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IISBN: 978-1-119-32170-5

ISSN: 0196-6219

CONTENTS

Preface

Introduction

Field Assisted Sintering

FLASH SINTERING OF ALUMINA AND ITS MICROSTRUCTURAL EVOLUTION
1. ABSTRACT
2. INTRODUCTION
3. EXPERIMENTAL PROCEDURE
4. RESULTS AND DISCUSSION
5. CONCLUSIONS
6. REFERENCES
ENHANCEMENTS ON FAST SINTERING SYSTEMS PROMOTE TRANSFER FROM THE LAB TO INDUSTRIAL APPLICATIONS
1. ABSTRACT
2. INTRODUCTION
3. FLEXIBLE “FAST” UNITS FOR THE LABORATORY
4. EFFICIENT “FAST” UNITS FOR INDUSTRIAL APPLICATION
5. CONCLUSIONS
6. ACKNOWLEDGEMENTS
7. REFERENCES
COMBINING FLASH SINTERING / SINTERFORGING WITH HYBRID FAST/SPS TECHNOLOGY FOR OXIDE AND NON-OXIDE MATERIALS
1. ABSTRACT
2. INTRODUCTION
3. EXPERIMENTAL
4. RESULTS AND DISCUSSION
5. CONCLUSIONS
6. REFERENCES
LOW TEMPERATURE FABRICATION OF TRANSPARENT MAGNESIUM ALUIMINATE SPINEL BY HIGH PRESSURE SPARK PLASMA SINTERING
1. ABSTRACT
2. INTRODUCTION
3. EXPERIMENTAL PROCEDURES
4. RESULTS AND DISCUSSION
5. CONCLUSIONS
6. REFERENCES

Advanced Processing and Manufacturing

DEFECT CONTROL OF SIC POLYCRYSTALLINE FIBER AIMING FOR HIGHER STRENGTH
1. ABSTRACT
2. 1. INTRODUCTION
3. 2. EXPERIMENTAL PROCEDURE
4. 3. RESULTS AND DISCUSSION
5. 4. CONCLUSIONS
6. ACKNOWLEDGMENTS
7. REFERENCES
TEM ANALYSIS OF INTERFACES IN DIFFUSION-BONDED SILICON CARBIDE CERAMICS JOINED USING METALLIC INTERLAYERS
1. ABSTRACT
2. INTRODUCTION
3. EXPRIMENTAL
4. RESULTS AND DISCUSSION
5. CONCLUSION
6. REFERENCES
MICRO-COMPUTED TOMOGRAPHY CHARACTERIZATION OF ISOTROPIC FILLER DISTRIBUTION IN MAGNETORHEOLOGICAL ELASTOMERIC COMPOSITES
1. ABSTRACT
2. INTRODUCTION
3. EXPERIMENTAL
4. CONCLUSIONS
5. ACKNOWLEDGEMENTS
6. REFERENCES

Additive Manufacturing

DEVELOPMENT OF ADVANCED CERAMIC FUEL CELLS USING ADDITIVE MANUFACTURING TECHNOLOGY (I): DESIGN AND MODELING
1. ABSTRACT
2. INTRODUCTION
3. METHODS OF FABRICATION OF SPIRAL FUEL CELL
4. FABRICATION OF SPIRAL CELL BY ADDITIVE MANUFACTURING
5. CONCLUSIONS
6. ACKNOWLEDGMENTS
7. REFERENCES
RAPID MANUFACTURING OF CERAMIC PARTS
1. ABSTRACT
2. 1. INTRODUCTION
3. 2. METHODOLOGY
4. 4. CONCLUSIONS
5. REFERENCES

Advanced Materials and Innovative Processing Ideas for the Industrial Root Technology

NANO TECHNOLOGY IN DEVELOPMENT OF FUNCTIONAL COATINGS
1. ABSTRACT
2. 1. INTRODUCTION
3. EXAMPLES OF SOME FUNCTIONAL COATINGS FORMULATED
4. 1.2 Anti-fouling, self-polishing smooth coatings
5. CONCLUSION
6. REFERENCES
TAILORING THE FUNCTIONAL PROPERTIES OF NIOBIUM CARBIDE
1. ABSTRACT
2. INTRODUCTION
3. METHODS OF NIOBIUM CARBIDE SYNTHESIS
4. BASIC PROPERTIES OF NIOBIUM CARBIDE
5. METAL BINDERS AND SECONDARY CARBIDE ADDITION
6. TRIBOLOGICAL BEHAVIOR OF NBC-BASED HARD MATERIALS
7. Cutting
8. SUSTAINABILITY CONSIDERATIONS
9. CONCLUSIONS
10. REFERENCES

