EA-6010-28

Li ^ Dist. Category UC-90C

k‘ U

MATERIALS RESEARCH FOR THE CLEAN UTILIZATION OF COAL

Quarterly Progress Report

April - June 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 responsibi 1 ity

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 .... 24

1

I. SUMMARY OF PROGRESS TO DATE

Brief Summary

1. Materials Performance and Properties

The major effort this quarter has been concentrated on the book

"Construction Materials for Coal Conversion —Performance and Properties

Data". The status of the various subsections of Section A (Materials

Considerations and Performance Data) is: 1) "Operating requi rements"—

completed, 2) "Performance Data" and "Candidate Materials" - being

drafted in final form. The assembling of test data for Section B is

essentially complete and analysis of this data is in progress. An

example of such an analysis is included in Appendix I. Background

and status of the computerized data bases is given in Appendix II.

The Data Center has transmitted 1100 computer abstracts of failure

events and ten hard copy reports in response to queries during this

quarter.

2. Creep and Related Properties of Refractories

Data was obtained on the creep of a fused cast a+B alumina

(Monofrax A) under thermal cycling conditions and on silicon nitride

using both linear variable differential transformers and specimen

dimension measurements.

1
II. DETAILED DESCRIPTION OF TECHNICAL PROGRESS

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

A. Perloff, W, A. Willard)

Progress : During the last quarter the Data Center has received five

requests for information and has responded by providing 1100 computer

abstracts of failure events and analyses and ten hard copy reports.

The major thrust of the Data Center effort this last quarter has been the

work on the book "Construction Materials for Coal Conversion--Performance

and Properties Data" in order to deliver the draft to DoE by the end of the

fiscal year. Completion of data tables for Section B, "Materials Testing

Results", and assembling these pages with appropriate headings and Tables

of Contents has been a massive job. Section B contains the summary tables

and graphs of data abstracted from the DoE materials research contractors

'

reports. Just one section, that on corrosion in alloys, consists of over 120

tables of graphical summaries, many of which are contained on several pages,

from 2 to almost 20 pages. Each of the subsections will have a separate

Table of Contents in addition to the main Table of Contents at the beginning

of the book. The main Table of Contents will contain only the major headings,

the contents of each smaller section being too voluminous to permit inclusion

and still have the Table convenient and usable.

Page headings for each page have been designed and are being entered on each

page of the book. These headings will identify the section of the book to

which that page belongs. For instance, the following are typical page headings

chosen at random:

A.l Coal Handling and Preparation Equipment

A. 1.1 Conveying Equipment

A. 1.1

page 1 of 1 -

A. 2. 2 Refractory Linings and Components--Dry-Bottom Vessels

A. 2. 2. 2 Performance Data

A.2.2.2.1

.

page 1 of

, 4

1 -

B.l Corrosion Effects, Chemical Reactions, and Phase Changes

B. 1 . 1. A1 loys

B.l. 1.15

page 2 of 7

-

B.l Corrosion Effects, Chemical Reactions, and Phase Changes

B. 1 . 2 Refractories

B.l .2.16

page 2 of 10

B.2 Erosion, Erosion/Corrosion, and Abrasion Effects

B.2.1 Alloys

B.^. 1.21

page 1 of 2

-

B.3. Mechanical Properties Testing

B.3.2 Refractories

B.3.2. 10

page 1 of 1 -

The identification of pages by such page headings will enable the user who

wishes to find specific tables, perhaps having first looked for a specific

material in the index, to keep track of the location of sections and tables

within the book.

2
Work on the index is progressing well. Since the index, which will enable

users to find data for specific materials and specific properties, is so vital to the usefulness of such a book, great care must be taken in its

preparation. The subsections of Section A, "Materials Considerations and

Performance Data", are in varying stages of preparation. The "Operating

Requirements" subsections are complete, while the "PerformanceData" and "Candidate

Materials" subsections are being drafted in final form. The analysis of data

from Section B is progressing. An example of such an analysis, taken from

the area of mechanical properties, is in Appendix 1.

Because of the enormous amount of effort needed to assemble the book in

final form, work on the computer data bases has lagged somewhat. Keyboarding

of masses of data has not begun, only small portions of test batches having

been entered. In order to save computer storage costs, little of the Materials

Properties Data Base is being retained in the computer at this time. The

Materials and Components Plant Performance Data Base is, of course, being

maintained fully in order to answer queries and enter new information as it

is submitted.

Appendix 2 constitutes a report on the background and current status of the

Data Base design for both data bases. Properties and Plant Performance, as required by our work statement.

