Field Assisted Sintering of Advanced Ceramic Materials, Nikhil Mohip, Seth Mongbeh, Alejandro ...

126 Pages·2015·5.09 MB·English

by  Sabri Tosunoglu

[1]

EML 4905 Senior Design Project

A B.S. THESIS
PREPARED IN PARTIAL FULFILLMENT OF THE
REQUIREMENT FOR THE DEGREE OF
BACHELOR OF SCIENCE
IN
MECHANICAL ENGINEERING

FIELD ASSISTED SINTERING OF
ADVANCED CERAMIC MATERIALS
Final Report

Nikhil Mohip
Seth Mongbeh
Alejandro Vera

Advisor: Professor Zhe Cheng

November 22nd, 2015

This B.S. thesis is written in partial fulfillment of the requirements in EML 4905.
The contents represent the opinion of the authors and not the Department of
Mechanical and Materials Engineering.
Ethics Statement and Signatures

The work submitted in this B.S. thesis is solely prepared by a team consisting of Nikhil Mohip,
Seth Mongbeh, and Alejandro Vera and it is original. Excerpts from others’ work have been
clearly identified, their work acknowledged within the text and listed in the list of references. All
of the engineering drawings, computer programs, formulations, design work, prototype
development and testing reported in this document are also original and prepared by the same
team of students.

Alejandro Vera Nikhil Mohip Seth Mongbeh
Team Leader Team Member Team Member

Dr. Zhe Cheng
Faculty Advisor

ii
TABLE OF CONTENTS
Chapter Page

Cover Page i
Ethics Statement and Signatures ii
Table of Contents iii
List of Figures vii
List of Tables x

Abstract ........................................................................................................................................... 1
1. Introduction ................................................................................................................................. 2
1.1 Problem Statement ................................................................................................................ 2
1.2 Motivation ............................................................................................................................. 2
1.3 Literature Survey ................................................................................................................... 3
1.3.1 Sintering.......................................................................................................................... 3
1.3.2 Sintering Driving Force .................................................................................................. 3
1.3.3 Sintering Mechanism ...................................................................................................... 4
1.3.4 Pressure Assisted Sintering ............................................................................................ 5
1.3.5 Hot Pressing .................................................................................................................... 5
1.3.6 Microwave Sintering ...................................................................................................... 5
1.3.7 Field Assisted Sintering .................................................................................................. 7
1.3.8 Joule Heating .................................................................................................................. 8
1.3.9 Effect of Electric Field ................................................................................................. 10
1.3.10 Effect of Particle Size ................................................................................................. 11
1.4 Related Standards ................................................................................................................ 12
1.5 Discussion ........................................................................................................................... 14
2. Project Formulation .................................................................................................................. 15
2.1 Overview ............................................................................................................................. 15
2.2 Project Objectives ............................................................................................................... 15
2.3 Design Specifications .......................................................................................................... 15
2.4 Addressing Global Design .................................................................................................. 15
2.5 Constraints and Other Considerations ................................................................................. 16
2.6 Discussion ........................................................................................................................... 17
3. Design Alternatives ................................................................................................................... 18
3.1 Overview of Conceptual Designs Developed ..................................................................... 18
iii
3.2 Design Alternate 1 ............................................................................................................... 18
3.3 Design Alternate 2 ............................................................................................................... 19
3.4 Design Alternate 3 ............................................................................................................... 20
3.5 Design Alternate 4 ............................................................................................................... 21
3.6 Integration of Global Design Elements ............................................................................... 22
3.7 Proposed Design .................................................................................................................. 25
4. Project Management ................................................................................................................. 26
4.1 Overview ............................................................................................................................. 26
4.2 Breakdown of Work into Specific Tasks ............................................................................ 27
4.3 Gantt Chart for the Organization of Work and Timeline .................................................... 27
4.4 Breakdown of Responsibilities Among Team Members .................................................... 28
4.5 Discussion ........................................................................................................................... 29
5. Engineering Design and Analysis ............................................................................................. 30
5.1 Overview ............................................................................................................................. 30
5.2 Material Selection ............................................................................................................... 30
5.2.1 Yttria Stabilized Zirconium .......................................................................................... 31
5.2.2 Silicon Carbide ............................................................................................................. 32
5.3 Ceramic Powder Die Design ............................................................................................... 33
5.4 Prediction of Sample Flash Sintering Temperatures ........................................................... 34
6. Prototype Construction ............................................................................................................. 40
6.1 Overview ............................................................................................................................. 40
6.2 Experimental Set Up ........................................................................................................... 40
6.4 Parts List .............................................................................................................................. 44
6.5 Construction ........................................................................................................................ 45
6.6 Prototype Cost Analysis ...................................................................................................... 48
6.7 Discussion ........................................................................................................................... 49
7. Testing and Evaluation ............................................................................................................. 50
7.1 Overview ............................................................................................................................. 50
7.2 Experimental Procedure ...................................................................................................... 50
7.2.1 Sample Pressing ............................................................................................................ 50
7.2.2 Apparatus Setup ............................................................................................................ 51
7.2.3 Constant heating ........................................................................................................... 54
iv
7.3 Test Results and Data .......................................................................................................... 55
7.3.1 Pure YSZ8 .................................................................................................................... 58
7.3.2 YSZ8 mixed with Platinum Powder ............................................................................. 62
7.3.3 YSZ8 mixed with PVA ................................................................................................. 63
7.4 Evaluation of Experimental Results .................................................................................... 69
7.5 Improvement of the Design ................................................................................................. 71
7.6 Discussion ........................................................................................................................... 76
8. Design Considerations .............................................................................................................. 77
8.1 Environment, Health and Safety (EHS) Overview ............................................................. 77
8.2 Ceramic Powder EHS Considerations ................................................................................ 77
8.2.1 Yttria Stabilized Zirconia (YSZ8-TC) Safety Data Sheet Relevant Information ......... 78
8.2.2 Silicon Carbide (SiC) Safety Data Sheet Information .................................................. 79
9. Design Experience .................................................................................................................... 81
9.1 Overview ............................................................................................................................. 81
9.2 Standards Used in the Project ............................................................................................. 81
9.3 Impact of Design in Global and Societal Context ............................................................... 81
9.4 Professional and Ethical Responsibility .............................................................................. 82
9.5 Life Long Learning Experience .......................................................................................... 82
9.6 Discussion ........................................................................................................................... 82
10. Conclusion .............................................................................................................................. 83
10.1 Conclusion and Discussion ............................................................................................... 83
10.2 Evaluation of Integrated Global Designs Aspects ............................................................. 83
10.3 Commercialization Prospects of the Product .................................................................... 83
Works Cited .................................................................................................................................. 85
Appendices .................................................................................................................................... 87
Appendix A: Engineering Drawings ......................................................................................... 87
Appendix B: Multilingual User’s Manuals ............................................................................... 89
Experiment Set up for YSZ8 mixed with PVA ..................................................................... 89
Configuración del Experimento para YSZ8 mezclada con PVA .......................................... 90
Experiment zum YSZ8 Set gemischt mit PVA1. Man wiegt 1 Gramm YSC8 Keramikpulver
............................................................................................................................................... 91
Appendix C: Commercial Catalogs and Documents................................................................. 93
Appendix D: Detailed Raw Design Calculations and Analysis .............................................. 106
v
Appendix E: Photo Album ...................................................................................................... 107
Materials .............................................................................................................................. 107
Lab Equipment .................................................................................................................... 109
Safety Equipment ................................................................................................................ 111