Author Index

EULA

List of Illustrations

Chapter 1

Figure 1: Dilatometric plot of field assisted sintered alumina with different voltage and current limit of 2 mA/mm². The shrinkage values are referred to the gage section.
Figure 2: (a) Linear shrinkage upon sintering as a function of the current density and (b) ratio between the shrinkage associated to FS and the total one.
Figure 3: SEM micrograph of the FS samples fracture surface showing the microstructural evolution at different current density: 2mA/mm² (a), 4mA/mm² (b) and 6mA/mm² (c). The micrographs are referred to specimens treated with 1500 V/cm.
Figure 4: Grain size evolution as a function of the nominal current density. The dashed line represents the fitting curve according to Eq. (4). For each current limit is also reported the relative bulk density (p).

Chapter 2

Figure 1. Multi purpose 25 ton lab unit (left) and high power Hybrid/FAST 320 ton industrial unit (right), both available at FCT technical center
Figure 2. Different types of multi-cavity molds (left) and serial-parallel 2x23 mold (right)
Figure 3. Combination of FAST/SPS in-situ heating (left) and an external heater (middle) allows compensation of thermal gradients (right).
Figure 4. Case study: consolidation benchmark of a 300 mm tungsten carbide disk using the FAST/SPS operation mode
Figure 5. Case study: consolidation benchmark of a 300 mm tungsten carbide disk using the Hybrid/FAST operation mode
Figure 6. Comparison of the densification curves of the 300 mm tungsten carbide case study
Figure 7. 200 mm diameter disc made of a Ti-based MMC (top left) with similar microstructure at center and rim (bottom left)¹¹; complex part made by FAST with homogeneous microstructure (right)¹². - left pictures by courtesy of M.A.Lagos¹¹, right picture by courtesy of A.Couret¹²
Figure 8. Hybrid heating and cooling of a 300 mm diameter disc made of pure tungsten carbide.
Figure 9. Schematic of a high throughput FAST production unit with separate preheating and cooling channel.
Figure 10. Example of a high throughput FAST production unit with separate preheating and cooling channel.

Chapter 3

Figure 1. Multi-purpose 2½ ton lab unit
Figure 2. Top: Temperature and densification of reference experiment (grey) compared to “Flash/FAST 1” (black); Bottom: Electrical data of “Flash/FAST 1”
Figure 3. Comparison of the densification curves vs temperature
Figure 4. Resistivity and density of 3YSZ vs. temperature at 50V/cm.
Figure 5. Densification and current vs. temperature with automatic mode switching

Chapter 4

Fig. 1. Microstructure of the specimens fabricated under 400 MPa at 1200°C (a) and 1100°C (b).
Fig. 2. Microstructure of the specimens sintered under 500 MPa at 1050°C (a) and 650 MPa at 1025°C (b).
Fig. 3. In-line transmittance of HPSPS-processed PMAS ceramics.
Fig. 4. SEM images of Vickers imprint under different loads for specimens sintered under 400 MPa at 1100°C. Note: The images were taken at different magnifications.
Fig. 5. Vickers hardness of PMAS as a function of the grain size.

Chapter 5

Fig. 1 The basic production process of Tyranno SA
Fig. 2 Estimated defects contained in the SiC-polycrystalline fiber
Fig. 3 Classifications of the material’s properties
Fig. 4 The relationship between the fracture size and the tensile strength of the filament
Fig. 5 Changes in the Gibbs free energy of SiO₂-SiO-CO reaction system
Fig. 6 The relationship between SiO vapor pressure and temperatures
Fig. 7 Preliminary improvement result (Surface roughness was remarkably improved.)

Chapter 6

Figure 1: SIM image of the diffusion bonded area after FIB cutting. Phase information and sample locations are shown in (b).
Figure 2: HAADF STEM images of a diffusion bond. A, B, and C correspond to sections in Figure 1(b)
Figure 3: STEM images from SA-THX area acquired with (a) SEM (b) BF-STEM (c) HAADF.
Figure 4: TEM images of a Mo-Ti(SS) grain.
(a) Bright-field image (b) Dark-field image.
Inset in (a) is a SAD pattern obtained from the same area.
Figure 5: Schematic of pillar-shaped TiC deposits in Mo-Ti(SS) matrix
Figure 6: SAD pattern from a region containi ng Mo-Ti(SS) and TiC.Reciprocal lattices of [100]_Mo-Ti and [011]_TiC are indicated with solid and broken lines, respectively.