Plans : During the next quarter, the final writing of sections and assembling

of the book "Construction Materials for Coal Gasification--Performance and

Properties Data" should be completed. The usual routine work of cataloging

reports, abstracting data, and answering queries will continue.

3
Appendix 1

Example of a section A "Materials Evaluation" Segment. The accompanying B section pages are not included.

Mechanical Properties of Metal Alloys Used

In Coal Gasification System

Mechanical properties, such as tensile test results, hardness, and fatigue

crack growth rates for metal alloys used in coal gasification systems are reviewed in this section. The focus is on nickel alloys, 2 1/4 chrome-1

molybdenum steels, stainless steels and low-carbon steels in various

environments, including hydrogen sulfide, hydrogen, dry argon, vacuum and

typical coal gasification atmospheres. Data tabulations appear in Sections

B.3.1.8 through S. 3. 1.12 and B.4,1.1 through B.4.1.3.

Some uniaxial tensile data on four alloys tested at elevated temperatures

appear in Table B.3.1.8. The yield and tensile strengths of each alloy

decreased with increasing temperature. The elongation shows a mixed response

to increasing temperature. In some cases it increased and in others it

decreased.

Some high temperature tests were performed to evaluate the effect of exposure

to typical coal gasification atmospheres on the uniaxial tensile properties

of four alloys (Table B.3.1.9). Exposure was for 100 hours at pressures of

500 and 1500 psi (34 and 102 atmospheres). Temperatures were 1382, 1600 and

1800 "’F. Two typical coal gasification atmospheres were used. The gas

compositions for each combination of pressure and temperature appear in

Table B.3.1.9, Hydrogen sulfide concentration ranged between 1 and 2 percent

and was close to 1% for atmosphere number 2. Following exposure, specimens were removed from the atmosphere and pulled to fracture under dry-flowing

argon in a constant crosshead speed testing machine at a temperature of 1382,

1600 or 1800 °F, Specimen design conformed to ASTM Designation E8. The

following tensile properties were measured: yield strength, tensile strength,

uniform strain and total elongation in a two inch gauge length. Test results

appear in figures 1 through 4, along with a reference value determined at

temperature on an unexposed specimen.

In general, these results show that a 100-hour exposure to the coal gasification atmospheres does not significantly affect the stability of the

tensile properties of the four alloys tested. Property changes are small,

but nevertheless, noticeable. Properties showed both increases and decreases.

In general, elongation changed more than strength. For example, the maximum

change in total elongation was a 50% decrease, whereas the maximum change

in yield strength was a 30% increase. Most of the observed changes in tensile

properties were smaller, e.g., ±10%. Figures 1 and 2 show that the yield and

tensile strengths of each alloy decreased with increasing temperature. The

elongation shows a mixed response to increasing temperature for all four

alloys. In some cases it increased and in others it decreased. These results

are the same as for unexposed specimens tested in vacuum (see Table B.3.1.8),

indicating that exposure to typical coal gasification atmospheres for 100 hours

does not have a major effect on the temperature dependence of tensile properties

for these alloys.

4
Figures 1 and 2 show that effects of the pressure of the coal gasification

atmospheres, 500 vs. 1500 psi, on the observed strength changes, were small.

Strength-change differences between the 500 and 1500 psi tests were about

±10%. Elongation-change differences between the 500 and 1500 psi tests

were somewhat larger, i.e., about ±20% (Figure 4).

Some 1000-hour aging treatments in vacuum were carried out at 1382, 1600

and 1800 °F, on some untreated test specimens to facilitate a comparison

of tensile property changes due to aging and to typical coal gasification

atmospheres (Table B.3.10). Exposure times were 1000 hours in vacuum

and in the coal gasification atmospheres. Two coal gasification atmospheres

were used at pressures of 500 and 1500 psi. The gas compositions for each

combination of pressure and temperature appear in Table B.3.10. Hydrogen

sulfide ranged between 1 and 2 percent, and was closer to 1% for atmosphere

number 2. Specimen design conformed to ASTM Designation E8. Specimens

were pulled to fracture under dry flowing argon in a constant crosshead

speed testing machine. Properties measured were ultimate tensile strength,

uniform strain and total elongation.

Test results appear in figure 5. The ratio of the property of the exposed

specimen to the property of the aged specimen has been plotted. Values

greater than one indicate an increase in the property of the exposed

specimen relative to the aged specimen, and vice-versa. In general, the

ratio for uniform strain showed a greater change with exposure than did the

ratios for total elongation and tensile strength. Inconel 671 and USS 18-18-2

showed the largest increases in the ratio for uniform strain, with the largest

ratio being 4.9. About half the tests for uniform strain showed a decrease in

the ratio, with the lowest ratio being 0.4.

