MATERIALS RESEARCH FOR THE CLEAN UTILIZATION OF COAL

Quarterly Progress Report

July - September 1981

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 tne 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."

EA-6010-28

Dist. Category UC-90C

MATERIALS RESEARCH FOR THE CLEAN UTILIZATION OF COAL

Quarterly Progress Report

July - September 1981

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."

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

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I. SUMMARY OF PROGRESS TO DATE

Brief Summary

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

A. Perloff, and W. A. Willard)

The major effort this quarter has continued to be concentrated on finalizing the first edition of the book, "Construction Materials for Coal

Conversion--Performance and Properties Data". The "Materials Evaluation"

sections are nearing completion, and the "Index" section is being keyboarded

for computerized manipulation and printing. Preparation of next year's

plans and a talk to be given at the Sixth Annual Conference on Materials

for Coal Conversion and Utilization was done. Regular activities of

cataloging and abstracting reports and responding to queries are continuing.

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

S. M. Wiederhorn)

Work during the quarter was concentrated on obtaining static load

data for hot-pressed silicon carbide and alpha alumina. Five compositions

of fused cast oxide refractories were obtained from the Refractories

Division of Carborundum for use in our testing program. These

are 6 x 4 x 24 in and are the smallest size available. The 5 compositions

and product designations are:

1. alumina-zirconia-silica Monofrax CS-3

2. alpha-beta alumina Monofrax M

3. alpha alumina Monofrax A

4. chrome-alumina Monofrax K-3

5. chrome-alumina spinel Monofrax E
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1. Materials Performance and Properties (H. M. Ondik, B. W. Christ,

A. Perloff, and W. A. Willard)

Progress : Data Center activities for the past quarter have included the

regular data activities; receiving and cataloging reports, answering

queries, abstracting data, etc., as well as work on the book, "Construction

Materials for Coal Conversion--Performance and Properties Data". Time

during the quarter was also spent in preparation of plans for the next

year of the project and in gathering material for a talk to be presented

at the Sixth Annual Conference on Materials for Coal Conversion and

Utilization in October at NBS. The topic of the talk is "Information

Systems for Fossil Energy Materials Applications" and will present an overview of data bases which are of use in the fossil energy field, as well as a description of the data bases operated by this Data Center.

In preparation for setting up the full computer data base for

Materials Properties beginning in the next quarter, the bibliography

has been coded for computer input so that keyboarding of the information

may start with the next contract period.

Completion of the first edition of the book of data for construction

materials has been the main occupation of the Data Center staff for this

last quarter. The "Performance Data" portions of Section A have proven

more time-consuming to prepare than was at first anticipated, but they are being put into final manuscript form. These "Materials Evaluations" pages

will include summaries and evaluations of the data which appear in Section B,

"Materials Testing Results". The index, which will enable users to

find data for specific materials and specific properties, is so vital

to the usefulness of the book that great care must be taken in its

preparation. A written form of the index has been completed and is

being keyboarded for entry into computer files. Since the index cannot

be considered finished unless all portions of the book are included,

it is necessary to make provision for entry of index items as sections

of the book are completed in manuscript form. With the portion of

the index which is finished so far in the computer, it will be possible

to add items, sort, edit, and even prepare the manuscript version of

the index under computer control. It is anticipated that the draft

manuscript of the first issue of the book will be delivered to the

Department of Energy program monitor by the end of October.

Plans :

The manuscript of the book, "Construction Materials for Coal

Conversion--Performance and Properties Data", will be delivered to the

program monitor at DoE. The major keyboarding effort will be started

to place the data of the Materials Properties Data Base on magnetic

tape and into the computer data base management system. The routine

activities of the Data Center, with respect to receipt and handling

of reports and data and the response to queries, will continue.
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2. Creep and Related Properties of Refractories (N. J. Tighe, C. L. McDaniel,

S. M. Wiederhorn)

Experimental Procedure : Static load data were obtained on, 1) alpha alumina

(Monofrax A) bars 5 x 10 x 50 mm at 1200 °C, and 2) hot-pressed silicon carbide

(NC 203) bars 3 x 4 x 50 mm at 1200 °C, 1400 °C and 1500 °C. The bars were

tested in four point bend configuration and the specimen deflections were

measured continuously during the test periods of up to 1000 hours.