Chapter 7

Fig. 1 (a). Basic viscoelastic properties of an elastomeric matrix. (b) Various application areas of MRE composites.
Fig. 2 (a1) Elastomer matrices N 1522, (a2) chemical composition of N1522, (b1) SEM image of ZA 22 with respective (b2) chemical composition . (c1) SEM micrograph of iron particles with the corresponding ( c2) particle size distribution
Fig. 3. Fabrication of MRE sample preparation.
Fig. 4. Isotropic and anisotropic particle arrangemnt within MRE composites.
Fig. 5 (a)Photographic image of cylindrical samples, and (b) SEM micrographs of the N1522 MRE composites with the influence of magnetic field (b1) without presence of magnetic field, ( c) SEM micrograph of ZA 22 with presence of magnetic field (c1) without presence of magnetic field .
Fig. 6. Micro-CT images of two dimensional views of the elastomer and composite.
Fig. 7. Three dimensional representations of the elastomer and MRE composites.
Fig. 8. SEM micrographs of the MRE samples and the corresponding self-assembly binary particles.
Fig. 9 (a) Particle volume fraction as a function of MRE composite height. (b) Filler particle distribution with respect to particle size as a function of composite height.
Fig. 10. Magnetic pole interaction mechanism during the analsysis.
Fig. 11. Schematic representation of particle distribution as a function of height in MRE composites.

Chapter 8

Figure 1. The spiral cell (recreated from the spiral cell concept in reference 1).
Figure 2. The spiral manifold.
Figure 3. YSZ 3-phase diagram.
Figure 4. Printed sample of the spiral cell with different geometry parameters.
Figure 5. (a) The developed 3D CAD design, (b) Pure zirconia 3D real object manufactured by SLS/M (c) Maximized top view and (d) Accurate geometry performed by LSL/M.
Figure 6. (a) Zirconia cube for porosity/density check, (b) SEM image of top view of the zirconia cube with 56% density¹² and (c) SEM image of zirconia cube with 56% density¹².
Figure 7. (a) Metal and ceramic building layers, (b) Metal and ceramic powder composite, (c) Micrograph of built steel/Cr₃C₂, and (d) Powder composite built steel/WC.
Figure 8. SEM images of hydroxyapatite scaffolds produced by: the first row powder-based 3D printing; second row are by direct ink writing¹⁸.
Figure 9. Compressive strength versus porosity for bio-ceramic porous components fabricated using different AM technologies¹⁷.
Figure 10. interconnection development step.
Figure 11. (a) Stack of two spiral cells with an interconnection, and (b) Interconnection with heat exchanger internal section

Chapter 9

Figure 1. The liquid deposit modeling schematic diagram 1, workbench 2, slice of the layer 3, greenware 4, nozzle 5, slurry silo
Figure 2. Ceramic parts made by the liquid deposit modeling
Figure 3. Defects of ceramic 3DP
Figure 4 The sketch map of the drying and sintering linear shrinkage

Chapter 10

Fig. 1 Water contact angle and sliding angle on the surface of PFTE modified coating with increasing concentrations of silica
Figure 2: Performance of the self-cleaning activity on solar panel confirming no loss of voltage when measured with and without application of self-cleaning coating for 30 days.
Figure 3: Panels after 30 days of immersion test
Figure 4: show panels after 60 days of immersion test
Figure 5: Yellowing and color change index of epoxy with unmodified and modified nano ZnO concentration upon UV exposure
Figure 6: yellowing and color change index of epoxy with flake like and spherical nano ZnO concentration upon UV exposure
Figure 7: Samples exposed to UV radiation for 24 hours a) coating modified with 2% nano ZnO b) modified with 1 % nano ZnO and c) Unmodified coating
Figure 8: a) Yellowing Index and b) Gloss index of epoxy coatings with variable ZnO content and variable exposure time to UVB radiation
Figure 9: Graphene characterization (a) TEM image of a graphene flake (b) HR-TEM image of graphene and the corresponding FFT image (inset). (c) Electron diffraction pattern of the produced graphene showing clearly a six membered ring. (d) Raman spectra of the graphene sample.
Figure 10: EIS Bode plot of functionalized graphene as compared to Cr (VI) pre-treatment primer as well as graphite based pre-treatment primer
Figure 11: Salt spray (fog) test results