Effect of Temperature and Environment on Fatigue of 2 1/4 Cr-1 Mo Steel

Fatigue crack growth kinetics of 2 T/4 Cr-1 Mo steel were evaluated in various

environments and over a range of temperatures and pressures. The test

environments were: vacuum, dehumidified argon, water vapor, dehumidified

hydrogen and hydrogen sulfide. Temperatures ranged between 295 and 477 °K.

Pressure varied between 0.1 and 5.0 torr in some tests. Results appear in

B. 3. 1.11 and B. 3. 1.12. These figures show that crack growth rate was in

the range 10'- to 10”5 inches per cycle for 20 <aK< 70. Increasing frequency

from 5 to lOHz Increased crack growth rate slightly. Crack growth rate

increased with increase in stress intensity factor range. For a fixed value of

stress intensity factor range, crack growth rate generally decreased with

Increase in temperature. Hydrogen sulfide atmospheres caused fastest crack

growth rates, and rates increased with increasing hydrogen sulfide pressure.

Dehumidified hydrogen caused the second fastest crack growth rates. Water

vapor, dehumidified argon and vacuum tests resulted in comparable crack

growth rates at AK^50MPa-m^/ 2

^

Effects of Exposure to Flue Gases from Four Different Coals

Six alloys, one clad alloy and 5 combinations of welded alloys were exposed

to flue gases from four different coals to determine how the different gases

affected the materials. Depth of corrosive attack and/or hardness were

measured to evaluate changes in the alloys. The test specimens were 2-inch

O.D, pipe sections threaded together to form two lengths of pipe, one of the

5
welded alloys and one of the remaining alloys. The pipe exteriors were

exposed to the flue gases in coal-fired commercial steam generators. Air

flowed inside the pipes to control temperature. Temperatures ranged from

800 to 1440 °F. Exposure times were from 3144 to 7368 hours. Data appear

in Tables B.4.1.1 and B.4.1.3. Tables I and II show some of the trends

detected for the influence of temperature and exposure time on severity

of corrosive attack or hardness changes. Severity has been rather

arbitrarily classified as low, medium or high, using the full range of

depth of attack in Table B.4.1.1 as the basis. Table B.4.1.3 shows that

weld hardness for three of the five combinations of welded alloys investigated

is significantly higher than for the other two. This table also shows that

lack of penetration is common to all five combinations of welded alloys.

6
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TABLE I

Severity of Corrosive Attack of Several Alloys

by Flue Gases From Four Coals

Subbitum

C

HV

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HV

Bitum. A

Lignite A

316SS L-M* M L-M L

31 OSS L L L L

12R72 L L L-M M-H

Incol oy

800

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Inconel

617

L-H L-M L L

Haynes

188

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Inconel

671

Clad on

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H L-M L L-H

*L - Low severity - 0 to 2.5 mils deep.

M - Medium severity - 2.5 to 4.5 mils.

H - High severity 4.5 to excessive.

12
Table n

Trends in

in coal “fired

hardness changes

commercial steam

for alloys exposed

generators.

to flue gases

ALLOY

Hardness Change f 1 ue__Gji_s Exposure From Each Type of Coal

Subbi Luminous C HV Bituminous C HV Bituminous A Lignite A

316 SS i ncreased decreased i ncreased increased

310 SS decreased decreased increased decreased

12 R 72 decreased decreased increased decreased

Incoloy 300 increased decreased increased decreased

Inconel 617 decreased increased i ncreased increased

Haynes 188 increased increased i ncreased increased

Inconel 671

clad on Incoloy 8u0

decreased decreased no change decreased
Appendix 2

Development and Design of Compatible Data Bases for Materials and Components

Plant Performance and for Materials Properties

The Materials and Components Plant Performance Data Base has operated since

1976 (under the title of Failure Information). The program began with the

submission to DoE and NBS of reports of operating events at coal gasification

and liquefaction pilot plants and development units. These operating event

reports, usually of failures of materials and components, were carefully

reviewed and the data abstracted and summarized by NBS staff experts in

materials. Frequently, the reports of the event are followed by comprehensive

diagnostic failure analyses which often contain recommendations for future

failure avoidance, and these reports are also abstracted and summarized. These

abstracts, containing all the pertinent information in the reports, were maintained as a data base in computer storage using a Data Base Management

System (DBMS) available on a government agency computer which was satisfactory

for the simple structure of the data base. The data stored in the computer

consists of the abstract as a block summary along with some nine keywords

which identify the abstract and permit the data to be retrieved by the use of a variety of the keywords. The data base can be searched and the file

sorted by one or any combination of these keywords--material name, component

name, process or plant name, failure mode, etc. The structure of this data

base is entirely suitable and no revision has been considered necessary.

