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ISBN: 978-1-119-32178-1
ISSN: 0196-6219

CONTENTS

Preface

Introduction

Geopolymers

Durability Performance of Alkali-Activated Metakaolin, Slag, Fly Ash, and Hybrids
1. Abstract
2. Introduction
3. Experimental Procedures
4. Results & Discussion
5. Summary and Conclusion
6. Acknowledgements
7. References
MICA Platelet-Reinforced Geopolymer Composites
1. Abstract
2. Introduction
3. Experimental
4. Results
5. Conclusion
6. Acknowledgements
7. References
Influence of Mix Design Parameters on Geopolymer Mechanical Properties and Microstructure
1. Abstract
2. Introduction
3. Experimental Investigation
4. Experimental Results and Discussion
5. Conclusions
6. Acknowledgements
7. References
Thermal Performance of Metakaolin-Based Geopolymers: Volume Stability and Residual Mechanical Properties
1. Abstract
2. Introduction
3. Experimental Program
4. Experimental Results and Discussion
5. Conclusions
6. Acknowledgements
7. References
Effect of Phyllosilicate Type on the Microstructure and Properties of Kaolin-Based Ceramic Tapes
1. Abstract
2. Introduction
3. Materials
4. Methods
5. Results and Discussion
6. Conclusion and Prospects
7. Acknowledgement
8. References
Effect of Alkali Cations on the Polycondensation Reaction
1. Abstract
2. Introduction
3. Experimental
4. Results
5. Discussion
6. Conclusions
7. References
Development of a Mold for Thermoplastics Based on a Phosphate Cement
1. Abstract
2. Introduction
3. Experimental Work
4. Results and Discussion
5. Proof of Concept
6. Conclusions
7. References
Properties of Cork Particle Reinforced Sodium Geopolymer Composites
1. Abstract
2. Introduction
3. Experimental Procedure
4. Results and Discussion
5. Conclusion
6. Acknowledgement
7. References
The Role of Alkaline Earth Ions in Geopolymer Binder Formation
1. Abstract
2. Introduction
3. Experimental Part
4. Results and Discussion
5. Conclusion
6. References
Investigations of the Thermally Induced Hydrogen Release of NaBH₄, NH₃BH₃ and Their Geopolymer Composites
1. Abstract
2. Introduction
3. Experimental
4. Results and Discussion
5. Conclusion
6. References
IR-Spectroscopic Investigation of Geopolymer and CSH-Phase Stability on Heating Temperature in Post-Fired Building Materials
1. Abstract
2. Introduction
3. Experimental
4. Results and Discussion
5. Conclusions
6. References
Mixed Alkali Regional Metakaolin-based Geopolymer
1. Abstract
2. Introduction
3. Experimental Procedures
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References
Bamboo-Geopolymer Composite: A Preliminary Study
1. Abstract
2. Introduction
3. Materials and Methods
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References
Metakaolin-Based Geopolymer Cements from Commercial Sodium Waterglass and Sodium Waterglass from Rice Husk Ash: A Comparative Study
1. Abstract
2. Introduction
3. Materials and Experimental Methods
4. Results and Discussion
5. Conclusion
6. Acknowledgments
7. References
Recycling of Grog by Addition into Heavy Clay Ceramic Manufacturing
1. Abstract
2. Introduction
3. Materials and Methods
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References

Virtual Materials Design and Ceramic Genome

Q-State Monte Carlo Simulations of Magnetic Anisotropy Applied to Paramagnetic and Diamagnetic Materials
1. Abstract
2. Introduction
3. The Model
4. Results
5. Conclusions
6. Acknowledgments
7. References
First Principles Study of Defect Formation in Bulk B₆O
1. Abstract
2. Introduction
3. Computational Details
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References
Modeling of Damage in an MMC with Lamellar Microstructure
1. Abstract
2. Introduction
3. Materials and Experimental
4. Analytical Modelling
5. FE Modelling
6. Results and Discussion
7. Conclusions and Outlook
8. Acknowledgement
9. References
Micro-Computed Tomography Image based Thermo-Elastic Properties Studies of Freeze-Cast MMC
1. Abstract
2. Introduction
3. Materials and Experimental
4. Material Modelling and Discussion
5. Conclusions
6. Acknowledgement
7. References

Materials for Extreme Environments

Densification and Phase Evolution of SHS Derived Ti₂AlN Active Precursor Powders During Hot Pressing Processes
1. Abstract
2. Introduction
3. Preparation
4. Results and Discussion
5. Conclusions
6. Acknowledgments
7. References
Max Phase Materials for Nuclear Applications
1. Abstract
2. Introduction
3. Experimental
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References
Analysis of Dynamic Young's Modulus and Damping Behavior of ZrB₂-SiC Composites by the Impulse Excitation Technique
1. Abstract
2. Introduction
3. Experimental Methods
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References

Advanced Ceramic Coatings

Study of Effect of Hafnium Addition on Oxidation Resistance of βNiAl Coatings Prepared by an in-situ Chemical Vapour Deposition Method
1. Abstract
2. Introduction
3. Experimental
4. Results
5. TGO
6. Discussion
7. Conclusions
8. Acknowledgments
9. References
Mass Transfer Mechanism in Mullite Under Oxygen Potential Gradients at High Temperatures
1. Abstract
2. Introduction
3. Experimental
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References