Chapter 11

Figure 1. Agglomerated NbC_0.88 crystallites after reduction of CBMM’s high purity Nb₂O₅ powder (used for “H1”)
Figure 2. Morphology of NbC_1.0 crystallites obtained by carbo-thermal reduction of CBMM’s high purity Nb₂O₅ powder (deagglomerated)
Figure 3. NbC_0.94 particles formed by primary precipitation in a carbon-alloyed iron melt.
Figure 4. Coarse NbC_0.95 particles precipitated in liquid iron after chemical leaching.
Figure 5. Binary Nb-C phase diagram indicating the existence of various sub-carbide phases [8]
Figure 6. Micro-hardness of niobium carbide phases as function of C/Nb ratio [14].
Figure 7. Hot hardness of NbC and WC hardmetal grades [20]
Figure 8. Elastic modulus versus temperature of NbC hardmetal grades
Figure 9. Impact of binder type on Vickers hardness and fracture toughness of NbC-based hardmetals prepared by KU Leuven.
Figure 10. Impact of secondary carbides on Vickers hardness and fracture toughness of cobalt (left) and nickel (right) bonded NbC hardmetals.
Figure 11. Impact of one or two secondary carbides to nickel bonded NbC grades on their Vickers hardness and fracture toughness.
Figure 12. Total wear coefficients of cobalt or Fe₃Al bonded NbCs and Fe₃Al-NbC (MMC) compared to different ceramics and hard metals under dry friction
Figure 13. Comparison of flank wear (left) and the crater wear (right) between the WC-6Co insert and the NbC-12Fe₃Al insert for the semi-finishing tests (100Cr6 205 HB, Vc =100 m/min, hex.= 0,2 mm, DoC = 1,5 mm, 10 bars emulsion, lead angle at 75°, nose radius 0,8 mm) [32]
Figure 14. Comparison of crater wear in hard turning of NbC-8Co SPS (left) and WC-6Co (right) (100Cr6 (205 HB), machining time= 5 min. 33 s., Vc= 100 m/min, f = 0,415 mm/rev, hex= 0,4, DoC = 3 mm, Kr (lead angle) = 75°, nose radius= 1,5 mm, emulsion 10 bars) [32]
Figure 15. Comparison of insert behavior during coolant-free interrupted milling of SABS 1431:300WA-SS (184 HV or 55.1 HRA) at v_c = 250 m/min (a_p= 0.5/1 mm) [33]

Preface

This CESP issue contains papers that were presented during three symposia held during the 40th International Conference and Exposition on Advanced Ceramics and Composites, Daytona Beach, Florida, January 24–29, 2016:

Symposium 8: 9th International Symposium on Advanced Processing and Manufacturing Technologies for Structural and Multifunctional Materials and Systems (APMT)
Symposium 11: Advanced Materials and Innovative Processing Ideas for the Industrial Root Technology
Focused Session 4: Additive Manufacturing and 3D Printing Technologies
Focused Session 5: Field Assisted Sintering and Related Phenomena at High Temperatures

Over 100 contributions (invited talks, oral presentations, and posters) were presented by participants from universities, research institutions, and industry, which offered interdisciplinary discussions indicating strong scientific and technological interest in the field of nanostructured systems. This issue contains 11 peer-reviewed papers that cover various aspects and the latest developments related to nano-scaled materials and functional ceramics.

The editors wish to extend their gratitude and appreciation to all the authors for their cooperation and contributions, to all the participants and session chairs for their time and efforts, and to all the reviewers for their valuable comments and suggestions. Financial support from the Engineering Ceramics Division of The American Ceramic Society (ACerS) and industry sponsors is gratefully acknowledged. The invaluable assistance of the ACerS staff of the meetings and publication departments, instrumental in the success of the symposium, is gratefully acknowledged,

We believe that this issue will serve as a useful reference for the researchers and technologists interested in science and technology of multifunctional or nanostructured materials and devices.

Tatsuki Ohji, Nagoya, Japan

Mrityunjay Singh, Cleveland, USA

Michael Halbig, Cleveland, USA

Kyoung Il Moon, Gyonggi-do, Korea

Advanced Processing and
Manufacturing Technologies
for Nanostructured and
Multifunctional Materials III

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

Preface

Advanced Processing andManufacturing Technologiesfor Nanostructured andMultifunctional Materials III

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

Advanced Processing and
Manufacturing Technologies
for Nanostructured and
Multifunctional Materials III

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