Jones and Co. Consulting

Advanced Ceramics CorpAdvancement of microporous insulation

Presented by: Darnelle Jones, Jeff Kay, Alex Melvin and Steven ChortosMentors: Ritch Mathews and Dr. ZhitomirskyApril 2nd, 2013

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Background Procedure and error Linear change results SEM and XRD Sustainability Gantt chart Future direction Conclusion

Contents

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Investigation done in 2011-2012 on AC80

Assumed by both parties that the properties were the same

AC80i vs AC80

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Background

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AC80i assumptions

Thermally resistant (1000 °C) Made of:

Amorphous fumed silica Rutile titania (mixture) Silica fibres

Process: Mixed together Pressed by 75 ton force Not fired (reduced cost)

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Degradation of thermal properties at 1000°C Onset of sintering

Shrinkage (densification) Cracking

What’s the problem?

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The overall goal of this project is to increase the operating temperature of AC80i by 100°C while keeping it economically viable.

Problem statement

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Testing methods

Fibre coating Reduce fibre-fibre contact (conduction) SEM

Addition of fumed alumina Inhibit sintering and phase change Linear shrinkage SEM XRD

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Procedure and error

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Total days spent testing = 36

Total hours of furnace operation = 966

Total samples tested = 145 Usable samples = 90

Testing overview

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Preparation

Fumed silica, TiO2 and silica fibres weighed and mixed in shear mixer

Alumina addition and final mixing The Al2O3 was weighed and added to the

bucket

Materials were mixed for approx 5 mins using a drill with a paint mixer attached to the end Error in homogeneity of mix

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Testing

Samples tested using a modified version of the ASTM C356-10 testing procedure Samples were placed in furnace and held at

temperature for 24 hours

Measurements Initial samples were measured in each dimension

Significant error due to inconsistent measuring practice

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Radiation Shields

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Ladle example

Feb 12th-19th

Shield #1

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Feb 25th-March 3rd

Shield #2

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March 4th-12th

Shield #3

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March 12th-April 1st (Morgan Thermal Ceramics

– insulating fire bricks)

Shield #4

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Linear change results

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Alumina added

0 wt% (AC80i) 6 wt% 9.5 wt% 12.5 wt% 19 wt%

Final brick design Cost vs linear shrinkage 12.5 wt%

Design compositions

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Importance of testing direction

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Morgan radiation shield

1 2 3 4 5 6 71000

1025

1050

1075

1100

6% Worst Case Scenario

0%6%5% linear change

Linear Change (%)

Tem

pera

ture

(°C

)

1 2 3 4 5 61000

1025

1050

1075

1100

9.5% Worst Case Scenario

0%9.5%5% linear change

Linear Change (%)

Tem

pera

ture

(°C

)

1 2 3 4 5 61000

1025

1050

1075

1100

12.5% Worst Case Scenario

0%12.5%5% linear change

Linear Change (%)

Tem

pera

ture

(°C

)

1 2 3 4 5 61000

1025

1050

1075

1100

19% Worst Case Scenario

0%19%5% linear change

Linear Change (%)

Tem

pera

ture

(°C

)

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Final brick

4 5 61000

1025

1050

1075

1100

1125

1150

ASTM Worst Case

0%FB5% linear change

Linear Change (%)

Tem

pera

ture

(°C

)

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SEM and XRD

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Distribution of titania particles

Hard/soft fracture

Open/closed pores

Coating of silica fibres

Went in looking for:

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Titania Particles

Titania acts as an opacifier, reducing the effects of radiation

Even distribution ensures effective scattering

Titania does appear to be distributed evenly

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3% alumina @ 1025 °C

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Sharp/soft fracture

Looking for: Sharp structures in the 1100 °C heated sample Rounder edges in pre-densified samples

Some differences noted, but results were not definitive

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3% alumina @ 1100 °C

3% alumina @ 1025 °C

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Open/closed pores

Unable to effectively image the pores using SEM

If the samples were mounted and polished rather than crushed, results may have been more informative

