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By: Jacob Scott Advisor: Dr. Rick By: Jacob Scott Advisor: Dr. Rick

By: Jacob Scott Advisor: Dr. Rick - PowerPoint Presentation

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By: Jacob Scott Advisor: Dr. Rick - PPT Presentation

Reidy Design of MultiLayer Ceramic Ballistic Plates Final Report Spring 2015 Classification Projectile Caliber Projectile Weight Velocity Type IIA 357 Magnum jacketed soft point 9mm ID: 800841

run tape ysz casting tape run casting ysz doctor impact plates density results blade amount sintering testing design small

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Slide1

By: Jacob ScottAdvisor: Dr. Rick Reidy

Design of Multi-Layer Ceramic Ballistic Plates: Final Report

Spring 2015

Slide2

Classification

Projectile Caliber

Projectile WeightVelocityType II-A.357 Magnum jacketed soft point9mm full-metal jacketed10.2 g (158 gr)8.0 g (124 gr)1,250 ft/s1,090 ft/sType II.357 Magnum jacketed soft point9mm full-metal jacketed10.2 g (158 gr)8.0 g (124 gr)1,395 ft/s1,175 ft/sType III-A.44 Magnum lead semi-wadcutter9mm full-metal jacketed15.55 g (240 gr)8.0 g (124 gr)1,400 ft/s1,400 ft/sType III*7.62 mm full-metal jacketed9.7 g (150 gr)2,750 ft/sType IV*.30-06 armor-piercing 10.8 g (166 gr)2,850 ft/s

Standards- National Institute of Justice3

*Type III and IV both contain hard or semi-rigid plates, while the rest are “soft/concealable”

3

NIJ Guide 100-98. US Department of Justice.

Selection and Application Guide to Police Body Armor

Slide3

Standards- NIJ Testing

Slide4

(Enhanced) Small Arms Protective Inserts (SAPI + ESAPI)First put through a selection of hot, cold, saltwater, oil, fuel, and then dropped

SAPI must stop 3 shots “against threats A,B,C”

ESAPI must stop 3 shots “against threats A,B,C” and 2 shots “against threat D”Threats A, B, C, D are classifiedStandards- Department of Defense44Report No. D-2009-047. Inspector General US:DOD. DoD Testing Requirements for Body Armor

Slide5

US Patent- US7556855 B2Uses layered tape cast yttria stabilized zirconia (YSZ)/alumina in a strain rate sensitive polymer

Recommends minimizing grain growth of YSZ to promote crack deflection

Only specifies overall weight percents, does not go into detail on types of YSZ, or casting proceduresLiterature ReviewItem 101- Strain rate sensitive polymerItem 110- Ceramics to break projectileItems 12X- Interconnected ceramics to further break and/or catch fragmentsItem 140- Ballistic fiber to catch fragments

Slide6

US Patent- US7803732 B1Mixing zirconia with silicon carbide increases controlled defects

Leads to increased surface area that is fractured during a ballistic event

Leading to the spreading and dispersion of the impact i.e. can disperse a larger projectileLiterature Review (Continued)

Slide7

Literature Review (Continued)

3

mol% YSZ8 mol% YSZStructureTetragonalCubicSpace Group#137- P42/nmc#225- Fm3mDefect Equations: (Anti-Frenkel)ZrO2 = ZrZrX+2VO**+2Oi’’ Y2O3= 2YZr’+VO**+3OOX

Slide8

Research has shown that 3 mol% YSZ has a 2-3 times higher flexural strength versus 8 mol% YSZ. 1

8mol% is generally used for solid oxide fuel cells

The recipe featured in Fabrication of electrolyte materials for solid oxide fuel cells by tape-casting, was investigated and found that the materials used are no longer available. Literature Review (Continued)1Fabrication of electrolyte materials for solid oxide fuel cells by tape-casting. P. Timakul et al.

Slide9

Tape casting of 3mol% YSZ with the recipe from C.

