two or more chemical species may be present.
Subgroup | Chemical species | Minerals |
---|---|---|
Kaolin Xn(Y2O5)(OH)4 | Kaolinites | Nacrite (Al2(Si2O5)(OH)4) Dikite (Al2(Si2O5)(OH)4) Livesite (Al2(Si2O5)(OH)4) Halloysite (Al2(Si2O5)(OH)4) |
Talc XB(Y2O5)(OH)2ZmH2O | Montmorillonites | Montmorillonites (Al1,51Fe0,07Mg0,60)(Al0,28Si3,72)O10(OH)2Na0,33 |
Beidellite (Al1,46Fe0,50Mg0,08)(Al0,36Si3,64)O10(OH)2Na0,4 | ||
Nontronite (Fe1,67Mg0,33)(Si4O10)(OH)2Na0,33 and Fe2,22(AlSi3O10)(OH)2Na0,33 | ||
Hectorite (Mg2,67Li0,33)(Si4O10)(F,OH)2Na0,33 | ||
Saponite Mg3(Al0,33Si3,67)O10(OH)2Na0,33 | ||
Illites | Wide variety of minerals | |
Chlorite | Chlorites | Chlorite |
X2n(Y2O5)2(OH)2 | [Mg2(Al,Fe(III))(OH)6][Mg3(AlSi3O10)(OH)2] |
The clays used in the ceramic manufacturing process can be classified into:
Carbonitic clays: they are formed by associations of illitic-chloritic and eventually illitic-kaolinite clay minerals. The amount of calcium carbonate present can be variable. These clays give the dough plasticity. Generally, after burning they have colors ranging from beige to orange [4].
Non-carbonitic clays: they are characterized by the almost total absence of carbonates. The clay minerals present are of the illitic-chloritic type. It has the function of giving plasticity to the dough, and generally after firing they give rise to well-sintered materials.
White plastic clays: the clay matrix is kaolinitic, with little illite. They give plasticity to the dough, and after burning they have a white color.
Kaolinitic clays: clays of low plasticity and normally free of fluxing oxides such as K2O and Na2O, therefore, with refractory characteristics.
According to Mackenzie [10], when a ceramic raw material is subjected to the action of heat, it experiences volumetric variations, usually permanent and irreversible, which can be classified as:
Oxidation of organic matter
Decomposition of compounds containing oxygen, such as sulfates, carbonates, etc.
Dehydroxylation of the clayey mineral
Crystallization by increasing the temperature
Vitreous phase formation
Solid solutions: adjacent crystals of two different materials but of similar structure can react with each other, forming a solid solution.
Kaolinitic clay: the scheme according to Figure 5 shows an endothermic peak between 560 and 590°C referring to the elimination of hydroxyls from the constitution water present in the clays, and an exothermic peak between 980 and 1000°C, due to the formation of mullite, which can be represented by the reactions 1 and 2 [8].
Differential thermal analysis of a kaolinitic clay [
Montmorillonite: montmorillonites have water that lodges in the mineral structure, that is, hydration water of adsorbed ions. The elimination of hydroxyl groups occurs at 700°C. At 850°C, a small endothermic peak may occur due to the loss of montmorillonite crystallinity. Illites can present loss of adsorbed water between 100 and 200°C and water loss in the constitution between 550 and 600°C, see Figure 6.
Differential thermal analysis of a montmorillonite clay [
Quartz: it appears in clays in colored or colorless round grains, whose percentage ranges from 0 to 60%. For high levels of quartz, the clay is called sandy and has low plasticity [11].
Hematite: iron can be present in the forms of hematite (α-Fe2O3), goethite (α-FeO⋅OH), and lemonade (a mixture of iron oxides and hydroxides of a weakly crystalline nature), or simply as Fe3+ ions in the clay structure. In the illite group, Fe3+ ions can replace Al3+ ions in the octahedral structure [11]. Fe2O3 is formed during sintering under oxidation conditions and from minerals in the clays, giving a reddish color to ceramic materials.
Feldspar: feldspars refer to a group of aluminum silicate minerals. The feldspar contained in the clays is a source of sodium and potassium oxides and plays an important role in ceramic materials with quality of flow agents, temperatures such as sintering temperatures, porosity after firing and facilitating phase formation [6]. The most representative are the orthoclase (KAlSi3O8) and albite (NaAlSi3O8).
Carbonates: calcium or magnesium carbonates can appear as coarse or small grains. If they are presented as large grains (>125 μm), they may not react completely and the resulting oxides may rehydrate causing expansion according to reactions [12, 13].