The requirements of the Materials Properties Data Base, however, could not

be supported by the simpler DBMS being used by the Plant Performance Data

Base. The design of The Materials Properties Data Base has evolved over a period of time although the complex structural relationships between data

items demanded by the nature of the data ‘have not changed. The data are

so varied in kind and style that a very flexible computer system is required

to handle them.

The numeric data include single-value numbers, ranges of numbers, and

values taken by digitizing values from graphs and histograms. Descriptive

textural information must also be accommodated in the computer. Along with

the data the specific experimental conditions must be stored as well as pertinent facts about the test procedure used. Each material must be

designated not only by appropriate synonyms but also by the processing

methods used, including its thermomechanical history. The data base must

be of such a design that it is open-ended with respect to the addition of new types of data as well as possible multiple entries from different sources

for similar information. Full bibliographic reference information must also

be included.

Data Center staff personnel have had the benefit of Data Base Management

System (DBMS) courses as well as practical demonstrations of a number of

DBMS by computer vendors. The first class was a special three-day general course taught by Professor E. Sibley of the University of Maryland. Staff

were introduced to the characteristics of DBMS, the great variety, advantages

and disadvantages of the various types of DBMS, and were also given a good

many caveats concerning the choice and use of such systems. We also had the

benefit of information in an NBS publication which compared several DBMS

14
(iNBS Technical Note 887, "Six Data Base Management Systems: Feature Analysis

and User Experience", by E. Fong et al., November 1975), as well as a number

of NBS Special Publications dealing with general information about DBMS and

interactive computer services. Using the knowledge thus gained the staff

decided to put further study into a specific major DBMS which has a hierarchical

structure. A week's course was taken and a data base was designed establishing

the data relationships required. A full description of this data base design

was reported in report EA-6010-18, "Materials Research for the Clean Utilization

of Coal", Quarterly Progress Report, October-December 1978.

A sample data base was set up using the hierarchical DBMS under a temporary

contractual arrangement. Testing of this sample materials properties data

base revealed that, although data storage was relatively economical in the

hierarchical structure which eliminated the necessity to repeat any information,

the query system was very complicated. Questions had to be very carefully,

often intricately, worded to insure the correct searches and answers. This

system would prove expensive in personnel time for use in our work, and we

considered it unsuitable for further serious consideration.

The sample data base and structure of this hierarchical system was extremely

valuable in providing a basis from which the competing vendors could work in

setting up demonstrations of their ability to cope with our data and in

performing benchmark tests upon which costs were based in awarding the

contract. Data Center Staff did have to expand the amount and kinds of data

in the base to provide for benchmark tests of realistic complexity. The

procurement procedure was a prolonged one, partly because of the fact that

commercial vendors are well-acquainted with business-oriented data bases but

have little or no experience with the kind of complex technical data with

which we deal

.

Services of a commercial computer vendor were procured which enable us to

fulfill the complex computer requirements as well as the need to comply with

the sponsor's request that we provide for future direct on-line access

capability for non-NBS users. The services include direct computer access

through a nationwide network and suitable computer software for managing

the data base in the form of a Data Base Management System. The DBMS now

In use is well-known as a "user-friendly" system, a real advantage for future

direct searching access by non-NBS users.

As reported in the January-March 1981 quarterly report, the Materials and

Components Plant Performance Data Base, having already been established

within a different DBMS, was transferred to the vendor's computer on the new

DBMS, maintaining the same capabilities for search and the same structural

relationships. The Plant Performance Data Base is operating on this new

system. The Materials Properties Data Base is being designed to be compatible

with the Materials and Components Plant Performance Data Base and will be

keyboarded as rapidly as possible.

Data bases are characterized in structure as hierarchical , relational, or network. The DBMS we have contracted to use is known as associative in that

it can support any one or any combination of the three^characteristics . It is

unique among DBMS in that several data bases can be searched in one query, the

15
separate nature of the several bases being "invisible" to the user. This last

characteristic is especially of interest for us because of the usefulness of

searching the Materials and Components Plant Experience Data Base and the

Materials Properties Data Base simultaneously. The two bases will be

searchable through these common elements:

material names (both data bases)

component names (both data bases)

failure mode (plant performance base) and testing behavior (properties

base) — an example here are terms such as corrosion or erosion.

There are two major search patterns which may be followed to retrieve items

in the Data Bases under the control of the DBMS language. It is possible to

search a given data item for a certain sequence of characters which may be

the entire content of the data item or only part. Such sequential searching

is not the fastest way to find data although demonstrations have shown it to

be practical for small amounts of information. It is more efficient to make

certain parts of the data bases directly accessible by setting up indexes of

certain records, that is, by designating data items as "keyed". Search for

the data items is therefore more direct, and more rapid.