Emerging Technologies— Carbon Nanostructures

SnO₂-Reduced Graphene Oxide Nanocomposite for Ethanol Sensing at Room Temperature
1. Abstract
2. Introduction
3. Experimental
4. Results and Discussion
5. Conclusions
6. Acknowledgements
7. References

Author Index

EULA

List of Tables

Chapter 1

Table 1 Chemical composition of solid materials (wt%)
Table 2 Mixture proportion of alkali-activated metakaolin (AAMK), fly ash (AAB), slag (AAH) and hybrids in weight ratio
Table 3 Mixture proportions of OPC, modified-OPC, and AAC mortar prisms

Chapter 2

Table 1 Thermal conductivity of geopolymer composites as a function of mica content

Chapter 3

Table 1 Chemical composition of Meta Max (Metakaolin from BASF Co., Germany)
Table 2 Mix proportion of metakaolin geopolymers

Chapter 4

Table I Chemical composition (by weight) of MetaMax (Metakaolin from BASF)
Table II Mix proportion of metakaolin geopolymers

Chapter 5

Table 1 Chemical compositions (wt.%) of the different clays
Table 2 Characteristic sizes and other physical parameters of kaolin, talc and palygorskite

Chapter 6

Table 1 Physical and chemical feature of silicate solutions before and after the addition of hydroxide pellets
Table 2 Physical and chemical features of metakaolin

Chapter 9

Table 1 The chemical compositions of the various geopolymer binders with A= Ca, Mg or Sr

Chapter 11

Table 1 Compressive strength of samples AAMK and AAH

Chapter 12

Table 1 Chemical composition of KA and MKA by XRF
Table 2 Average compressive strength of 25x50-mm tested samples with Weibull parameters
Table 3 Average 4-point flexural strength of 30x12-mm tested samples with Weibull parameters

Chapter 13

Table 1 Third-point loading flexural strength results and Weibull parameters

Chapter 14

Table 1 Chemical composition of Dibo, RHA and PRHA in mass percent
Table 2 Compressive strength of geopolymer cements (MPa), the values of main band on the IR spectra of geopolymer cements (cm^-1) and mass loss (%)

Chapter 15

Table I Chemical composition of the raw materials (wt %)

Chapter 17

Table I Change in cohesive energy (Δ CE) and Percent Unit Cell Volume Contraction for single and multi-atom 1^st, 2^nd, 3^rd, and 4^th nearest neighboring vacancies in B₆O. See Figure 2 for site notation. Note: B_{p-intericosahedral} is the inter-icosahedral link to a polar boron site from nearest neighboring boron icosahedra and Ochain is the nearest neighboring oxygen to O1

Chapter 18

Table 1

Chapter 20

Table I Phase composition of Ti₂AlN SHS synthesis products
Table II Phase evolution of hot-pressed SHS derived Ti₂AlN powders obtained as a result of synthesis of 3Al + 4 Ti₃Al under 1.5 atm. nitrogen pressure [wt.%]
Table III Phase evolution of hot-pressed SHS derived Ti₂AlN powders obtained as a result of synthesis of 2Al + 4 Ti₃Al under 1.5 atm. nitrogen pressure [wt.%]
Table IV Phase evolution of hot-pressed SHS derived Ti₂AlN powders obtained as a result of synthesis of 2Al + 4 Ti₃Al under 5 atm. nitrogen pressure [wt.%]
Table V Apparent densities of hot-pressed Ti₂AlN materials [g/cm³]

Chapter 21

Table 1 The investigated Zr-Al-C starting compositions, sintering temperatures and identified phase assemblies. The majority phases are indicated in bold. The composition of the Zr₄AlC₃, Zr₃AlC₂ and Zr₂AlC nominal stoichiometries are presented in the bottom three rows
Table 2 Experimental lattice parameters for the Zr₂AlC and Zr₃AlC₂ compounds, as obtained by Rietveld refinement of the XRD spectra
Table 3 Mechanical properties of Nb₄AlC₃ and (Nb_0.85,Zr_0.15)₄AlC₃ at room temperature

Chapter 22

Table I Mechanical properties of ZrB₂-SiC composites
Table II Coefficients A₀, A₁ and A₂ of (3) with T in (°C) and E in (GPa), obtained from the best fits to the experimental data shown in Figure 4. In the last column, the goodness of the fit is given by the coefficient of determination R²
Table III Damping peaks and temperature for each ZrB₂-SiC composite

Chapter 23

Table 1 show an averaged EDS point analysis taken at different locations of coating cross-sections as-deposited condition

List of Illustrations

Chapter 1

Figure 1 Comparison between FTIR spectra of AAC (K0.6 series) before and after the accelerated carbonation test, exposed to CO₂ concentration of 3 vol% for 9 days
Figure 2 A comparison between OPC and AAC mortars immersed in H₂SO₄ with pH 0.5: weeks, and (c) AAC mortars with AAC coating layer at 11 weeks
Figure 3 AAMK and AAFA mortars (K0.5 and K0.64) immersed in H₂SO₄ with pH 0.5: (a) after 2 days, (b) after 9 weeks
Figure 4 AAMK and AAH mortars (K0.5 and K0.64) immersed in H₂SO₄ with pH. 0.5: (a) after 2 days, (b) after 9 weeks
Figure 5 AAB and AAB/MK mortars (K0.5 and K0.64) immersed in H₂SO₄ with pH 0.5: (a) after 2 days, (b) after 9 weeks
Figure 6 AAH and AAH/MK mortars (K0.5 and K0.64) immersed in H₂SO₄ with pH 0.5: (a) after 2 days, (b) after 9 weeks

