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Dist. Category UC-90C

MATERIALS RESEARCH FOR THE CLEAN UTILIZATION OF COAL

Quarterly Progress Report

July - September 1982

S. J. Schneider

Project Manager

Center for Materials Science

National Bureau of Standards

U. S. Department of Commerce

Washington, D. C. 20234

PREPARED FOR THE UNITED STATES DEPARTMENT OF ENERGY

Office of Advanced Research and Technology

Under Contract No. EA-77-A-01-6010

"This report was prepared as an account of work sponsored by the United

States Government. Neither the United States nor the United States

Department of Energy, nor any of their employees, nor any of their

contractors, subcontractors, or their employees, makes any warranty,

expressed or implied, or assumes any legal liability or responsibility

for the accuracy, completeness, or usefulness of any information,

apparatus, product or process disclosed, or represents that its use would not infringe privately owned rights."

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TABLE OF CONTENTS —- PAGE

I. SUMMARY OF PROGRESS TO DATE. .

' 1

II. DETAILED DESCRIPTION OF TECHNICAL PROGRESS . 2

1. Materials Performance and Properties 2

2. Creep and Related Properties of Refractories .... 3

i

1

I. SUMMARY OF PROGRESS TO DATE

Brief Summary

1. Materials Performance and Properties (H. M. Ondik, B. W. Christ,

and A. Perl off)

The book, "Construction Materials for Coal Conversion--Performance

and Properties Data," has been completed, was published in September and

is now available for sale from the Superintendent of Documents, Government

Printing Office.

2. Creep and Related Properties of Refractories (N. J. Tighe, C. L. McDaniel,

and S. M. Wiederhorn)

Unit creep measurements were made on the five fused cast oxide

refractories in order to identify the maximum use temperatures under

static stress conditions. The materials were tested up to 1400 °C using

stresses of 10 to 30 MPa (1.4 to 4.4 kpsi). Strength measurements of

siliconized silicon carbide were made at temperatures up to 1400 °C

preliminary to carrying out static load tests.
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II. DETAILED DESCRIPTION OF TECHNICAL PROGRESS

1. Materials Performance and Properties (H. M. Ondik, B. W. Christ,

and A. Perloff)

Progress ;

The book, "Construction Materials for Coal Conversion- -Performance

and Properties Data," has been completed. During the last quarter, the

various incomplete subsections were finished and reviewed. The total

manuscript was revised, reviewed by the publications division and submitted

for publication. The printed books, with issue date September, 1982,

are in hand and available for purchase. The book is a National Bureau

of Standards Special Publication, number 642. NBS SP642 is available

under stock number 003-003-02442-2 from the Superintendent of Documents,

Government Printing Office, Washington, DC 20402, for $16.00 (add 25%

for mailing outside the U.S.).
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2. Creep and Related Properties of Refractories (N. J. Tighe, C. L. McDaniel,

and S. M. Wiederhorn)

Progress :

Failure stresses and temperatures for the five fused cast oxide

refractories were determined under conditions of unit creep. In this

technique specimens were held under constant stress for periods of 24

hours at temperatures starting at 800 °C; and, then the temperature was

raised 100 °C each 24 hours until excessive creep or failure by crack

propagation occurred. Measurements were made using stresses of 10, 20

and 30 MPa for each of the materials. The results of the tests are

summarized in Tables 1 and 2. The most creep resistant materials were

the a alumina and the chrome alumina spinel, as determined from the

deflection measurements.

The microstructures of two fused cast materials are shown in

Figure 1. The varying grain size and porosity in the materials are

clearly seen in these light micrographs. Thin sections of the materials

were made for examination by electron microscopy in order to identify

the phase distribution within the compacts.

Some preliminary tests were carried out on a siliconized silicon

carbide material. The billet was one of five received from the Norton

Company and designated NC-435. The billet was 10 x 10 x 0.6 cm and was

cut into bars 4 x 5 x 50 mm for testing in four-point bending mode.

Sets of 3 bars were broken at room temperature and after holding for one

hour at 1200, 1300, and 1400 °C. The results are shown in Table 3. The

strength decrease at 1400 °C occurred, of course, because the silicon

space filling component melted. Spheres of melted silicon were found on
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the fracture surface of specimens broken at 1400 °C. The silica film

that formed on the exposed ground surfaces during the soaking period

prevented the phase from extruding through these surfaces.

Specimens were held under a static load for 168 hours to determine

any creep or strength loss as a result of stress. As seen from the

tabulation in Table 4 there is a slight strength increase. There was no

measurable creep during this period.

Plans :

A final report on the fused cast and silicon carbide materials will

be prepared and will include the creep results as well as the microstructural analyses.
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1 Table 1. Summary of strength obtained with dynamic load.

Material — Modulus of Rupture, Dynamic

MPa

25 X 1000 °C

AlaOa'ZrOa'SiOa

Monofrax CS-3

93.0 + 7.5 109.0 + 13.8

25 X 1100 X

a + 3 AI 2 O 3 Monofrax M

38.1 + 1.9 36.2 + 3.0

a AI 2 O 3 Monofrax A64.6 + 5.6 52.3 + 1.8

Cr-M Spinel

Monofrax E '37.0 + 2.4 47.5+ 4.3

Cr-A£ Oxide

Monofrax K-3

42.2 + 3.4 27.3 + 10.0

Table 2. Failure temperature for samples under static load.

Material Static Load 10 MPa

Failure Temperature °C

Static Load 20 MPa

Failure Temperature °C

Static Load 30 MPa

Failure Temperature °C

A1 2 O 3 • Zr02 • Si

O

2 Monofrax CS-3

900 900 800

a + 3 A1 2 O 3 Monofrax M

1400 1100 *

a AI2O3

Monofrax A

1300 1300 *

Cr-M Spinel

Monofrax E

1400 1100

Cr-AJl Oxide

Monofrax K-3

1400 1100

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Table 3. Strength of Siliconized SiC

Temperature

25

1200

1300

1400

Modulus of Rupture

MPa

367 + 74

439 + 47

376 + 56

91 + 30

Table 4. Strength of siliconized Sic after

1 168 hours under static load.

Temperature Static Load Modulus of Rupture

X MPa MPa

1200 100 481 + 59

1300 100 394 + 38
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Figure 1. Light micrographs of polished sections of fused cast refractory

samples, (a) alumina-zirconia-sil ica, showing plates of

alumina and alumina containing zirconia in an alumina-silica

glass; (b) chrome-alumina showing plates of chromia in a chrome alumina matrix.
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