The Materials and Components Plant Performance Data Base structure, essentially

unchanged even though the data are now under the control of the new DBMS, is

defined in the new DBMS by the following table, known as a Fields Definition

Table (FDT). The transfer from one DBMS to the other was performed by the

computer vendor.

16
Materials and Components Plant Performance Data Base FDT

Field Name Key Type Stored Length Structure Repeats Notes

INFONO PFX CHR 5 BASE SCALAR

INFONUM UNP 5 SUBF SCALAR 1 to 5(INF0N0)

INCIDENT PFX CHR 5 BASE SCALAR

INCIDNUM UNP 5 SUBF SCALAR 1 to 5(INCIDENT)

DATE PFX CHR 6 BASE SCALAR

DATENUM UNP 6 SUBF SCALAR 1 to 6(DATE)

PROCESS PFX CHR 15 SCALAR

LAB PFX CHR 20 SCALAR

REPORT PFX CHR 10 2

AUTHOR PFX CHR V 30 5

MATERIAL PFX CHR V 30 10

FAILl PFX CHR V 30 SCALAR

FAIL2 PFX CHR V 30 5 COMPl PFX CHR V 30 SCALAR

C0MP2 PFX CHR V 30 4

TEMP UNP 4 SCALAR

PRESSURE UNP 4 SCALAR

ATM PFX CHR 30 3

SUBSYS PFX CHR 30 3

REFER CHR V 305 SCALAR

SUMMARY CHR V 5000 SCALAR

Explanation of terms 1n the above Table :

INFONO = the NBS file number which corresponds to a number assigned to the

original report received

INFONUM = an identifier which makes the INFONO field searchable as a numeric field

INCIDENT = a number assigned to a given plant event within a report (a

report may provide information about several incidents)

INCIDNUM = an identifier which makes the INCIDENT field searchable as a numeric field

DATE = date entered on the report

DATENUM = an identifier which makes the DATE field searchable as a numeric field

PROCESS = name of the plant and/or the process

LAB = origin of the report

REPORT = type of report (example: failure event, failure analysis,

materials evaluation)

AUTHOR = name(s) of writer of the report

MATERIAL = name(s) of the material (s) in the failed component

17
FAIL! = the general cause of failure (example: corrosion)

FAIL2 = the specific cause of failure (example: sulfidation)

COMPl = general terminology regarding the component (example: pumps, valves)

C0MP2 = specific failed part (example: bearings housing, gate)

TEMP = temperature at which the component operated

PRESSURE = pressure at which the component operated

ATM = the environment surrounding the component (example: composition of

gaseous atmosphere)

SUBSYS = the area of the plant in which the component part is situated (example:

gasifier vessel, coal handling)

REFER = the full reference for the report, title, author(s), date, etc.

SUMMARY = abstracted summary version of the report

Data Center staff have participated in two courses, one to familiarize us with the overall computer control system used by the vendor and one which

trained us in the use of the DBMS. It was this latter course, combined with

consultation with the vendor's systems analysts, which permitted Data Center

staff to arrive at the current design for the Materials Properties Data Base.

The current design of the Materials Properties Data Base is dependent on the

multiple data base capability of the DBMS. The Materials Properties Data Base

will actually consist of three data bases, which can be searched separately or

as one base. The ability to cross-link the information in the multiple data

bases permits the setting up of information in such a way that data items

need not be repeated at all or only a minimum number of times. Computer storage

charges are greatly lowered thereby. It is possible to allow for a variable

length field for a data item (such as comments) up to a very large maximum. A

variable number of repeat fields may also be allowed for a data item (such as synonyms), again up to a large maximum. Since the DBMS structure allows for

this assignment of space to data items without payment of storage charges for

unused space there is relative freedom and good flexibility in planning for

data items in the data base. The three data bases of the present design also

carry data items which are identifiers linking the three, simple 8 character

words which provide the search links. These identifiers are keyed items. Small

amounts of data have been tested. The keyboarding procedures have been programmed

for our computer terminals and entering data will be relatively simple. This DBMS

is "user friendly" at the input end of the data effort as well as the search and

output end.

References will be stored in one of the data bases. The data items to be

included in this base are: report or article title, author's names, full

reference, report number, contractor name, contractor address, contract

number, keywords. A definition of the structure of the reference Data Base

is contained in the following Fields Definition Table.