Chapter 2

Figure 1 Increasing flexure strength with mica content at room temperature, as indicated from left to right
Figure 2 Increase in flexure strength with mica content after 700 °C heat treatment. Samples without mica were too weak to test after heat treatment
Figure 3 Effect of heat treating 20 wt% mica in K-GP composite, with temperatures being read from left to right
Figure 4 Thermal conductivity as a function of mica content. Square symbols indicate 24 h of equilibration, while diamond symbols indicate only 3 h of equilibration
Figure 5 SEM micrograph of pure mica platelets between 100 and 5 microns in diameter
Figure 6 SEM micrograph of 20 weight percent mica in K-GP with no heat treatment
Figure 7 SEM micrograph of 20 wt % mica in K-GP after 1 hour at 700 °C
Figure 8 SEM micrograph of 20 weight percent mica in K-GP after 1 hour at 700°C

Chapter 3

Figure 1 Geopolymer Synthesis
Figure 2 Density of geopolymers (a) Density vs w/solids for different Si/Al ratios (b) Compressive strength Vs density for all the geopolymer samples
Figure 3 Analysis of compressive strength data (a) Plot for compressive strength versus Si/Al (b) Plot for compressive strength versus w/solids
Figure 3 Analysis of the compressive strength data (c) Plot for compressive strength versus Al/Na (d) Plot for compressive strength versus H₂O/Na₂O
Figure 4 SEM images of geopolymers with Si/Al 1.03 and 2.0 observed at magnification level 10k

Chapter 4

Figure 1 Visual observation of metakaolin geopolymer specimens (50 mm cubes) after subject to elevated temperature
Figure 2 The volume shrinkage of geopolymer cube specimens with different Si/Al ratios after exposure to high temperature
Figure 3 Weight loss of cube specimens with different Si/Al ratios when exposed to high temperature
Figure 4 Influences of Si/Al and temperature on microstructure of MK-geopolymers
Figure 5 Residual compressive strength vs Si/Al after different temperature exposures
Figure 6 Cement paste disintegrated at 900°C
Figure 7 Variation in residual density of geopolymers with Si/Al ratio

Chapter 5

Figure 1 Typical structure of (a) kaolinite, (b) talc and (c) palygorskite minerals
Figure 2 Simplified representation of a tape casting set-up and slurry preparation
Figure 3 Thermal analysis diagrams of the starting talc clay
Figure 4 Thermal analysis curves of typical kaolin-palygorskite tapes a) DTA-TG and b) thermodilatometry. Heating rate = 5°C/min under dry air
Figure 5 Biaxial flexural strength of some green and sintered (1100°C) kaolin-palygorskite samples. For each series from left to right: green tape 1.6 mm; sintered tape 1.6 mm; green tape 1 mmm and sintered tape 1 mm
Figure 6 SEM micrographs and open porosity values of the kaolin-palygorskite samples before and after firing at 1100°C
Figure 7 DTA-TG and DTG curves for the K50T50 sample (heating rate = 5°C/min, dry air)
Figure 8 a) Open porosity (from left to right: 900, 1000 and 1100°C) and b) stress to rupture values for some kaolin-talc tapes upon firing (from left to right: K90T10, K50T50 and T100)

Chapter 6

Figure 1 FTIR spectra of (A) SN_Na, (B) S1_K and (C) S3_K solutions before and after the addition of MOH hydroxide pellets
Figure 2 Infrared spectra of [S3_K^KOH] mixture at various time
Figure 3 Evolution of the Si-O-M peak position as a function of time for (a) ▄ [SN_Na^NaOH], A [S1_K^KOH], and o [S3_K^KOH] and (b) □ [SN_Na^KOH], ▴ [S1_K^NaOH], and • [S3_K^NaOH]
Figure 4 Evolution of the specific compressive strength (σ_ρ) values versus the Si molar concentration for the different samples [Sx_M ^MOH] (▄ SN_Na^NaOH, □ SN_Na^KOH ▄ S1_K^NaOH, ▴ S1_K^KOH, • S3_K^NaOH, and O S3_K^KOH)

Chapter 7

Figure 1 View of the digital image correlation (DIC) test setup
Figure 2 XRD diffractograms for partially and fully cured specimens for the three curing regimes, at the right hand side, reference diffractograms are given (http://webmineral.com/data/)
Figure 3 Average linear deformation during 1st heating and cooling cycle (RT - 300°C - RT) for different curing methods. As all specimen shrink only negative deformations are observed
Figure 4 Comparison of tensile stress-strain curves cured at RT and 60°C
Figure 5 (a). The master mold in wooden
Figure 5 (b). Master model covered with frame wax sheet
Figure 6 Workability of topcoat with AEROSIL and Dupont Alesta HR filler
Figure 7 (a). Impregnation of the CSM with
Figure 7 (b). Impregnation of the CSM with topcoat. Vubonite matrix
Figure 8 Matched die TRC mold
Figure 9 Mold placed in the industrial press
Figure 10 Thermoformed Twintex part

Chapter 8

Fig 1 Plot of four-point flexural strength vs. solids loading for cork particle reinforced sodium geopolymer. An increase in flexural strength as solids loading increased was noted
Fig 2 Measured flexure stress vs. flexure strain for a sample in the 60 wt% cork sample group

