Rational Bureau of Standards

Library, E-01 Admin. Bldg. MAY 14 1971

Reference book not to be

taken from the Horary.

NBS SPECIAL PUBLICATION 333

Research Materials

Developed Under the

NBS Inorganic

Materials Program
NBS TECHNICAL PUBLICATIONS

PERIODICALS JOURNAL OF RESEARCH reports National Bureau of Standards research and development in physics, mathematics, chemistry, and engineering. Comprehensive scientific papers give complete details of the work, including laboratory data, experimental

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Superintendent of Documents

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UNITED STATES DEPARTMENT OF COMMERCE • Maurice H. Stans, Secretary NATIONAL BUREAU OF STANDARDS • Lewis M. Branscomb, Director

Research Materials Developed Under the

NBS Inorganic Materials Program

Edited by F. E. Brinckman and J. B. Wachtman, Jr.

Inorganic Materials Division

Institute for Materials Research

National Bureau of Standards Washington, D.C. 20234

U- St National Bureau of Standards. Special Publication 333,

' "Nat. Bur. Stand. (U.S.), Spec. Publ. 333, 71 pages (September 1970) CODEN: XNBSA

Issued September 1970

For sale by the Superintendent of Documents. U.S. Government Printing Office. Washington, D.C. 20402 (Order by SD Catalog No. C 13.10:333), Price 70 cents,
NATIONAL BUREAU QF STAND/ MAY 1 7 497t ,fp

Library of Congress Catalog Card Number: 70-608227
Contents

Page

1. Introduction V

2. Definition of Research Materials V

2.1. General Definition V

2.2. Differences in Degree of Characterization Needed for Research on Properties With Varying Degrees of Structure Sensitivity VI

2.3. Inhomogeneity VI

2.4. Metastable Materials VI

3. Relation to Standard Reference Materials VI

4. Organization of the Tables VI

4.1. Rationale VI

4.2. Use of Tables—Key VII

5. References VII Tables

I. Gases 1

II. Liquids : 7

III. Glasses 16

IV. Single Crystals 20

V. Polycrystals 41

VI. Multiphase Systems 61

in

Research Materials Developed Under the

NBS Inorganic Materials Program

F. E. Brinckman and J. B. Wachtman, Jr.

The National Bureau of Standards develops many specialized materials in the process of carrying out research supporting its measurements, standards, and service activities. These materials include gases, liquids, glasses, single crystals, polycrystals, and various multiphase materials;

their compositions (including trace elements in some cases) and physical characteristics are

tailored to specific research needs, but the materials are often of use for other research purposes. Production is usually limited to immediate internal needs and samples are not generally

available for distribution, but knowledge of production techniques and materials characteristics which may be helpful to other scientists is available. The present listing of research materials developed in the Inorganic Materials Division accordingly gives names of scientific staff members who may be contacted for this type of information as well as giving a brief summary of the

nature, method of preparation and properties determined for each material. Key words: Chemical properties; composition; gases; glasses; liquids; multiphase materials; physical properties; polycrystals; preparation; research.

1. Introduction

Improved materials are critically needed in many

areas of technology. Attempts to provide such superior

materials are frequently -empirical and sometimes

wasteful of time and funds [l].1 An empirical component will probably always be present in any materials development program, but the establishment of

a science of materials that increasingly affords predictable and reliable results in devising new materials

for specific tasks is most desirable. Not only will this increase the efficiency of materials development pro- grams, but also can ultimately lead to development of completely new materials or new applications. Much

thought has been given to opportunities arising from

recent developments in materials science [2] and to roadblocks preventing engineering achievement of

scientifically feasible materials including the areas of

characterization [1] and processing [3]. Advances

in materials science assist materials development on

the one hand, but depend upon development of materials suitable for research on the other. This inter- dependence of materials development and materials

science is widely recognized and new programs on

the properties of materials increasingly have as a major component a research material development

subprogram. The experimental and theoretical competence needed to produce and characterize specimens

is frequently quite different from that needed for the subsequent property study so that the decision to undertake a property study on a new material fre- quently means that a large investment of time and

resources, perhaps comparable to the property measuring effort itself, must be made before the property

study can begin. In these circumstances the availability of a few trial specimens, even if not of completely satisfactory quality for the final study, can

be very valuable in permitting a test of the experi- mental feasibility of the contemplated measurements

and perhaps in providing guidance on how closely the character of the specimen must be controlled for

the final study. When trial specimens are not available, knowledge of previous preparation techniques and of the nature and quality of specimens which have

1 Fiprures in brackets indicate the literature references on pase 3.

been produced successfully is usually quite valuable

in planning and carrying out the sample preparation

aspect of a new research program. The present list- ing of research materials produced in the Inorganic