vi
LIST OF FIGURES
Figure Page

Figure 1: Schematic drawing of apparatus for continuous microwave sintering [1] ...................... 6
Figure 2: Power per Unit Volume versus Time for limiting current of 15A (1) ............................ 9
Figure 3: Effect of Current Density During Isothermal Flash Sintering at 100 Vcm -1 (3). ........ 10
Figure 4: Shrinkage versus Strain plot for four different particle size specimens (12). ............... 11
Figure 5: Conventional Die ........................................................................................................... 18
Figure 6: Die Alternative 1 – Circular Dog Bone Die .................................................................. 19
Figure 7: Die Alternative 3 – Rectangular Dog Bone Die ............................................................ 20
Figure 8: Die Alternative 4 - Three Piece Die .............................................................................. 21
Figure 9: Oxygen Sensor developed by Robert Bosch Gmbh during the late 1960's ................... 23
Figure 10: Zirconia based Oxygen Sensor .................................................................................... 23
Figure 11: Diagram showing the power supply connected to the sample by means of platinum
wires....................................................................................................................................... 25
Figure 12: Distribution of Team Member Tasks .......................................................................... 27
Figure 13: Dog Bone Shape Die ................................................................................................... 33
Figure 14: Machined Dog Bone Shape Die .................................................................................. 33
Figure 15: Theoretical Linear Graph for YSZ8-TC Temperature vs Power Dissipation ............. 35
Figure 16: Theoretical Graph of YSZ8-TC Temperature vs time at 500 Watts ........................... 36
Figure 17: Theoretical Graph of YSZ8-TC Temperature vs. time at 700 Watts .......................... 36
Figure 18: Theoretical Graph of YSZ8-TC Temperature vs time at 1,000 Watts ........................ 37
Figure 19: Theoretical Graph of YSZ8-TC Temperature vs time at 1, 250 Watts ....................... 37
Figure 20: Theoretical Graph of YSZ8-TC Temperature vs time at 1,500 Watts ........................ 38
Figure 21: Theoretical Linear Graph for SiC vs Power Dissipation ............................................. 39
Figure 22: Apparatus including a circular pellet ........................................................................... 41
Figure 23: Magnified View of the Pellet within the Furnace ....................................................... 42
Figure 24: Manual Press ............................................................................................................... 43
Figure 25: Sorenson X100 1500 Watt Power Supply ................................................................... 45
Figure 26: Power Supply's Power Cable Setup ............................................................................ 46
Figure 27: ATS Furnace Program Panel ....................................................................................... 47
Figure 28: Low Tolerances of Manufactured Dog Bone Die ....................................................... 49
Figure 29: Power Supply AC Wiring Placement [15] .................................................................. 51
Figure 30: Power Supply Rear Panel Diagram [15] ..................................................................... 52
Figure 31: Dog Bone Shape Die Pressing..................................................................................... 56
Figure 32: Visible gaps in the center of the die due to high tolerances ........................................ 57
Figure 33: Set up used for pure YSZ8 and YSZ8 mixed with platinum powder .......................... 57
Figure 34: Initial Die Design ........................................................................................................ 59
Figure 35: Assembled Die design 1 .............................................................................................. 59
Figure 36: Weighing of YSZ8 before sample pressing ................................................................ 60
vii
Figure 37: Experimental set with furnace heating the sample at a constant temperature ............. 60
Figure 38: Pure YSZ8 After Attempted Flash Sintering shows No Positive Signs of Densification
............................................................................................................................................... 61
Figure 39: Constant heating of YSZ8 mixed with Platinum Powder ........................................... 62
Figure 40: Platinum Wires Set up ................................................................................................. 64
Figure 41: Experimental Set up for YSZ8 mixed with PVA ........................................................ 65
Figure 42: Platinum Wires Set Up with Attached Sample ........................................................... 66
Figure 43: Melted Platinum Wire shows temperature reached well above 1700°C ..................... 67
Figure 44: YSZ8 sample after test. From Top to Bottom: Top left: Side one, Top right: Side 2,