Chapter 9

Figure 1 (A) The protocol for the synthesis of the geopolymer binder with A = Ca, Mg or Sr (B) The molar composition of different mixtures of ternary Si-Al-(Na+Ca) /O ((•)
Figure 2 (A) The evolution of the FTIR spectrum of sample C1sol (B) The intensity ratio (Si-O-CaO / H₂O) as a function of the nCa /nSi ratio at (•) 0, (▄) 60, (▴) 90 and ▴ 120 min
Figure 3 (A) Thermal analysis curves obtained at 25 and 70°C (B) Mass losses for different samples
Figure 4 Diffractograms of different samples: (A) Anatase 00-021-1272 (B) Calcium aluminum oxide carbonate hydrate 00-041-0219 (Q) Quartz 00-003-0419 (T) Thermonatrite 00-008-0448 (C) Calcite 01-072-1937 (H) Calcium hydroxide 00-033-0268
Figure 5 (A) Infrared spectra at 12 h for samples (a) (b) (B) XRD patterns of the same samples ((Q) Quartz 00-003-0419 (B) hydrated calcium phase 00-041-0219 (T) Thermonatrite 00-008-0448 (C) Calcite 01-072-1937 (M) Magnesium hydroxide 04-011-5938 (S) Strontianite 00-005-0418)
Figure 6 Thermal analyses of different samples
Figure 7 SEM micrographs of (A) (B) and (C)

Chapter 10

Figure 1 TG, dTG (dashed line) and heat flow curves of AB-G heated under synthetic air to 300°C
Figure 2 TIR spectra of (a) AB and (b) AB-G in KBr matrix. The IR modes of BH₄⁻ in KBr matrix are indicated
Figure 3 TIR spectra of (a) AB and (b) AB-G in KBr in the presence of NaNO₃ tracer from 25 to 180°C, in the spectral range between 600 and 1800 cm^-1. Asterisks indicate the BH₄⁻ peak at 1123 cm^-1 (ν₄) and the NH₂ deformation mode at 1566 cm^-1
Figure 4 Variation of the integral intensity of ν₂(NO₃⁻) of NaNO₃ tracer for AB (stars) and AB-G (squares) as a function of the temperature in the TIR spectra using NaNO₃ tracer, in comparison with the thermal behavior of a reference NaNO₃/KBr pellet (open circles). The heat flow curve of AB-G (dashed line) is overlaid for comparison
Figure 5 TG/DTA of SB-G under He (upper graph, dashed line is for dTG) and under synthetic air (lower graph, solid and dash-dotted lines are for the measurements performed with and without pre-evacuating the samples before the heating runs, respectively)
Figure 6 TG/DTA of SB under synthetic air (upper graph, solid and dash-dotted lines are for the measurements performed with and without pre-evacuating the samples before the heating runs, respectively) and under He (lower graph, dashed line is for dTG)
Figure 7 TIR spectra of SB/KBr (at the left side). At the right side, the corresponding spectra are zoomed between 1200 and 1700 cm^-1. Asterisks are used to follow the intermediary peak at 1575 cm^-1. Dashed lines are for the TIR spectra between 400 and 1800 cm^-1 in the presence of NaNO₃
Figure 8 Integrated intensities (Int. I) of B₃O₆³⁻ (triangles), BH₄⁻ (circles), NO₃⁻ (filled-square) in TIR of SB/KBr in the presence of NaNO₃ tracer. Non-filled squares are for the reference pellet NaNO₃/KBr. Integral intensities are for the TIR spectra of samples cooled down to 25°C from T as denoted (lines are guide for eyes)

Chapter 11

Figure 1 IR-absorption spectra (KBr-method) of hardened cement pastes CEM I 52,5 N (= CEM I), CEM III/B 42,5 N (=CEM III), CEM I with the addition of 50% H (CEM I_H), unheated and heated at 600°C (gray)
Figure 2 XRD pattern of hardened cement paste CEM I 52,5 N (= CEM I) unheated and at 600°C (gray) and their difference as denoted. Some peak positions has been marked (CSH_* by arrows)
Figure 3 IR absorption spectra (KBr-method) of CEM I 42,5 R based series of cement pastes
Figure 4 IR absorption spectra (ATR method) in relative transmissivity of CEM I 42,5 R based series of cement pastes
Figure 5 Density of states peak maximum (DOSPM) of the asymmetric Si-O vibration (ATR-method) of series of samples as denoted
Figure 6 Density of states peak maximum (DOSPM) of the asymmetric Si-O vibration (ATR-method) of series of mortars compared to their compressive strength behavior
Figure 7 Density of states peak maximum (DOSPM) of the asymmetric Si-O vibration of series of concretes (Micro-IR in transmission mode of probes pressed between diamond plates)
Figure 8 XRD pattern of AAMK and AAH (a, right) and AAH compared to CEM III and CEM I (b, left). Details are given in the text
Figure 9 IR absorption spectra (KBr-method) of 3 examples of AAH samples, unheated, 600°C and 800°C heated each (AAH₁ with WG₁, AAH₂ and AAH₃ with WG₂, compare experimental)
Figure 10 IR absorption spectra of AAMK samples unheated (two spectra) and heated at 800°C taken from a solid piece and fine material after the strength measurement