Materials Division is offered as a means of promoting

direct scientist-to-scientist exchange of information on

production and characterization of materials for which

the division has some special competence. In some

cases, specimens may be on hand and available on

request; in other cases, facilities and staff may be

available to produce additional specimens for pur- poses coming within the NBS mission. Provision of information, rather than specimens, is the principal

goal, however, because maintenance of a stock of the numerous and extremely varied materials produced in small batches or maintenance of specialized production

facilities on a standby basis is not feasible. Information concerning nationwide sources of many

research materials, especially single crystals, is avail- able from the Oak Ridge Research Materials Information Center [4]. The present listing of materials may be useful to

scientists and engineers interested in the production

of a material or its general availability for purposes

other than research. No claim is made concerning

exhaustive knowledge of the materials listed, but the

staff members involved in the production or characterization of unusual materials sometimes have special knowledge relevant to other applications in addition

to research.

2. Definition of Research Materials

2.1. General Definition A research material is here considered to be one

sufficiently well-characterized to be useful for a particular type of current research. Ideally, a fully characterized material is desirable; that is, the character (chemical composition, structure, microstructure,

etc.) should be uniform and held within such narrow

and known limits that all the chemical and physical

properties of the material are well determined. Practical considerations usually limit the characterization to v
the factors thought to control the property being

studied and limit the accuracy of the characterization. Thus, a material useful at a particular stage of re- search may no longer be useful for the same type of research as measurement techniques improve and

finer details of behavior are studied or as new factors are discovered to have an influence on properties at the level being studied. A valid research material can cease to have this distinction as a field of study

progresses but the same material can sometimes again become an important research material as new phe- nomena are investigated. For example, ruby grown

by the Verneuil process for bearings, wear surfaces, or jewels suddenly became an exciting research material when the ruby laser was invented.

2.2. Differences in Degree of Characterization Needed for Research on Properties with Varying Degrees of Structure Sensitivity. The characterization needed for certain research, such as phase equilibria, is sometimes limited pri- marily to the major element composition and such

factors as trace impurities or surface condition are

relatively unimportant. This fact is reflected in the

listing, for example, of a number of crystalline materials developed for phase equilibria studies and a number of glasses developed for bulk optical or

elasticity studies; major component characterization was sufficient for these purposes. Some of these materials have subsequently become the object of re- newed research interest in connection with other

properties dependent primarily upon major component composition such as electro-optic properties,

photoelasticity. and mechanical properties under pressure. Certain structure-sensitive properties, such as

transport, plastic deformation, and fracture depend upon trace impurities and upon small deviations from stoichiometry. Samples made for research in these areas, even though of the same major component

composition as some of those mentioned previously, require more careful processing and characterization and are accordingly listed as separate entries with an indication of their special features.

2.3. Inhomogeneity

Among both the bulk composition and trace impurity types there are cases where a deliberate degree

of inhomogeneity is required. Thus, a series of

glasses with the same total composition but differing degrees of phase separation forms an interesting family of research materials. An example of an even

finer scale of deliberately produced inhomogeneity is a

series of crystals of CaF_. all having the same level of Gd additive but differing in the degree of association of point defects with Gd atoms. This last example

illustrates another feature of some of the listed materials; in this case specimens of given bulk composition were produced bv a commercial supplier to NBS

specifications. The NBS contribution was the develop- ment of special treatments and measurement techniques needed to produce and determine different degrees of association.

2.4. Metastable Materials

Still another category of research materials in- volves those which are not stable or have a very short

lifetime under ordinary conditions but which occur

as important components under special conditions such as high temperature vapor species, high pressure

crystalline phases, or short-lived reactive inter- mediates. Such materials generally cannot be kept in stock but the technology of preparation and the tech- niques for measurement of concentration and properties during the brief lifetime of the material are important aspects of research material information. An

overlapping family of research materials consists of

those which are dangerous (toxic, explosive, or cor- rosive) and so require special handling procedures during processing, storage, or property measurement. An example of such a difficult research material is the high pressure polymorph of the detonator ex- plosive lead azide.

3. Relation to Standard Reference

Materials A few of the research materials listed here have

been developed into Standard Reference Materials and many of the Standard Reference Materials are used as research materials but the two categories should not be confused despite the fact that there is some overlap. Standard Reference Materials are kept

in stock by the National Bureau of Standards and

sold by the Office of Standard Reference Materials. Each Standard Reference Material is certified with

respect to the aspects of chemical and/or physical

properties relevant to the material's intended application. Perhaps the greatest use of these materials is for calibration of instruments and checking of measurement procedures, but the high degree of homogeneity and extensive characterization associated with Standard Reference Materials frequently makes them

useful as research materials. A full listing of Stan- dard Reference Materials is available [5].