18
REFERENCES DATA BASE FDT

Field Name Kej:. Type Stored Length Structure Repeats Notes

REPTID PFX CHR 8 scalar

CONTRCTR PFX CHR 8 scalar

CONTRNAM

CONTRLOC

DCD

DCD

VV

150

150

scalarv

seal ar'^ decode on CONTRCTR

TITLE CHR V 200 scalar

AUTHORS CHR V 200 seal ar CONTRNUM CHR V 30 scalar

REPTNUM CHR V 20 scalar

REFERENC CHR V 200 scalar

NTISNUM CHR V 30 scalar

KEYWORD CHR 20 V 15

Explanation of terms in the above Table :

REPTID = an internal identification number for the specific reference

CONTRCTR = an abbreviated description for the contractor

CONTRNAM and CONTRLOC = full name and address of the contractor (these items are in a separate file called a Decode file. They can be called up by the

CONTRCTR entry. CONTRCTR is a maximum of 8 characters and is repeated with

each reference, but the full name and address need be entered and stored

only once no matter how many reports belong to the same contractor)

TITLE = title of the report

AUTHORS = all authors named for the report are included

CONTRNUM = the number of the contract supporting the work of the report

REPTNUM = the number of the individual report

REFERENC = the kind of report (i.e., annual, quarterly, etc.), the date and

year, the name of the sponsor, etc.; full identification of the report

NTISNUM = the number by which the report can be obtained from NTIS

KEYWORD = up to 15 different words or phrases can be accommodated in this

field and can be searched

The PFX in the Key column indicates that that is a "keyed" item. The CHR

in the Type column indicates a character field (as opposed to numeric); DCD

in the same field indicates DECODE field items as explained above. A V in

the Stored Length field indicates that the field length is not fixed but

variable and may contain any number of characters up to the stated maximum.

Under the Repeats column, the word scalar indicates that there is no repeat

of that data iteni; V followed by a number indicates that a variable number of

such data items may appear up to the stated maximum.

19
Materials designations will form the second base: material type, material

name, synonyms, composition in terms of constituents and the amounts, preparation,

characteristics , manufacturer, and a comments item for any necessary clarification of any of the above. The Fields Definition Table for this data base follows.

Materials Data Base FDT

Stored

Field Name Key Type Length Structure Repeats Notes

MATLID PFX CHR 8 scalar

REPTID PFX CHR 8 V 500

PROPID PFX CHR 8 V 500

MATLTYP PFX CHR V 70 scalar

MATLNAME PFX CHR V 35 scalar

NAMELIST PFX CHR 35 V 10

COMPSTN CHR 32 Base V 50

CONSTIT PFX CHR 20 Subf V 50 (1-20)

AMOUNT CHR 12 Subf V 50 (21-32)

AMTNUM UNP 6 Subf V 50 (21-26)

AMTUNIT CHR 6 Subf V 50 (27-32)

MATLPREP CHR V 1000 scalar

MATLCHAR CHR V 1000 scalar

MANUFAC CHR V 70 scalar

COMMENTM CHR V 1000 scalar

Explanation of terms in the above Table :

MATLID = an internal identification number for the material

REPTID = an internal identification number for the specific reference

PROPID = an internal identification number for the property or performance item

(Note: MATLID, PROPID and REPTID are the items through which the data bases

are linked)

MATLTYP = material type, i.e., alloy, refractory, etc.

MATLNAME = name of the material

NAMELIST = MATLNAME plus synonyms

COMPSTN = composition of the material. This field is a base field which

consists of the four subfields which follow and which are all individually

searchable. The Notes column indicates which characters within the COMPSTN

field form the individual subfield

CONSTIT = the chemical constituents of the material

AMOUNT = the amount of the constituent in the material

AMTNUM = an identifier which makes the AMOUNT field searchable as a numeric field

AMTUNIT = designation of the units belonging to amount, i.e., weight percent,

mole percent, etc.

20
MATLPREP = the method of preparation and treatment of the material,

thermomechanical history, etc.

MATLCHAR = the characterization of the material

MANUFAC = manufacturer of the material

COMMENTM = any comments concerning any of the above items about the material

The actual properties or test results will be in a third base: material name,

component name, name and units of the property, test conditions, test results

or value(s) of the property; this last actually consists of a large number of

data items to accommodate the complex and varied nature of the data we must

include: a comments item will also be included in this base to allow space

for any necessary clarification. The current design of the properties data

base is outlined in the following table.