Chapter 12

Figure 1 (A) Water-treated bamboo culms; (B) water-treated BF1W reinforcement; (C) washed BF4W reinforcement just before use
Figure 2 (A) Potassium-Sodium water glass K75Na25-WG; (B) Amazonian metakaolin MKA
Figure 3 Cylindrical compressive 25x50-mm specimens MKA76 GPC
Figure 4 Four-point flexural plate and specimen MKA76-BF GPC
Figure 5 TGA for KA
Figure 6 (A) KA and (B) MKA XRD, 2Θ 5°-80°
Figure 7 SEM of K75Na25-MKA76 GP
Figure 8 SEM of K75Na25-MKA76-BF4W GPC showing imprints of the pulled out BFs
Figure 9 Typical stress-strain curve for BF4W GPC tested in bending. Strain units are in percent

Chapter 13

Figure 1 Green bamboo (a) culms, (b) chips and (c) fiber bundles
Figure 2 Bamboo-reinforced geopolymer composite (a) plate and (b) tested specimens
Figure 3 SEM micrographs of bamboo-reinforced K-based geopolymer composite tested specimen, showing gaps and crack propagation in back scattered composite (BEC) mode, 230x and BEC mode, 150x
Figure 4 SEM micrographs of untreated Guadua BF, showing starch (small-round particles) in the parenchymal cells in secondary electron (SEI) and back scattered (BES) modes, 500x
Figure 5 Stress-strain curves for bamboo-reinforced K-based geopolymer composite tested in four-point bending
Figure 6 Weibull plot for flexural strength data of bamboo-reinforced geopolymer composite
Figure 7 XRD pattern of bamboo-reinforced geopolymer composite

Chapter 14

Figure 1 X-ray pattern of metakaolin, MK. (I, A and Q denote peaks of illite, anatase and quartz respectively)
Figure 2 X-ray patterns of rice husk ash (RHA) and pure rice husk ash (PRHA)
Figure 3 IR spectra of rice husk ash (RHA) and pure rice husk ash (PRHA)
Figure 4 IR spectra of metakaolin (MK) and quartz subtracted (MK-0.25 quartz) in comparison to quartz
Figure 5 ATR-IR spectra of sodium waterglass (S1, S2 and S3)
Figure 6 XRD patterns of geopolymers cements Geo1, Geo2, Geo3. A and Q denote peaks of anatase and quartz respectively
Figure 7 Difference XRD patterns of samples as denoted
Figure 8 IR absorption spectra of samples Geo1, Geo2 and Geo3 at 28 days
Figure 9 Evolution of the values of compressive strength as a function of mass loss and the values of the wavenumber of the main bands of geopolymer cements Geo1, Geo2 and Geo3
Figure 10 Difference IR spectra of samples as denoted
Figure 11 TG curves of geopolymers cements Geo1, Geo2, Geo3

Chapter 15

Figure 1 XRD patterns of the raw materials. A: amphibole; K: kaolinite; M: micaceous mineral; Q: quartz
Figure 2 Particle size distribution of the raw materials
Figure 3 DTA/TG curves of the grog
Figure 4 Prognostic of the extrusion stage through the Atteberg's plasticity limits¹⁴
Figure 5 Linear shrinkage of the compositions
Figure 6 Correlations among amount of grog incorporated and increased linear fired shrinkage and decreased linear dried shrinkage
Figure 7 Water absorption and flexural rupture strength of the compositions

Chapter 16

Figure 1 Magnetic anisotropy between grains ρ₁ and ρ₂ promotes grain boundary mobility in the direction of the largest free energy; in this case towards grain ρ₁
Figure 2 Magnetic field and c-axis vectors relative to the rolling, transverse and normal directions
Figure 4 Grain growth contours at t=0 and t=200 MCS for WMF (a,b) and WOMF (d,e) representative hexagonal polycrystalline materials; Also shown is the WMF/WOMF evolutions of average grain size (c) and total grain boundary energy (f)
Figure 5 WOMF/WMF misorientation angle distributions corresponding to Case 1 at t = 200 MCS for representative hexagonal and cubic polycrystalline materials
Figure 6 WOMF/WMF Ф distributions corresponding to Case 1 at t = 200 MCS for representative hexagonal and cubic polycrystalline materials
Figure 7 WOMF/WMF Misorientation distributions corresponding to Case 2 at t = 200 MCS for representative hexagonal and cubic polycrystalline materials
Figure 8 WOMF/WMF Ф distributions corresponding to Case 2 at t = 200 MCS for representative hexagonal (a) and cubic (b) polycrystalline materials

Chapter 17

Figure 1 Crystal structure of pristine 2x2x1 B₆O unit cell. Left: off-axis view; Right: perpendicular to c-axis; B and O atoms are pink and red respectively
Figure 2 Site Notation for single boron icosahedra from unit cell identifying vacancy locations which correspond to notation in Table I
Figure 3 ELF iso-slices through different atomic planes of pristine B₆O with (right) and without (left) a single vacancy. (a) Slice perpendicular to c-axis through O1 in B₆O (Left) and through O1 vacancy (Right) (b) Slice along <110> through atomic plane containing O_chain-O₁-Be₁ in B₆O (Left) and with O₁ vacancy (Right) (c) Slice perpendicular to c-axis through diameter of icosahedra in B₆O (Left) and with B_e6 vacancy (Right) (d) Slice through O_chain-O_chain-B_e6 in B_6O (Left) and with B_e6 vacancy (Right) (e) Slice through B_p- B_p- B_p plane within icosahedra in B_6O (Left) and with B_e6 vacancy (Right) (f) Slice through B_p- B_p- B_p plane within icosahedra in B_6O (Left) and with B_p1 vacancy (Right) (g) Slice through plane containing inter-icosahedra Bp-Bp1 bonds in pristine B_6O (Left) and with Bp1 vacancy (Right). Red indicates areas where ELF = 1, whereas ELF = 0 for the dark blue region. The atoms and bonds that are shown as connected balls and sticks exist in the plane slice, whereas the atoms displayed as lines are exterior. Pink and red balls represent boron and oxygen respectively
Figure 4 Local defect structure and relative defect energies for single atom and multi-atom vacancies. See Figure 3 for notation explanation and Table I for corresponding unit cell contractions and changes in cohesive energy