4. Organization of the Tables

4.1. Rationale

As noted in the Introduction, entries have been

tabulated into sections derived chiefly from gross

physical state at ordinary conditions (e.g., gases, polycrystals, multiphases. etc.). Clearly a number of exceptions occur, particularly for research materials

of low stability or transient existence, but their loca- tion will be fairly obvious to the reader. Since this compilation tends to emphasize composition rather than properties, special care was taken

in organizing the tables. Use of the widely accepted Chemical Abstracts Formula Index does not always

generate familiar empirical chemical formulae, nor

VI
does this system readily lend itself to classification of

glasses, but we chose it for its rational basis. Moreover, significant progress has been achieved for computer searching and retrieval; indeed, the parent pro- gram is now in use by the Patent Office.

4.2. Use of Tables—Key

a. The arrangement of symbols in formulae is alphabetic except that in carbon compounds C always comes first followed immediately by H if hydrogen

is also present.

b. The arrangement of formulae or entries is also alphabetic, except that the number of atoms of any

specific kind influences the order of listing; e.g., all Ci compounds appear before C2 , thus CC1 2 0, CCl4 , CHCL, CHN, CH2 0, CO, C2 Ca, C2H4 02

. c. Water of hydration is not made a part of the formulae indexed.

d. Polymers having different names and recog- nized as different substances, e.g., acetaldehyde and

paraldehyde, are all entered under their accepted formulae; but a definite compound for which differ- ent polymeric formulae are in use is entered under

the simplest formula.

e. For series of compounds listed under a single entry heading "M" refers to metallic or metalloidal components (e.g., K, Li, Rb) and "X" denotes elec- tronegative substituents such as Cl, F, 0, S, etc.

f. Approximate compositions are indicated by en- closing listing in quotation marks, "—", such as in

interstitial compounds or alloys.

g. Glasses, polyphases, and compounds of given

stoichiometry but indefinite structure are cited alphabetically by M, followed by X; thus B03 -3Nb2 05 ; Cr2 0:; -Ir02 ; B2 0,-Ba0-Si02 ; etc. h. Isotopic compositions are presumed to be of ter- restrial abundance unless otherwise indicated.

i. Wherever practicable conventional formulae and/or nomenclature is listed to the right of the index formula.

j. Great effort has been made to maintain accuracy and provide current information. In some instances, through staff changes, some authors cited are no

longer in the Inorganic Materials Division, yet inclu- sion of their recent efforts was deemed significant to

this compendium. Hence, these individuals are signified by an asterisk. The reader may contact these individuals for further information, but it would

probably be more expedient if the editors were

contacted. Many of the materials listed in this report were produced as part of programs sponsored by other

agencies. Acknowledgements for specific materials

are given in the references and are too numerous to repeat in detail here. The support by the Air Force

Materials Laboratory, the Air Force Cambridge Research Laboratory, the Army Research Office (Dur- ham), the Advanced Projects Research Agency (Materials Office), the Atomic Energy Commission (Re- search Division), the National Aeronautics and Space

Administration, and the Office of Naval Research

is 'gratefully acknowledged.

5. References

[1] Characterization of Materials, prepared by the Committee

on Characterization of Materials of the Materials Advisory Board, H. W. Leverenz, Committee Chairman.

National Academy of Sciences—National Academy of Engineering Publication MAB-229-M, March 1967. [2] Research in Solid-State Sciences—Opportunities and Rele- vance to National Needs, prepared by a Committee of the Solid State Sciences Panel for the Coordinating Committee for Materials Research and Development of the Office of Science and Technology, R. Smoluchowski, Committee Chairman, Publication 1600, National Acad- emy of Sciences, 1968.

[3] Ceramic Processing, prepared by the Committee on Ce- ramic Processing, of the Materials Advisory Board, Joseph A. Pask, Committee Chairman, Publication 1576, National Academy of Sciences, 1968. [4] J. W. Cleland, Purity and Perfection of Research Speci- mens of Oxides in Mass Transport in Oxides, Nat. Bur.

Stand. (U.S.), Spec. Pub. 296, (224 pages) edited by

J. B Wachtman, Jr. and A. D. Franklin, issued August

1968. The address of the Research Materials Information Center is Building 3001, Oak Ridge National

Laboratory, Box X, Oak Ridge, Tennessee 37830.

[5] Catalog of Standard Materials, Nat. Bur. Stand. (U.S.), Spec. Publ. 260, July 1970. See also supplements for price lists and changes.

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