. Is, NBS

Infrared Reflectances of Metals at

Cryogenic Temperatures- A Compilation

From the Literature

348

P. F. DICKSON AND M. C. JONES

*z

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U.S. DEPARTMENT OF COMMERCE

National Bureau of Standards
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NBS TECHNICAL NOTE 348

ISSUED OCTOBER 14, 1966

INFRARED REFLECTANCES OF METALS AT CRYOGENIC

TEMPERATURES-A COMPILATION FROM THE LITERATURE

P. F. DICKSON AND M. C. JONES

Cryogenics Division

Institute for Materials Research

National Bureau of Standards

Boulder, Colorado

NBS Technical Notes are designed to supplement the Bureau's regular publications program. They provide a means for making available scientific data that are of transient or limited interest. Technical Notes may be

listed or referred to in the open literature.

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, D.C., 20402

Price: 40 cents.

CONTENTS

ABSTRACT ...... 1. INTRODUCTION .....

2. SPECTRAL REFLECTANCE

2. 1 Aluminum

Table 2. 1 Spectral

.....

Reflectance of Aluminum

Figure 2. 1 Spectral Reflectance of Aluminum

2. 2 AntimonyTable 2. 2 Spectral Reflectance of AntimonyFigure 2. 2 Spectral Reflectance of Antimony

2. 3 Bismuth and Bismuth-Tellurium Alloys

Table 2. 3 Spectral Reflectance of Bismuth

and Bismuth-Tellurium Alloys

Figure 2. 3 Spectral Reflectance of Bismuth

and Bismuth-Tellurium Alloys

2. 4

Table

Copper

2.4

.....

Figure 2. 4

2. 5 Gold

Table 2. 5

Figure 2. 5

2. 6 Lead

Table 2. 6 Spectral

....

Reflectance of Lead

Figure 2. 6 Spectral Reflectance of Lead

2. 7 Nickel

Table 2.7 Spectral Reflectance of Nickel

Figure 2. 7 Spectral Reflectance of Nickel

2. 8 Silver

Table 2. 8 Spectral

.....

Reflectance of Silver

Figure 2. 8 Spectral Reflectance of Silver

2. 9 Sodium

Table 2.9 Spectral

.....

Reflectance of Sodium

Figure 2. 9 Spectral Reflectance of Sodium

2. 10 Tin

Table 2. 10 Spectral

.....

Reflectance of Tin

Figure 2. lOSpectral Reflectance of Tin

2.11

Figure

Brass

2. 11

.....

Spectral Reflectance of a-Brasses

Spectral Reflectance of Copper

Spectral Reflectance of Copper

Spectral Reflectance of Gold

Spectral Reflectance of Gold

PAGE

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27

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30

31

32

33

34

35

36

37

iii
TOTAL REFLECTANCE

Table 3. 1 Total Reflectance of Aluminum

Table 3. 2 Total Reflectance of Copper

Table 3. 3 Total Reflectance of Gold .. Table 3.4 Total Reflectance of Lead . Table 3. 5 Total Reflectance of Nickel and Nickel

Table 3. 6

Alloys

Total Reflectance

....

of Silver

Table 3.7 Total Reflectance of Steel and Various

Stainless Steels

Table 3.8 Total Reflectance of Tin

Table 3.9 Total Reflectance of Various Brasses

Table 3.10 Total Reflectance of Various Metals

and Alloys ....

REFERENCES .....

38

39

41

43

44

45

47

48

51

52

53

58

IV
INFRARED REFLECTANCES OF METALS AT CRYOGENIC

TEMPERATURES --A COMPILATION FROM THE LITERATURE

P. F. Dickson and M. C. Jones

Spectral and total reflectances for metals at cryogenic

temperatures in the infrared wavelength region are compiled

from the literature. Information concerning sample preparation and purity, radiation source, and methods of reflectance

measurement are also presented. Observations regarding the

effects on reflectance of temperature, oxide layer, wavelength,

and sample preparation are given . Key Words: Compilation, cryogenic, infrared, metals,

reflectance.

1. Introduction

Calculation of radiative heat transfer at cryogenic temperatures

requires a knowledge of thermal radiative properties of materials at

these temperatures. From the nature of thermal radiative processes at

low temperatures it is evident that one needs data in the infrared, and in

particular in the far infrared. This can be seen from Wien's displacement law for a black body (X T = 2898 p,°K). The wavelength of

XXXcuC maximum emitted radiative energy shifts from \ s 9. 8 p, at room temperature (T s 2959 K) to X ^ 725 p, at 4°K. This survey comprises information, summarized here in graphical and tabular form, currently

available in the infrared wavelength region (through mid- 1966) on thermal radiative properties of metals, in particular, reflectances, at

cryogenic temperatures.