Bottom left: Side 1 Close up, Bottom right: Sample ready for further hardness tests .......... 68
Figure 45: Platinum Wires Making Connection with the Circular Sample .................................. 70
Figure 46: Using Infrared Light to Solidify the Ceramic Bond .................................................... 72
Figure 47: Proposed set up for Platinum Wires and Thermocouple using Ceramic Bond to attach
them to the Aluminum Oxide Plate ....................................................................................... 73
Figure 48: SolidWorks model for the proposed sample holding set up. Black wire: Positive
Platinum wire, Blue: Thermocouple, Red: Negative Platinum wire ..................................... 73
Figure 49: Improved Dog Bone Die Design including High Precision Tolerances ..................... 74
Figure 50: Future Improvements of Experimental Setup ............................................................. 75
Figure 51: Magnified View of Future Improvements. Dog Bone Shaped Sample Connected to the
Sample Holder: Red and Black wires represent the platinum wires, Blue wire represents the
thermocouple ......................................................................................................................... 75
Figure 52: Ceramic Powder Die – Bottom/Top Piece .................................................................. 87
Figure 53: Ceramic Powder Die - Sleeve ..................................................................................... 88
Figure 54: Sika Product Information ............................................................................................ 93
Figure 55: Safety Data Sheet - YSZ8-TC pg.1 ............................................................................. 94
Figure 56: Safety Data Sheet - YSZ8-TC pg.2 ............................................................................. 95
Figure 57: Safety Data Sheet - YSZ8-TC pg.3 ............................................................................. 96
Figure 58: Safety Data Sheet - YSZ8-TC pg.4 ............................................................................. 97
Figure 59: Safety Data Sheet - YSZ8-TC pg.5 ............................................................................. 98
Figure 60: Safety Data Sheet - YSZ8-TC pg.6 ............................................................................. 99
Figure 61: Safety Data Sheet - YSZ8-TC pg.7 ........................................................................... 100
Figure 62: Safety Data Sheet - SiC pg. 1 .................................................................................... 101
Figure 63: Safety Data Sheet - SiC pg. 2 .................................................................................... 102
Figure 64: Safety Data Sheet - SiC pg. 3 .................................................................................... 103
Figure 65: Safety Data Sheet - SiC pg. 4 .................................................................................... 104
Figure 66: Safety Data Sheet - SiC pg. 5 .................................................................................... 105
Figure 67: Raw Data Calculations .............................................................................................. 106
Figure 68: YSZ8-TC Powder ...................................................................................................... 107
Figure 69: SiC Powder ................................................................................................................ 108
Figure 70: Nano-Fabrication Lab Furnace .................................................................................. 109
viii
Figure 71: Furnace Interior ......................................................................................................... 110
Figure 72: Face Mask.................................................................................................................. 111
Figure 73: Thermal Gloves ......................................................................................................... 112
Figure 74: Nitrile Gloves ............................................................................................................ 113
Figure 75: Safety Glasses............................................................................................................ 114
Figure 76: Lab Coats ................................................................................................................... 115
Figure 77: Conduction of Flash Sintering Experiment ............................................................... 116

ix
LIST OF TABLES

Table Page

Table 1: Mechanism of Sintering in Polycrystalline Solids............................................................ 4
Table 2: Gantt Chart...................................................................................................................... 27
Table 3: Properties of YSZ8 ......................................................................................................... 31
Table 4 - YSZ8-TC Flash Sintering Parameter Predictions.......................................................... 35
Table 5: SiC Temperature vs. Power Dissipation Predictions ...................................................... 39
Table 6: Prototype Construction Cost Analysis ............................................................................ 48

x