Properties Data Base FDT

Field Name Key Type Stored Length Structure Repeats Notes

REPTID PFX CHR 8 V 500

MATE ID PFX CHR 8 V 500

PROPID PFX CHR 8 scalar

MATLNAME PFX CHR V 50 scalar

COMPNAME PFX CHR 30 V 10

PROPNAME PFX CHR V 50 scalar

PROPUNIT CHR V 50 scalar

TESTCOND CHR V 1000 scalar

COMMENTP CHR V 1000 scalar

RSLTTEXT CHR V 1000 scalar

RSLTEQUA CHR V 500 scalar

VARIABLE CHR 30 Base V 6

VARNAME PFX CHR 20 Subf V 6 (1 to 20)

VARUNIT CHR 10 Subf V 6 (21 to 30)

VARDATA CHR 60 Base V 200

VARINUM UNP 10 Subf V 200 (1 to 10)

VAR2NUM UNP 10 Subf V 200 (11 to 20)

VAR3NUM UNP 10 Subf V 200 (21 to 30)

VAR4NUM UNP 10 Subf V 200 (31 to 40)

VAR5NUM UNP 10 Subf V 200 (41 to 50)

VAR6NUM UNP 10 Subf V 200 (51 to 60)

VARIALFA CHR 10 Subf V 200 (1 to 10)

VAR2ALFA CHR 10 Subf V 200 (11 to 20)

VAR3ALFA CHR 10 Subf V 200 (21 to 30)

VAR4ALFA CHR 10 Subf V 200 (31 to 40)

VAR5ALFA CHR 10 Subf V 200 (41 to 50)

VAR6ALFA CHR 10 Subf V 200 (51 to 60)

Explanation of terms in the above Table:

REPTID, MATLID , PROPID and MATLNAME have been defined above

21
COMPNAME = name of the plant component or plant use area for which the material

property was studied

PROPNAME = the name of the property or performance item

PROPUNIT = the units in which the data are reported (Data Base is to be

standardized on SI units)

TESTCOND = the experiemental methods and conditions of the test

COMMENTP = any necessary comments about any of the items in this properties file

RSLTTEXT = any test results which is given verbally, i.e., non-numeric,

qualitative, or descriptive

RSLTEQUA = any test result given in the form of an equation

VARIABLE = a repeating field which lists each test variable (such as temperature, pressure, gas composition, etc.) and their units (maximum

of six variables)

VARNAME = subfield of "variable" containing the name of the variable, e.g.,

temperature

VARUNIT = subfield of "variable" containing units for the variable, e.g., kelvin

VARDATA = numerical data point consisting of up to six values, one for each

parameter listed under variable

4 « VARINUM = numerical value of first variable

VAR6NUM = numerical value of sixth variable

VARIALFA = alternative field in case first variable is non-numeric value

(e.g., if first variable is "gas exposure", value might be "after"

VAR6ALFA = alternative field in case sixth variable is non-numeric value

There is a possibility that the data base may be altered somewhat to provide a fourth, simple base containing only test conditions. The advantage is the

diminished amount of keyboarding and the smaller use of storage space since

this item can be quite lengthy and must be repeated under the present structure.

This alteration is simple at this stage and does not disturb the overall design

of the Materials Properties Data Base.

Although the design of the Data Bases has so far accommodated the small amounts

of test data, only a large scale test can confirm their suitability and permit

permanent stabilization of the designs. It is anticipated that the Reference

and Materials Data Bases will not change but that the Properties Data Base, bein'

the most complicated portion, will have some changes and perhaps additional data

items to be included.

22
Once the designs have stabilized the Data Center staff can focus on the

instructions to be included in a user's Manual for non-NBS users. The queries

required by the DBMS are very close to normal English and the rules are not

difficult to learn. The user language of the DBMS permits selective retrieval

of data and varied designing of report formats. Although some searches may

be performed by using more than one manner of querying to obtain the same

result, the staff will probably standardize only one for the outside user

to simplify the situation. It is possbile to design queries which are sequences of several command statements and to designate these sequences to

be stored for later use. These commands are retrievable by an assigned label.

The designated sequence is called a "macro" and the label is called a "macro

name". These "macros" can be used over and over again when the same queries

are desired to be used. Data Center staff will be able to design macros

for non-NBS users use which will enter the query and produce a tabulated

print out with very little trouble to the user. The user will not be

required to learn about the detailed structure of the Data Bases or the

various methods of searching or how to obtain the various styles of tabulated

presentations of the results. These macros can be written so as to present

the multiple data bases of our system as one base to the user. Although Data

Center staff recognize that there must be a great deal of careful testing of

the system and the instructions to be given in a User's Manual it is not

anticipated that any non-NBS users will experience any great difficulty with

a well-tested system.