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Coating of silica fibres

Compressive shear mixing was proposed to coat the silica fibres in a layer of fumed silica

Munson Machinery was investigated to mix, but communication fell through

Devised our own shear mixing method, but did not achieve fibre coating

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Centrifugal compressive-shear mill

Tomato strainer

33Coated fibres

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XRD Analysis

Went in looking for cristobalite in our samples

Alumina was originally added as a phase change and sintering suppressant

No cristobalite was found, even in the 0% alumina samples Due to the difference in titania content

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Results

2Th Degrees7472706866646260585654525048464442403836343230282624222018161412108

Co

un

ts

11,000

10,500

10,000

9,500

9,000

8,500

8,000

7,500

7,000

6,500

6,000

5,500

5,000

4,500

4,000

3,500

3,000

2,500

2,000

1,500

1,000

0-1000C.raw0-1025C.raw0-1075C.raw0-1100C.raw

2Th Degrees7472706866646260585654525048464442403836343230282624222018161412108

Co

un

ts

16,500

16,000

15,500

15,000

14,500

14,000

13,500

13,000

12,500

12,000

11,500

11,000

10,500

10,000

9,500

9,000

8,500

8,000

7,500

7,000

6,500

6,000

5,500

5,000

4,500

4,000

3,500

10-1025C.raw10-1050C.raw10-1075C.raw10-1100C.raw

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Sustainability

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No increase in health risks to workers or

users

No change in the environmental impact

Environmental

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New markets

No new processing machines needed

Economical

53%

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Gantt chart

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Meeting with Ritch Mathews

Preliminary research

Indepth research of proposed solutions

Meeting with Dr. Zhitomirsky

Problem statement presentation

Meeting with Dr. Malakhov

Proposal presentation preparation

Proposal presentation

Written proposal

Testing preperation and testing

Progress presentation #2

Progress presentation #3

Final presentation preparation

Final presentation

Final written report

9/20/12 11/9/12 12/29/12 2/17/13 4/8/13Proposed Gantt Chart

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Meeting with Ritch Mathews

Preliminary research

Indepth research of proposed solutions

Meeting with Dr. Zhitomirsky

Problem statement presentation

Meeting with Dr. Malakhov

Proposal presentation preparation

Proposal presentation

Written proposal

Initial contact with Munson

Contacting and ordering Al2O3

Contacting for TiO2

Correspondance with Munson

Industry pick-up

Industry visit (sample prep)

Progress presentation #2

Furnace testing (JHE

Correspondance with CANMet

Progress presentation #3

SEM analysis

XRD analysis

Final report

Final presentation preparation

Final presentation

9/20/12 11/9/12 12/29/12 2/17/13 4/8/13

Final Gantt Chart

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Future direction

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General Heat Equation

q” = kΔT + hΔT + ϵσΔT4

ConductionConvection

Radiation

k: thermal conductivityh: convective heat transfer coefficientϵ: emissivityσ: Stefan-Boltzmann constant

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Optimize particle size / opacifier material

Optimized opacifier = less radiant heat transfer

Evidence through radiation shields

Radiation shield in industry

Recommendations

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AC80i radiation shield

0 5 101000

1025

1050

1075

1100

Densification Results (AC80i Shield)

6%9.5%12.5%19%5% linear change

Linear Change (%)

Tem

pera

ture

(°C

)

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Morgan radiation shield

1 2 3 4 5 6 71000

1025

1050

1075

1100Worst Case Densification Results

6%

9.5%

12.5%

19%

0%

5% linear change

Linear Change (%)

Tem

pera

ture

(°C

)

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Design a solid radiation shield

Easy loading and unloading Consistent heating Accurate and reproducible results

Homogenous mix Consistent mixing procedure Reduction in error

Sample orientation Consistent orientation of samples

Suggestions

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AC 80i – Best option up to 1100 °C Less linear shrinkage Cheaper

Conclusion

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Thank you• Ritch Mathews• Dr. Zhitomirsky• All of the MSE faculty

Acknowledgements

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Questions?