Suciu

et al2 created thin tapes with minimal cracking, clean burn out. Literature Review (Continued)2Water-based tape-casting of SOFC…. Of their pellets. C. Suciu et al. PartWeight PercentPowder (TZ-3Y-E)48.1Binder (WB4101)21Defoamer (DF002)0.3Solvent (DI Water)30.1PH balancer (Ammonium Hydroxide)0.2

Slide10

Design a plate that will stop a single 200 joule impact force (equivalent to typical .22LR caliber bullet impact)

Design Goal

Slide11

The main constraints for this project are the thickness and the weight of the plates.

Constraints

Slide12

Tape cast crack-free YSZ tapesLayer tapes to increase thicknessSinter tapes to achieve full tetragonal phase

Achieve 95% theoretical density (6.0 g/cm^3)

Achieve Vickers hardness value 1250 HVObjectives

Slide13

Create and mill slurry of YSZ, binder, defoamer, water

Tape cast slurry forming tape

Section tape, and layer increasing thicknessSinter layered tapes into plates to join layersCharacterize though SEM, XRD, impact testing, hardness testing, density measurements, etcIncrease number of layers until design goal metDesign of Experiment

Slide14

Gantt Chart

Slide15

Pert Chart

Slide16

Tape Casting Diagram

Slide17

Run 1- “Trial Run”

Slide18

Run 1 Results

Appears to have pink tint- Believed to be caused by incorrect amount of ammonia hydroxide added due to calculation error

Significant crackingCracking believed to be caused by too high of bed heat and too large of doctor blade heightLarge amount of batch wasted from spillage

Slide19

Run 2

Slide20

Run 2 Results

Changes

Lowered bed temperatureLowered doctor blade heightAdded correct amount of ammonia hydroxideAdded slightly more defoamerUsed wider film to cast onto to help with spillageResultsCracks formed on thicker sideThickness gradient resulting from unlevel tableWhite color achievedHave a large section of useable crack free tape Still small amount of spillage

Slide21

Run 3

Slide22

Run 3- Results

Changes

Leveled tableCreated slurry as directed by recipeUsed similar doctor blade height as first test to observe if having table level would reduce cracking along with the appropriate amount of ammonium hydroxide addedResultsNo spillage from film, but the slurry did still spread on filmLarge amount of cracking

Slide23

Run 4

Slide24

Run 4

Slide25

Run 4- Results

Changes

Reduced doctor blade height to 0.35 ± 0.02mmIncreased casting speedAdded similar amount of defoamer as Run 2ResultsFirst ~70% of casting had lots of crackingLast ~30% of casting had a mostly crack free zone of good useable tape

Slide26

Run 5

Slide27

Run 5- Results

Changes

Slightly reduced doctor blade height to 0.25 ± 0.02mmCast using 12” doctor bladeDid not add ammonium hydroxideResultsVery small cracking in first few inchesOverall very uniform and crack free tape

Slide28

Run 6

Slide29

ChangesRaised bed cover to vent humidity

Followed recipe from run 5, now standard

Increased doctor blade height slightly to 0.30 ± 0.02mmResultsLeading edge had some crackingSeveral small cracks dispersed throughoutTape dried noticeably quickerOverall very good, useable tapeFound better way to remove tape from Mylar™ backingRun 6- Results

Slide30

Run 7

Slide31

ChangesBed cover was replaced, not vented

Doctor blade increased slightly to 0.33

± 0.02mmResultsFirst ~3 inches and 0.5 inch border cracked, rest of tape was pristine minus a couple small flawsRun 7- Results

Slide32

Sintering

Slide33

Sintering

Schedule: 40*C/hour until 650*C > 145*C/hour until 1200*C/held for 4 hours cooled at 145*C until room temperature

Sintering was done in 1 of 4 different batchesTime at max temperature not confirmed in first batchForth batch max temperature time was lengthened 1 hourStrong texturing in first 2 batches from the “sandwich plates” Some plates have small gaps where tapes are layeredTapes that were sintered without weight on top didn’t adhere together