Chapter 18

Figure 1 SEM micrographs showing the progressive damage evolution in one region in single-domain sample at different applied stresses. A compressive load was applied at 45° to the domain orientation (=horizontal direction). The actual stress–strain plot is shown in the image. The micrographs correspond to the locations marked by the numbers on the stress–strain plot
Figure 2 a) Schematics showing a composite sample with multiple cracks in the ceramic layer; b) representative segment bounded by two cracks without crack widening; c) representative segment bounded by two cracks with crack widening 2l
Figure 3 FE model of a quarter of the representative segment with thicknesses 2h_c and h_m of the ceramic and metallic layers. 2s is the crack spacing und 2l is the crack widening
Figure 4 Normalized axial stress in the ceramic layer as a function of co-ordinate x₂ for a range of crack spacing to layer thickness ratios as predicted by the analytical model: a) no widening D_w = 0; b) with relative crack widening D_w = 10%
Figure 5 Axial stress distribution in the cracked ceramic layer for three crack half-spacing to layer thickness ratios: a) s/h_c =1.3 ; b) s/h_c =1.0; c) s/h_c =0.7. No crack widening
Figure 6 Axial stress distribution in the cracked ceramic layer for s /h_c = 1.3 : a) without crack widening D_w = 0; b) with relative crack widening D_w = 10%; c) with relative crack widening D_w =15%
Figure 7 Axial stress distribution in the ceramic layer for s / h_c = 1.0: a) without crack widening D_w =0; b) with relative crack widening D_w = 10%; c) with relative crack widening D_w =15%
Figure 8 Shear stress distribution in the cracked ceramic layer for three crack half-spacing to layer thickness ratio s/h_c =1.3: a) without crack widening D_w = 0; b) with relative crack widening D_w = 10%; c) with relative crack widening D_w =15%

Chapter 19

Figure 1 μCT pictures for 2D and 3D model with a) 100³ voxels (single domain structure) and b) 250³ voxels (poly domain structure); c) ABAQUS finite element model 100x100x100 elements
Figure 2 Variation of the ceramic content along the axes a) Z and b) Y; c) normal and d) shear components of the stiffness tensor
Figure 3 Comparison of experimental measurements⁹ with modeling results (3D model)
Figure 4 3D Microstructure view for different specimens used for thermal studies: a) T3, b) T4, c) T5 consisting of 375x375x75 voxels; 2D singe slices for d) T3, e) T4, f) T5 (in this image ceramic is white) (750x750 grey)
Figure 5 a) Heat conductivity calculated using 2D and 3D models of the microstructure (see Figure 4), b) thermal expansion calculated using 2D and 3D models of the microstructure (see Figure 1)
Figure 6 Experimental and modeling results for thermal conductivity of the ceramic preform for following models: 1) 375x375x75 voxels; 31% alumina; 2) 250x250x250 voxels ; 44% alumina and comparing with analytical models
Figure 7 Experimental and modeling results for thermal conductivity of the composite (31% alumina). The experimental measurements were provided parallel and perpendicular to the freeze-casting direction. Calculations were provided using FE for the microstructures T3 and T5 (see Figure 4)

Chapter 20

Figure 1 XRD pattern of the large Ti₂AlN powders obtained by SHS reaction 2 under 5 atm. nitrogen pressure
Figure 2 Morphology of SHS derived Ti2AlN powders
Figure3 XRD pattern of the Ti₂AlN sample hot-pressed at 1300°C

Chapter 21

Figure 1 Ternary Zr-Al-C phase diagram showing the different Zr₄Al_wC_x (in blue) and Zr₃Al_yC_z (in black) starting compositions (see Table 1), together with the Zr_n+1AlC_n reference compositions (in red)
Figure 2 XRD patterns of the Zr₄Al_wC_x ceramics hot pressed at 1550°C (a) and Zr₃Al_yC_z ceramics hot pressed at 1525°C (b)
Figure 3 HRTEM images of Zr₃AlC₂ (a) and Zr₂AlC (b) combined with a mapped atomic stacking (green = Zr, blue = Al, grey = C)
Figure 4 Lattice parameters of (Nb_1-x,Zr_x)₄AlC₃ as function of the composition (a) and backscattered electron (BSE) detector images of the microstructure of Nb₄AlC₃ and (Nb_0.85,Zr_0.15)₄AlC₃ (b). The black dots are Al₂O₃ particles
Figure 5 The dynamic elastic properties of Nb₄AlC₃ and (Nb_0.85,Zr_0.15)₄AlC₃ as function of temperature plotted together with the temperature dependence of the 4-point flexural strength of (Nb_0.85,Zr_0.15)₄AlC₃