Ceramic enamels and frits: can be used in matte enamels as a source of CaO to form crystals such as wollastonite, anorthite, gehlenite or in transparent enamels giving shine.
Masses for ceramic coating: as a source of CaO up to the limit of 3%, CaCO3 assists in the formation of the vitreous phase. CaO levels that vary from 8 to 14% favor the formation of crystalline phases such as gehlenite, wollastonite, pseudo wollastonite, and anortite.
Putties for limestone porcelain: calcium carbonates provide the CaO that are used as a flux in limestone porcelain masses.
Ceramic pigments: the calcium carbonate provides calcium oxide, which together with SnO2 produces pink pigments.
Glasses: glasses based on NaOH and CaO use CaCO3 in their composition.
Obtaining settlement mortars: as a plasticizing agent for water retention and aggregate incorporation.
Steel: CaCO3 acts as a flux and pH regulator in water treatment and as lubricant for drawing steel rebars.
Sánchez et al. [14] defined some specification parameters for choosing raw materials for formulations of coating masses, as shown in Table 2 below.
Product | (%) of carbonates | Max. particle size of CaCO3 (μm) | Organic matter (%) | Sulfate content max. (%) | IP (%) |
---|---|---|---|---|---|
Stoned | ≤3 | ≤125 | ≤0.3 | 0.2 | 20–40 |
Porous | ≤40 | ≤125 | ≤0.3 | 0.2 | 20–40 |
Specifications for choosing raw materials.
IP: index of plasticity.
Calcium or magnesium carbonates can appear as coarse or small grains. If they are presented as large grains (>125 μm), they may not react completely, and the resulting oxides may rehydrate causing expansion.
In compositions of ceramic floor covering with low water absorption, CaCO3 acts as a flux until the limit of 3%; above this value, CaCO3 increases porosity and can be accepted up to 40% in porous coatings.
Enrique [15] recommends that the CaCO3 particle size should be less than 125 μm, because particles of larger sizes, the CaO resulting from the dissociation of carbonates when calcined at 900°C, do not react with the SiO2 present in the clays and feldspars that should form the pseudo-wollastonite and wollastonite phases, which can give rise to Ca(OH)2 formed by the hydration of CaO, when the part comes into contact with the humidity of the air, generating problems of expansion by humidity, with consequent cracking.
The ceramic tile and brick industry have grown enormously in recent years in Brazil. The clays must have sufficient plasticity to provide mechanical resistance when forming by pressing, in order to guarantee the integrity of the piece in the path between the press and the oven. The feldspar contained in the clays are sources of sodium and potassium oxides, acting as fluxes at temperatures above 800°C for bricks and above 1100°C for ceramic tiles, which facilitates the formation of a vitreous phase and reduces porosity [16, 17].
Quartz is mixed with clay during geological formation. If it is present in a smaller proportion, it helps in the formation of the vitreous phase, in the degassing of organic matter and water. However, large proportions of quartz lead to a drastic reduction in mechanical strength after firing [18]. Iron oxide is present in ceramic raw materials in the form of hematite or goethite, giving the finished product a red color.
Calcite, which appears in most clays used in the production process of ceramic tiles of type BIIb, is a mineral that needs special care in its use due to its high loss to fire. When present in a proportion equal to or less than 3%, this mineral acts as a flux. However, in higher proportions, calcite can cause an increase in the final porosity of the product. In addition, the size of the calcite particle for processing ceramics must be less than 125 μm. For larger sizes, it is observed that the CaO resulting from the dissociation of carbonates can hydrate after burning, promoting variations in the dimension of the piece. Therefore, the use of limestone clays is a challenge, requiring care in processing and control in the formulation and burning of coatings. To ensure the correct sintering of the product, proper grinding and pressing of the raw material are necessary, in addition to efficient, fast burning with the lowest possible energy consumption.
Table 3 shows the chemical compositions of a typical Brazilian limestone clay used in ceramics [19]. The chemical compositions of the raw materials were determined by X-ray fluorescence spectroscopy by wavelength dispersion (WDFRX), in a Bruker S8 Tiger equipment, in which the percentages of constituent oxides were estimated by the method semi-quantitatively. For these measurements, samples with a mass of 10.0 g were pressed as discs with 40.0 mm diameter and 4.0 mm thickness. During measurements, the samples were kept in a vacuum of 10−6 bar. A mixture of P-10 (90% argon and 10% methane) was used in the proportional counter.