Results :

Alpha alumina (Monofrax A): The static load tests for the fused-cast

bar specimens were scheduled to last 1000 hours with a stress of 20 MPa in

order to compare the results with the simple compression tests. The first

test of 3 specimens terminated at 596 hours because of a cooling water failure;

the specimens were cooled to room temperature under load. The deflection

curve, shown in figure 1, was obtained from the LVDT readings and was plotted

for one hour intervals for the first 24 hours and at 24 hour intervals for

the remaining 23 days. As seen in the curve a constant deflection rate of

5.6 X lO'^s"^ was recorded after 'a^ 50 hours under load. The measured

deflection rates for the two regions of constant deflection are shown in Table 1.

Table 1. Static Load Deflection Rate for Fused Cast Alpha Alumina at 1200 °C

and 20 MPa.

Specimen Region I (in/in/s) Region II

1 8.1 X 10'^ 1.1 X 10'^

2 4.4 X 10‘® 4.7 X 10’^

3 6.1 X 10'^ 5.6 X 10’^

The test bars were bent noticeably when removed from the furnace but had

not fractured during cooling. Only alpha alumina was present in the x-ray

diffraction pattern in accord with earlier observation on the loss of beta

alumina during heating. A second series of samples is being run to complete

the 1000 hour test.

It should be noted that the Monofrax A material contains 3-10% beta alumina

in the as-received condition and that the beta phase is lost after heating

at 1200 °C. This behavior was discussed in earlier reports.

Silicon Carbide (NC 203 ): Silicon carbide has important uses in high

temperature moderate stress applications. Our initial strength measurements

were made after exposure at 1200 °C, 1400 °C and 1500 °C for times up to

1000 hours. The results of the tests for averages of 3 specimens per furnace

are shown in Table 2. It is clear that the strength decreases significantly

after exposure at 1500 °C.
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Table 2. High Temperature Flexure Strength of SiC (NC 203)

Temperature °C Time

"o" load

1200 1/2

1200 168

1400 168

Static Load

1500 168

200 MPa 1200 168

150 MPa 1400 168

hr . Flexure Strength, MPa

427 ±92

419 ±137

413 ±23

339 ±13

496 ±38

419 ±26

Static load tests were undertaken as part of the program to evaluate the

strength degradation, and to identify failure mechanisms under stress. During

this quarter tests have been conducted at 1200 °C, 1400 °C and 1500 °C under

static load of 150-300 MPa for one week. Specimens were broken at the end

of the test period at temperature without removing the static load. Loads were

selected from consideration of the strengths in Table 2. The initial results

are summarized in figure 2 which shows the failure times and the static loads.

Creep was not detected at 1200 °C under the loads used; and some specimens

failed during the test indicating that crack propagation occurred. The

reduction in percent of failures by lowering the applied stress indicates we

are close to a static fatigue limit at 1200 °C. At 1400 °C three specimens

under a stress of 150 MPa survived for one week and showed little or no creep.

The three specimens tested at 1500 °C broke within 9 hours. These test series

of one week exposures should be finished during the next quarter.

Plans : The static load test series on silicon carbide NC 203 will be

continued to achieve at least one week and then 1000 hour durability tests

at 1200 and 1400 °C. Specimens of sintered alpha silicon carfeide have been

prepared and will be scheduled for the long-term tests during the next few

quarters. The Monofrax series will be analyzed to compare the compressive

and flexure test procedures. We will try to obtain additional samples

of the same production run from Montana State. The fused-cast refractories

will be cut into slabs and examined for homogeneity before cutting out test

samples. The Refractories Division at Carborundum has done some testing

on these materials and we will coordinate our tests with theirs.
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Figure 1. Deflection measured at 1200 °C for alumina (Monofrax A) with

static load of 20 MPa.

Figure 2. Plot of static lo^d ys. failure time for hot-pressed silicon

carbide ^NC 2Q3).
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