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MATERIALS RESEARCH FOR THE CLEAN UTILIZATION OF COAL

Quarterly Progress Report

April - June 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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I. SUMMARY OF PROGRESS TO DATE

Brief Summary

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

and A. Perloff )

.

Completed sections of the book, "Construction Materials for Coal

Conversion—Performance and Properties Data", have been submitted to

readers, and corrections and changes are being made in the manuscript.

Several remaining subsections are being completed. Normal activities of

the Data Center with regard to handling of reports and data and responding to queries have been conducted.

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

C. L. McDaniel and S. M. Wiederhorn)

Specimens from the five fused cast refractory bricks were tested

under unit creep to determine the upper temperature limit for use without

appreciable creep.
••
TABLE OF CONTENTS

I.

II.

PAGE

SUMMARY OF PROGRESS TO DATE 1

DETAILED DESCRIPTION OF TECHNICAL PROGRESS 2

1. Materials Performance and Properties 2

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

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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 :

Major emphasis this quarter has continued to be the compilation of

the book, "Construction Materials for Coal Conversion—Performance and

Properties Data." The present version of the manuscript (over 600

pages) has been reviewed by readers who are well qualified in metallurgy

and refractory science. Suggested changes and corrections have been

made. The current status of the subsections mentioned in the last

quarterly report as being in progress is as follows: the two refractories

subsections are complete and are being reviewed by the readers; the

discussion of materials tested for aqueous corrosion resistance is half

finished; the subsections dealing with in-plant service performance of

materials in various components of coal gasification pilot plants is

only partially complete. Preparation of the final version of the index

is dependent upon completion of these subsections. A cover design for

the looseleaf binder of the book was submitted to the DoE sponsor, and

approval has been given for the use of the design.

Appreciable time was spent in performing a number of searches of

the plant performance computer data base, not only in order to respond

to queries received this last quarter, but also to update and maintain

an office file of copies of the various sort lists which can be obtained

from the computer. Ten different variations of the data base contents

have been printed and filed.

The regular activities of the Data Center, as outlined in previous

reports, have continued: receiving and cataloging of DoE materials

research contractors' reports, answering queries, and abstracting data.

Plans :

The complete manuscript of the book, "Construction Materials for

Coal Conversion—Performance and Properties Data," will be sent to the

sponsor. The regular activities of the Data Center will continue.

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

McDaniel and S. M. Wiederhorn)

Progress :

The slabs of the five fused cast refractories were cut into bars

5 X 10 X 50 mm. Because of porosity in the refractories, the number of

bars cut from each slab varied from 50-100. The bars were ground

longitudinally and were numbered according to their position in each

slab. They were chosen for testing in accord with a set of generated

random numbers. The bars were tested in four-point bend configuration

using alumina fixtures. For the dynamic modulus of rupture tests, six

specimens were broken at 25 °C; and three specimens were held at 1000 °C or 1100 °C for one hour before breaking. For the initial creep tests,

bars were held under static load of 10 MPa (1400 psi) for 24 hours at

temperatures from 800 °C to a maximum of 1400 °C. The temperature was

increased 100 °C after 24 hours until at least one of three specimens

showed rapid creep or failed by creep rupture. This mode of testing was used to establish quickly the maximum use temperature.

The data are summarized in Table 1. The creep behavior of the

alumina-zirconia-silica (AZS) (CS-3) samples was discussed briefly in

the last report. The AZS samples failed at 900 °C when the glassy

silicate phase softened. Thus, although the material has high strength

under rapid loading conditions, it has essentially zero strength under

static load conditions at temperatures >_ 900 °C. The other four refractories

in Table 1 retained some strength under static load of 10 MPa at temperatures

up to 1400 °C.

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Table 1. Summary of Strength and Static Load Tests

Mater ial Modulus of Rupture, Dynamic

MPa

Creep

Temperature

°C

Failure

Static Load

MPa

25 °C 1000 °C

AZS 93.0 + 7.5 109.0 + 13.8 900 10

Monofrax CS-3

25 °C 1100 °C

a + 3 AI 2 O 3 38.1 + 1.9 36.2 + 3.0 1400 10

Monofrax M

a AI 2 O 3 64.6 + 5.6 52.3 + 1.8 1300 10

Monofrax A

Cr-A& Spinel 37.0 + 2.4 47.5 + 4.3 1400 10

Monofrax E

Cr-A& Oxide 42.2 + 3.4 27.3 + 10.0

Monofrax K-3

Plans

The creep rates will be obtained using different static loads near

the maximum use temperatures. The microstructure will be examined by

light and scanning electron microscopy to identify the failure sites.
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