Oxide (%) | C1 | C2 | C3 | C4 |
---|---|---|---|---|
SiO2 | 63.0 | 52.1 | 50.2 | 45.3 |
Al2O3 | 16.7 | 18.6 | 15.5 | 14.1 |
Fe2O3 | 4.7 | 6.8 | 6.2 | 7.1 |
CaO | 0.9 | 2.1 | 7.2 | 12.7 |
K2O | 3.8 | 4.7 | 3.2 | 3.2 |
Na2O | 0.6 | 0.4 | 0.5 | 0.7 |
MgO | 1.5 | 2.3 | 2.2 | 2.3 |
TiO2 | 0.6 | 0.8 | 0.7 | 0.8 |
L.O.I | 8.2 | 12.1 | 14.3 | 13.8 |
The results show that all clays are composed mainly of SiO2 and Al2O3. These elements are associated with clay minerals, quartz, and feldspar structures [17]. The highest amount of SiO2 was determined for sample C1. This component is important for the manufacture of ceramic tiles, as it improves workability and favors compaction. However, SiO2 can also cause low mechanical strength of sintered ceramic bodies, in addition to reducing shrinkage during firing.
The amount of Fe2O3 detected in the samples was between 4.7 and 7.1%. These values are acceptable for use in ceramic tiles, such as bricks and tiles, this element being responsible for the reddish color of the sintered pieces as well as being a powerful flux [20]. The high content of calcium oxide in C4 (12%) and C3 (7%) stands out, characterizing these clays as limestone [21]. C4 clay was previously studied in Alcântara [16], which reports the formation of stains on the ceramic bodies produced with this material, after sintering at 1120°C. This behavior was associated with a high content of CaO, estimated at 10%, which during the burning phase, the dissociation of CaCO3, promotes a high mass loss. C4 (13%) generates many pores, reducing water absorption and resistance of the final product. Thus, the higher the CaO content, the higher the CaCO3 content and in addition, the higher the mass loss.
Analyzing the levels of alkaline oxides, it is observed that the sample C2 has the highest concentration of K2O, while the concentration of Na2O is approximately the same in the four samples studied. Alkaline and alkaline earth compounds have a melting effect, which facilitates the formation of liquid phase and linear shrinkage during burning [13].
Table 4 was arranged according to the increasing amount of CaO present in the clays. Note that C1 and C2 have CaO content below 3%. According to Enrique [15], CaO acts as a flux until the limit of 3% in masses of ceramic coating. The percentage of alkali oxides (Na2O and K2O), also presented in Table 3, is another major factor for the densification process, due to the great tendency of liquid phase formation during burning. Considering the sum of the percentages of CaO and alkali oxides in samples C3 and C2, it can be concluded that C2 has a higher proportion of fluxing oxides, suggesting that this sample is the most promising. On the other hand, clays with a high limestone content, such as C3 and C4, tend to have greater porosity and less mechanical resistance after firing. Additionally, these two raw materials have lower alkaline oxide ratios than those observed for C3 and C2.
Clay | CaO (%) | Na2O + K2O (%) |
---|---|---|
C1 | 0.9 | 4.4 |
C2 | 2.1 | 5.1 |
C3 | 7.2 | 3.7 |
C4 | 12.7 | 3.9 |
The X-ray diffraction patterns of the clays are shown in Figure 7 and correlate positively with the results observed by X-ray fluorescence. The X-ray diffractometry (XRD) technique was used to determine the crystalline phases. The samples were dried in an oven at 110 °C for 24 h, ground, and passed through a 150-μm mesh sieve. The diffraction patterns were obtained in a Rigaku D-MAX 100 equipment, using Cu Kα1 radiation (λ = 1.5418 Å). All measurements were carried out in the continuous scanning mode with speed of 1°/min, in the range of 5 to 65° and in the range of 2 to 15° in samples saturated with ethylene glycol for 1 h to identify montmorillonite by displacing the diffraction peaks at smaller angles compared to dry sample testing. The crystalline phases were identified through Match! (Phase Identification by Powder Diffraction) in the demo version, according to the ICSD (Inorganic Crystal Structure Database).
X-ray diffraction patterns of the clays [
The main phases identified were quartz, kaolinite, muscovite, montmorillonite, calcite, feldspar, and hematite. Minerals from kaolinite and montmorillonite clay were identified in all analyzed clays. According to Celik [20], these clay minerals provide the necessary plasticity to guarantee conformation through the pressing process. The percentage of each crystalline phase present in the samples was estimated from the relative intensity of the main peaks in each phase. The values are shown in Table 5. The percentage of carbonates increases from 0.9% in C1 to 12.4% in C4.