Slide34

Run

Average Density g/cm

3Std Dev22.760.13543.320.25952.680.16563.120.41873.130.540Density MeasurementsGreenBatch(run)Average Density g/cm3Std Dev% Theoretical Density1 (5)2.990.45150%2 (5)4.220.21871%3 (6)4.890.20381%4 (7)4.170.618

69%

Sintered

The highest density from a single plate came from the third sintering batch with a density of 5.15 g/cm^3 (~85% TD)

Slide35

SEM

Sintering Batch

Average Grain Size (nm)Standard DeviationAppears Porous13120.089Yes22800.098No32830.077No

Slide36

XRD

Values in black represent tetragonal reflections, while values in orange represent monoclinic reflections. Using formulas found in [6] that compare relative intensity ratios, the raw powder was calculated to be 67.5% tetragonal 32.5% monoclinic; the green tape was calculated to be 63.6% tetragonal 36.4% monoclinic. The increase of monoclinic content can be attributed from phase transformation toughening that occurred during ball milling and tape casting. The sintered plates were completely tetragonal as expected based on sintering temperature.

Slide37

Batch

Hardness (HV)

Standard Deviation2950240.443139065.084153071.48VickersVickers microhardness testing was performed on 3 samples from 3 different sintering batches. The average hardness value is based on 10 tests per sample. The average hardness value in literature ranges from 1250-1300 HV.

Slide38

Impact testing was performed by dropping a rod of ATI 718Plus

© that weighed 1.22 kg from various heights.

Impact TestingDrop Height (cm)ResultEnergy (J)Thickness (mm)Layers7.45Pass0.890.4589.58Pass1.140.458

21.59Pass

2.57

0.79

8

21.59

Fail

2.57

0.48

8

21.59

Pass

2.57

0.65

8

21.59

Pass

2.57

1.05

16

21.59

Pass

2.57

1.05

16

21.59

Pass

2.57

1.21

16

32.385

Pass

3.86

0.52

6

32.385

Fail

3.86

0.5

6

Slide39

Using the 100% success rate of the 16 layer samples stopping 2.57 J at minimum, and assuming a linear trend, it would take 78 plates with combined 1248 layers, with a mass of 229.75 g, and a total thickness of 8.58 cm to stop a single 200 J impact.

Achieving 95+% theoretical density should reduce this thickness dramatically

Meeting the Design Goal

Slide40

YSZ was tape casted, sintered, characterized, and impact tested. To meet the design goal it would take an estimated 1248 layers with an estimated thickness and mass off 8.58 cm and 229.75 g respectively.

Summary

Slide41

I would like to thank Dr. Rick Reidy for his insight and help with the project, Polymer Innovations for supplying a sampling of their products for use, David Bryce for performing SEM and XRD on the samples,

Oseoghaghare

Okobiah for sputter coating the SEM samples, Dr. Rajiv Mishra for letting me use his Vickers microhardness tester, and the UNT Materials Science department for providing the funding for the rest of the materials and equipment use. Acknowledgements

Slide42

US Patent: US7556855 B2 US Patent: US7803732 B1

[1]

Fabrication of electrolyte materials for solid oxide fuel cells by tape-casting. P. Timakul et al. [2] Water-based tape-casting of SOFC composite 3YSZ/8YSZ electrolytes and ionic conductivity of their pellets. C. Suciu et al. [3] NIJ Guide 100-98. US Department of Justice. Selection and Application Guide to Police Body Armor [4] Report No. D-2009-047. Inspector General US:DOD. DoD Testing Requirements for Body Armor [5] Tape Casting Theory and Practice. R. E. Mistler, E. R. Twiname. The American Ceramic Society, 2000. [6] Quantitative Analysis of Pholymorphic Mixes of Zirconia by X-ray Diffraction. H. K. Schmid.[7] H. McMurdie, Pow. Diff. Jour., 1, 1986, 275.[8] G. Teufer, Acta. Cryst., 15, 1962, 1187.References