Chapter 22

Figure 1 Schematic of the sintering cycles (S1 and S2) used during PECS
Figure 2 Particle morphology of commercial (a) and self-synthesized (b) ZrB₂ powders
Figure 3 Backscattered SEM micrographs of ZrB₂-SiC ceramics, CZS-S1, SZS-S1(a) and CZS-S2, SZS-S2(b) prepared by sintering cycle S1 and S2 respectively
Figure 4 Temperature dependent Young's modulus and damping spectra of ZrB₂-SiC composites prepared by sintering cycle S1 (a) and S2 (b)

Chapter 23

Figure 1a - f shows the cross-sections of the undoped βNiAl and Hf-βNiAl samples in as-deposited condition with EDS line profile across the thickness and (g) corresponding XRD spectra of the coatings
Figure 2 shows the TGO morphologies; (a) - (c) simple βNiAl and (d) - (f) Hf-βNiAl. Typical ridge morphology, thick and multiphase TGO is observed in simple βNiAl while similar ridge and essentially single phase TGO is seen in Hf-βNiAl
Figure 3 shows the TGO growth rates and stresses of both doped and undoped coatings after oxidation (at 1150oC for 100 hours in air)

Chapter 24

Figure 1 Effect of P_o2 in the upper chamber on the oxygen permeability constants (PL·S_gb^-1) of polycrystalline mullite and Al₂O₃ at 1873 K. The P_o2 in the lower chamber was constant at 1 Pa
Figure 2 SEM micrograph of the P_o2(hi) surface and a cross-section of a mullite wafer exposed to a P_o2(hi)/P_o2(lo) ratio of 10⁵ Pa/1 Pa at 1873 K for 10 h
Figure 3 Equilibrium partial pressures Pi of the primary volatile species for mullite under a total pressure of 10⁵ Pa
Figure 4 Arrhenius plots of the |A_i|·S_gb^-1 values of polycrystalline mullite wafers exposed to P_o2(hi)/P_o2(lo) ratios of 1 Pa/(10^-9–10^-6) Pa for oxygen and 10⁵ Pa/1 Pa for Al, respectively
Figure 5 Oxygen permeability constants (PL·S_gb^-1) of polycrystalline mullite as functions of the P_o2(hi)/P_o2(lo) ratio at 1873 K. P_o2(lo) was held constant at 10^-6 Pa
Figure 6 SEM micrograph of a cross-section of the P_o2(hi) surface of a mullite wafer exposed to a P_o2(hi)/P_o2(lo) ratio of 10⁵ Pa/10^-6 Pa at 1873 K for 10 h
Figure 7 SEM micrograph of a cross-section in the vicinity of the P_o2(lo) surface of a mullite wafer exposed to a P_o2(hi)/P_o2(lo) ratio of 10⁵ Pa/10^-6 Pa at 1873 K for 10 h

Chapter 25

Figure 1 XRD patterns of (a) graphite oxide (GO), (b) SnO₂-RGO nanocomposite
Figure 2 FTIR spectrum of (a) graphite oxide (GO), (b) SnO₂-RGO nanocomposite
Figure 3 FESEM images of SnO₂-RGO of (a,b) low magnification, (c) high magnification. (d) EDS spectrum of SnO₂-RGO
Figure 4 (a) TEM image, (b) HRTEM image, and (c) SAED pattern of SnO₂-RGO sample
Figure 5 Response of SnO₂-RGO as function of ethanol concentration at room temperature
Figure 6 Responses of SnO₂-RGO to ethanol and methanol (1,000 ppm) at room temperature

Preface

This CESP proceedings issue contains a total of 25 contributions from select symposia held during the 40th International Conference on Advanced Ceramics and Composites (ICACC), in Daytona Beach, FL, January 24–29, 2016.

The wide range of topics in this issue were presented in the following Symposia and Focused Sessions:

Symposium 2—Advanced Ceramic Coatings for Structural, Environmental, and Functional Applications
Symposium 10—Virtual Materials (Computational) Design and Ceramic Genome
Symposium 12—Materials for Extreme Environments: Ultrahigh Temperature Ceramics and Nanolaminated Ternary Carbides and Nitrides
Focused Session 1—Geopolymers and Chemically Bonded Ceramics
Emerging Technologies Symposium on Carbon Nanostructures

The editors wish to thank the symposium organizers for their time and efforts, the authors and presenters for their contributions; and the reviewers for their valuable comments and suggestions. In addition, acknowledgments are due to the officers of the Engineering Ceramics Division of The American Ceramic Society and the 2016 ICACC program chair, Andrew Gyekenyesi, for their support. It is the hope that this volume becomes a useful resource for academic, governmental, and industrial efforts.

WALTRAUD M. KRIVEN, University of Illinois at Urbana-Champaign, USA JINGYANG WANG, Institute of Metal Research, Chinese Academy of Sciences, China YANCHUN ZHOU, Aerospace Research Institute of Material & Processing Technology, China

DONGMING ZHU, NASA Glenn Research Center, USA
GUSTAVO COSTA, NASA Glenn Research Center, USA

Introduction

This collected proceedings consists of 104 papers that were submitted and approved for the proceedings of the 40th International Conference on Advanced Ceramics and Composites (ICACC), held January 24–29, 2016 in Daytona Beach, Florida. ICACC is the most prominent international meeting in the area of advanced structural, functional, and nanoscopic ceramics, composites, and other emerging ceramic materials and technologies. This prestigious conference has been organized by the Engineering Ceramics Division (ECD) of The American Ceramic Society (ACerS) since 1977. This year's meeting continued the tradition and added a few grand celebrations to mark its 40th year.