Minerals (%) | C1 | C2 | C3 | C4 |
---|---|---|---|---|
Quartz | 55.7 | 51.8 | 65.1 | 57.1 |
Kaolinite | 6.3 | 10.7 | 7.4 | 5.5 |
Muscovite | 11.8 | 14.0 | 11.2 | 12.1 |
Montmorillonite | 5.6 | 4.9 | 4.6 | 6.7 |
Calcite | 8.6 | 2.8 | 1.1 | 13.7 |
Feldspar | 6.3 | 9.9 | 6.2 | 3.2 |
Hematite | 5.7 | 5.9 | 4.4 | 1.7 |
Mineralogical compositions of clays determined by XRD.
To verify the dimensional changes of expansion and thermal retraction of the samples, dilatometry tests were performed on a Netzsch dilatometer, model DIL 402PC, under synthetic air flow at 130 ml/min. For these analyses, the samples were compacted in a cylindrical shape, 12.0 mm in length and 6.0 mm in diameter. Under a constant heating rate of 10°C/min, the length of the compacted body is measured as a function of time and temperature, which varied from room temperature to 1150°C.
In Figure 8 we can observe a slight expansion in all curves up to approximately 850°C, and at 573°C, the expansion was more pronounced due to the transformation of α quartz to β [22, 23], except for C2, which presents a lower percentage of free quartz. From 573°C, there was a gradual reduction in the expansion rate, occurring or starting with sintering, followed by an exponential retraction [22].
Dilatometric curves of clays at a heating rate of 10°C/min [
The results shown in Table 5 with the percentages of CaO, Na2O, and K2O recommended by XRF measurements point out that sample C2 has a greater amount of funds (calcium carbonate up to a limit of 3% and alkaline oxides), or what is known as a greater linear shrinkage. Despite its advantages over the other samples, the C2 clay underwent deformation during firing up to 1150°C. This effect, known as pyroplastic deformation, may be due to the large proportion of funds in the sample, a high content of Fe2O3, and, even, the amount of organic matter [24]. One of the ways to control deformation during firing is to adjust the thermal cycle through the dilatometric curves, so that the plate remains within the required standards [25].
Clays containing limestone when subjected to burning, CaCO3 after heating, in the temperature range between 850 and 920°C, form CaO and release CO2. An intense endothermic peak of approximately 35–44% of the mass loss can be observed in differential thermal analysis. In ternary diagrams, it is observed that there is a eutectic point (above 1170°C), which reduces the dimensional stability in ceramic products, which can melt quickly (Figure 9).
Ternary diagram of CaO, SiO2, and Al2O3.
Clays when mixed with limestone can behave differently, as shown by Sánchez [25]. Figure 10 shows a standard clay with 5 and 10% of incorporated limestone. It was observed that as the limestone and temperature increase, respectively, the dimensional instability increases. In other words, the retraction increases constantly, when it undergoes an exponential increase, reaching the melting point.
Ceramic coating mass with incorporated calcite waste.
This phenomenon can be explained as follows: when exhibiting CaO up to the limit of 3%, this, associated with SiO2 and Al2O3 present in clays and feldspars, helps in the formation of eutectic systems at 1170°C, with consequent formation of liquid phase and contributing to obtain the desired mechanical strength and porosity. When introduced in percentages above 4%, CaCO3 levels are increased, and the composition moves from the eutectic line, forming crystalline phases such as CaSiO3 (pseudo-wollastonite) and 2CaO⋅Al2O3⋅SiO2 (gehlenite). So, a larger number of pores is left by the eliminated CO2. In this way, the porosity of the final product is increased, as shown in Figure 11. In Figure 12 is shown a photo of a clay mass with 10% calibration in which the porosity exerted can be observed.
Firing curve of a calcite clay.
Scanning electron microscopy of a ceramic with 10% of CaO.
Limestone is a contaminant for clay that above 125 μm can cause expansion and consequently cracks.
Rapid tests that mix clay with HCl can promote effervescence due to the release of CO2 and contribute to decrease the amount of limestone.
In the ceramic industry, wet grinding of components is carried out in ball mills and grinding will be more efficient if the sieves are 150 to 325 μm. In ceramic mass formulations, the amount of CaO up to 3% contributes to the formation of the vitreous phase, however, between 8 and 14%, it favors the formation of crystalline phases, reducing the absorption of water and increasing the mechanical resistance.
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