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EA-6010-e^

Dist. Category UC-90C

MATERIALS RESEARCH FOR THE CLEAN UTILIZATION OF COAL

Quarterly Progress Report

October - December 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

1

1

I. SUMMARY OF PROGRESS TO DATE

Brief Summary

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

and A. Perloff )

The major effort this quarter has continued to be the completion of

the first issue of pages of the book, "Construction Materials for Coal

Conversion--Performance and Properties Data"; the first version was delivered to the DoE monitor. A talk was given at the Sixth Annual

Conference on Materials for Coal Conversion and Utilization.

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

and S. M. Wiederhorn)

During this quarter, five fused cast refractory bricks were sectioned

and examined for homogeneity. The alumina-zirconia-silica refractory

was chosen for testing on the basis of its good density and its higher

strength and durability during exposure. Creep rupture tests were

continued on the silicon carbide samples discussed previously.
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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 :

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".

The draft manuscript of the first issue of the book was delivered to the

Department of Energy program monitor in the third week of December

without the index. Further material is to be inserted in the book, and

the indexes are to be completed.

A talk was presented at the Sixth Annual Conference on Materials

for Coal Conversion and Utilization in October at NBS. The topic of the

talk was "Information Systems for Fossil Energy Materials Applications"

and presented an overview of data bases which are of use in the fossil

energy field, as well as a description of the data bases of this Data

Center.

Five requests for information were received from various refractories manufacturers following an announcement that refractories data

for use in dry ash gasifiers generated by DoE programs is available from

NBS. The announcement appeared in the November 1981 issue of The Refractories Institute Newsletter.

Plans :

The final manuscript of the book, "Construction Materials for Coal

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

program monitor at DoE. The routine activities of the Data Center, with

respect to receipt and handling of reports and data and the response to

queries, will continue, and work will begin on an update of the book.
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2.

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

and S. M. Wiederhorn)

Experimental Procedures:

Slabs one inch thick were cut from the ends of the five fused cast

billets which are identified as follows:

1. alumina-zirconia-silica

2. alpha-beta alumina

3. alpha alumina

4. chrome-alumina

5. chrome-alumina spinel

Monofrax CS-3

Monofrax M

Monofrax A

Monofrax K-3

Monofrax E

The Monofrax designations are the Carborundum designations. A

compilation of the material properties presented by Carborundum is given

in Table 1. Values for high temperature strength are not presented for

the materials.

Table 1. Properties of fused cast refractories*

Max. Temp. Modulus of Rupture, RT Compressive Strength, RT Thermal Exp.

°C Ksi MPa Ksi MPa cm/cm °C X lO"^

CS-3 1590 9.8 68.6 20 140 7.3

M 1870 3.5 24.5 18 126 7.9

A 1930 5.8 40.9 20 140 7.9

K-3 1870 8.0 56.0 20 140 7.9

E 1930 5.7 39.9 20 140 7.4

*Carborundum

The pictures of the slabs in Figure 1 show the porosity in the

central regions and the range of inhomogeneity across the slab face.

From examination of the slabs, the alumina-zirconia-silica billet appears

more homogeneous than the other billets. This slab was cut into ^50

bars for flexure creep rupture tests. Bars 5 x 10 x 50 mm were cut with

the two orientations shown in Figure 2. Machined specimens were heated

several hours at 800 '’C to remove the grinding oils. The manufacturers
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analysis in wt. percent is: 50.1 AI

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, 34.2 Zr02> 14.2 Si02> 1.1 Na20,

0.12 Fe202» 0.05 Ti02- Phases identified from powder X-ray diffraction

patterns made of the as-received material were alpha alumina, monoclinic

zirconia and an amorphous silica phase. Samples that were heated for 24

hours at 1200 °C, 1300 °C, and 1400 °C had the same powder diffraction

patterns

The creep tests on the silicon carbide samples which were being run for 1000 hour periods were terminated after several hundred hours because

of water cooling problems. A closed cycle cooler was purchased and is

being installed.

Plans :

The flexure strength will be obtained at room temperature and at

1200 °C for the alumina-zirconia-silica specimens. From these results,

the static loads for the creep experiments will be selected. Annealing

conditions required for the precipitation of the tetragonal phase of

Zr02 will be identified. The phase composition and the microstructural

changes will be identified and monitored using powder X-ray diffraction

and analytical electron microscopy.
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Figure 1. Cross-section of slabs from fused-cast billets a) aluminazi rconia-si 1 ica , b) a-3 alumina, c) a alumina, d) chrome

alumina, e) chrome-alumina spinel.

Figure 2. Section of billet of alumina-zirconia-si 1 ica showing

orientation of test bar specimens.
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