The 40th ICACC hosted more than 1,100 attendees from 42 countries that gave over 900 presentations. The topics ranged from ceramic nanomaterials to structural reliability of ceramic components, which demonstrated the linkage between materials science developments at the atomic level and macro level structural applications. Papers addressed material, model, and component development and investigated the interrelations between the processing, properties, and microstructure of ceramic materials.

The 2016 conference was organized into the following 17 symposia and 5 Focused Sessions:

Symposium 1	Mechanical Behavior and Performance of Ceramics and Composites
Symposium 2	Advanced Ceramic Coatings for Structural, Environmental, and Functional Applications
Symposium 3	13th International Symposium on Solid Oxide Fuel Cells (SOFC): Materials, Science, and Technology
Symposium 4	Armor Ceramics: Challenges and New Developments
Symposium 5	Next Generation Bioceramics and Biocomposites
Symposium 6	Advanced Materials and Technologies for Direct Thermal Energy Conversion and Rechargeable Energy Storage
Symposium 7	10th International Symposium on Nanostructured Materials: Functional Nanomaterials and Thin Films for Sustainable Energy Harvesting, Environmental and Health Applications
Symposium 8	10th International Symposium on Advanced Processing & Manufacturing Technologies for Structural & Multifunctional Materials and Systems
Symposium 9	Porous Ceramics: Novel Developments and Applications
Symposium 10	Virtual Materials (Computational) Design and Ceramic Genome
Symposium 11	Advanced Materials and Innovative Processing ideas for the Production Root Technology
Symposium 11	Materials for Extreme Environments: Ultrahigh Temperature Ceramics (UHTCs) and Nano-laminated
Symposium 12	Ternary Carbides and Nitrides (MAX Phases)
Symposium 13	Advanced Materials for Sustainable Nuclear Fission and Fusion Energy
Symposium 14	Crystalline Materials for Electrical, Optical and Medical Applications
Focused Session 1	Geopolymers, Chemically Bonded Ceramics, Eco-friendly and Sustainable Materials
Focused Session 2	Advanced Ceramic Materials and Processing for Photonics and Energy
Focused Session 3	Materials Diagnostics and Structural Health Monitoring of Ceramic Components and Systems
Focused Session 4	Additive Manufacturing and 3D Printing Technologies
Focused Session 5	Field Assisted Sintering and Related Phenomena at High Temperatures
Focused Session 6	Hybrid Materials and Processing Technologies
Focused Session 7	40th Jubilee Symposium: Engineered Ceramics'Current Status and Future Prospects
Special Symposium	5th Global Young Investigators Forum
Special Symposium	Emerging Technologies Symposium: Carbon Nanostructures and 2D Materials and Composites

The proceedings papers from this conference are published in the below seven issues of the 2016 CESP; Volume 37, Issues 2–7, as listed below.

Mechanical Properties and Performance of Engineering Ceramics and Composites XI, CESP Volume 37, Issue 2 (includes papers from Symposium 1)
Advances in Solid Oxide Fuel Cells and Electronic Ceramics II, CESP Volume 37, Issue 3 (includes papers from Symposia 3 and 14)
Advances in Ceramic Armor, Bioceramics, and Porous Materials, CESP Volume 37, Issue 4 (includes papers from Symposia 4, 5, and 9)
Advanced Processing and Manufacturing Technologies for Nanostructured and Multifunctional Materials III, CESP Volume 37, Issue 5 (includes papers from Symposia 8 and 11 and Focused Sessions 4 and 5)
Ceramic Materials for Energy Applications VI, CESP Volume 37, Issue 6 (includes papers from Symposia 6 and 13 and Focused Session 2)
Developments in Strategic Materials II, CESP Volume 37, Issue 7 (includes papers from Symposia 2, 10, 12, Focused Sessions 1, and the Special Symposia on Carbon).

The organization of the Daytona Beach meeting and the publication of these proceedings were possible thanks to the professional staff of ACerS and the tireless dedication of many ECD members. We would especially like to express our sincere thanks to the symposia organizers, session chairs, presenters and conference attendees, for their efforts and enthusiastic participation in the vibrant and cutting-edge conference.

ACerS and the ECD invite you to attend the 41st International Conference on Advanced Ceramics and Composites (http://www.ceramics.org/icacc2017) January 23-28, 2017 in Daytona Beach, Florida.

To purchase additional CESP issues as well as other ceramic publications, visit the ACerS-Wiley Publications home page at www.wiley.com/go/ceramics.

MANABU FUKUSHIMA, National Institute of Advanced Industrial Science and Technology (AIST), Japan
ANDREW GYEKENYESI, Ohio Aerospace Institute/NASA Glenn Research Center, USA

Volume Editors
August 2016

Developments in Strategic
Ceramic Materials II

A Collection of Papers Presented at the
40th International Conference on
Advanced Ceramics and Composites
January 24–29, 2016
Daytona Beach, Florida

Preface

Introduction

Geopolymers

A Collection of Papers Presented at the40th International Conference onAdvanced Ceramics and Composites January 24–29, 2016 Daytona Beach, Florida

A Collection of Papers Presented at the
40th International Conference on
Advanced Ceramics and Composites
January 24–29, 2016
Daytona Beach, Florida