23
2. Creep and Related Properties of Refractories (N. J. Tighe, C. L. McDaniel,

S. M. Wiederhorn)

Progress : In order to evaluate the creep test facility capability for

measuring specimen deflection continuously over a 1000 hour test period,

specimens of silicon nitride from a wel 1 -characteri zed billet were tested

in static loading in four-point bend configuration. Three linear variable

differential transformers (LVDT) were mounted on the upper frame of one furnace in a position to contact the upper loading ram. In this position,

we are measuring the difference between the specimen movement and the frame.

This choice was made over an LVDT system in direct contact with a specimen

because of the difficult contact problems and the cost of such a system.

Since the objective of the present program is to carry out screening tests

rather than precision creep experiments, the simple frame to push rod

system appeared justified. We therefore used specimens for the initial

tests for which we had some creep data for comparison.

The tests were run for 1000 hours at 1200 °C using 6 specimens 3 x 4 x 50 mm,

three specimens were in the furnace with the LVDTs and three were in another

furnace. The LVDTs were monitored continuously with multiple point recorders.

We used the long test period to evaluate several recorders and, based on their performance, purchased a 12 point sequential recorder that was most

satisfactory. This recorder should be delivered in late July. On the basis

of the performance of the 3 LVDTs, we completed the purchase of the required

12 for the system and they will be ready in late July.

The outer fiber strain curve drawn from the deflections measured for the

silicon nitride specimens is shown in Fig. 1. The data points were taken

from the continuous recording at 1 hour intervals for the first 24 hours

and at 24 hour intervals for the next 41 days. The deflections were similar

for all of the specimens and the plots showed three regions of different

deflection rate or creep as indicated on the diagram. The rate calculated

for the two regions of constant creep are: Region II 6.9 x 10“°/second,

and Region III 2.3 x 10"°/second,

Additional thermal cycling tests were carried out on the fused cast

a+6 alumina (Monofrax A) reduced, cross-section specimens tested in

compression. We had planned to run for 1000 hours with cycling every 1/2 hour

between 1400 ”C and 1200 °C, However, the tests were terminated after one week because of a water-clog problem. During these tests we recorded the

LVDTs and found that they cycled over 'a., 05 cm because of thermal expansion

changes in the load train. A correction for the LVDT readings must be

considered in the analysis of thermal cycling in our system. The cycles were symmetrical throughout the test interval and the end points could be

averaged for a total deflection reading. In preparation for carrying out

four-point bend tests on the alumina-type refractories we have had new fixtures made from the same recrystal 1 i zed alumina material used for rams.

24
Plans : During the next quarter we will carry out static fatigue tests on the

silicon carbide discussed in the previous report. Tests will be run for

1000 hours at 1200 °C and 1300 °C. Specimens of Monofrax A will be cut and

tested in the four-point bend configuration in order to compare the material

properties in this mixed mode with the simple compression results.

Because of the recent change in emphasis from refractories for MHD air

preheaters to refractories for more general coal derived fuel applications

such as heat exchangers and vessel liners for gasifiers and liquefaction

systems, we are including some of these materials in our screening program.

The following materials are of interest for structural refractories in fossil

energy generating systems for insulating liners, structural supports, and heat

exchanger tubing. For some of the materials there is data on coal slag

corrosion resistance but there is very little data on the strength or creep

resistance of the materials under the types of stresses they would be exposed

to for periods of thousands of hours. Some ranking of the materials with

respect to creep resistance in air at temperatures up to 1600 °C for periods

of up to 1000 hr. will be required for future design purposes. We plan to

include some of these materials in our testing program.

Oxide ceramics, fused cast :

a-alumina: a+3Al202, 92-95% aAl202 and 5-8% 6(Na20*llAl202) (Monofrax A)

6-alumina, AI

2

O

2

(Na 20 *llAl 202 )

Magnesia-spinel, (Mg0*Al202) + MgO

Chrome-sp’inel , 80% (MgCr) 0^ + 15% (Or, Fe, A1 ) 0^ ss

Chrome-alumina, 60-65%, (Cr, Fe, A1 ) 0^ ss + 35-40% (Mg, Cr) 0^

Zirconia-alumina, ^.11% Zr02» '^47% Al20^, ^11% Si02

Oxide ceramics, sintered :

Alumina, 85-98% AI

2

O

2

Silicon oxy-nitride Si2N20

Non-oxide ceramics :

Silicon carbide, SiC-sintered a, hot-pressed, sintered a+6

Silicon carbide bonded with silicon nitride

Silicon nitride, Si^N^-reaction-sintered, hot-pressed, sintered.

25
TIME, hr

Figure 1. Plot of the outer fiber strain calculated from the deflection

measured during 1000 hours at 1200 with a load of 250 MPa

for hot-pressed silicon nitride (NO 132).

26