The survey was undertaken as a preliminary to an experimental

program. As will be evident, very little work has been done in the far
infrared, the only reported measurements beyond 14 p, being those of

Aronson, et al. [ 1964] on stainless steel, an aluminum alloy, a magnesium alloy, and chromium. The ±5% error quoted by these authors

serves to underline the difficulty of making reflectance measurements on

highly reflecting materials in the far infrared by conventional spectrophotometric techniques.

Theoretical considerations and experimental techniques in determining optical constants of metals were reviewed by Givens [ 1958] and

Ehrenreich [ 1965] , and a review of the subject at low temperatures was

given by Corruccini [ 1962] . Previous surveys on total emissivity data

at low temperature have been given by Fulk and Reynolds [ 1957a] and

Corruccini [ 1957].

Since the surveys of Fulk and Corruccini were published (containing no spectral data at low temperatures) several spectral studies

have appeared in the literature. Along with this aspect there has also

been an apparent realization by the same workers that the older data in

the literature are of little more than qualitative interest due to their

ir reproducibility; the reflectance of a metallic surface depends strongly

on the method by which it was prepared. Much effort has gone into producing surfaces of high purity with no work-hardened surface layer

present. This has culminated in the highly reproducible pure metallic

surfaces produced by ultra-high -vacuum vapor deposition (~ 10 mmHg)

by Bennett at the Michelson Laboratory. The room temperature reflectances of these surfaces are higher than what had previously been

achieved. They are discussed and used below as a comparison with the

work of other authors to illustrate the effects of both temperature and

surface preparation. Such was the improvement in room temperature

reflectances obtained by the use of ultra -high-vacuum vapor deposition

that one can only regret, as yet, no similar measurements have been
reported at low temperature and longer wavelength where even higher

reflectances are to be expected. Rate of deposition also has an effect

on reflectance as indicated by Bennett, Silver, and Ashley [ 1963], with

greater reflectance values obtained for increased deposition rates.

In view of this later work it has seemed desirable to present the

results of this compilation in two sections. Section 2 consists of all

spectral data reported and contains only one work published before 1959.

Section 3 contains total reflectance data and is mostly older data, some

of which were reviewed previously by Fulk and by Corruccini. However,

original references are given where known. The word "total, " as here

applied to reflectance, means the value obtained by integration over all

wavelengths. It should be remembered that this value is dependent on

the wavelength distribution of incident flux.

The total or spectral reflectance (p or p ) of a surface may be

t A. obtained by a number of direct experimental techniques. It may also be

obtained indirectly for an opaque surface from a measurement of the

absorptance {a or a), for then p = 1 - a. A second indirect method is

t A. to calculate the normal reflectance (p^ ) from measurements of the

A., refractive index n and the absorption coefficient k by use of the Fresnel

A. A

formula

P K - 1 > 2 + k

x

2

\0 , ,,2,2 („ x+

l) +k

x

Measurements of the total or spectral emittance (e or e ) have also

t A

been used in the past by invoking Kirchoff's law: a, = e and or. = e. . t t A A

Recently, however, a theoretical question has arisen as to the general

applicability of Kirchoff's law [ Ashby and Schocken, 1964] , and this
seems to be particularly important at long wavelengths and low temperatures.

In the tables and graphs which follow, reflectances are reported

as such when they are either from direct measurements or derived from

measurements of ex or n and k; reflectances are not derived from emittance measurements. Reflectances are normal (p ) unless otherwise

stated. It may be noted that in the limit of zero absorptance the ratio of

hemispherical to normal absorptance approaches the value 4/3 for metals

[Jakob, 1949].

The methods by which data were obtained are indicated in the

tables below by the following general classification:

Method 1. Direct measurement of normal reflectance by

multiple reflection techniques.

Method 2. Direct measurement of normal reflectance or absorptance by calorimetric techniques.

Method 3. Calculation, by either the original authors or

the present authors, of normal reflectance from

optical constants n and k determined by:

(a) measurements of absorptance at oblique

incidence for two polarization components (perpendicular and parallel to the plane of incidence)

by a calorimetric technique, or

(b) measurement of the phase shift and relative

magnitudes of the perpendicular and parallel

components of a reflected beam at oblique incidence.

Method 4. Measurement of absorptance or emittance by rate

of boil-off of a cryogenic liquid. This method

gives total hemispherical values.
Method 5. Direct measurement of normal emittance bycomparison of emitted radiation with that emitted

by a black body at the same temperature.

These general experimental techniques are referred to in the

tables, and any variations, when applicable, are noted.

Information as to type of radiation source (e. g. , monochromatic,

wavelength band, total radiation from a source at a given temperature)

accompanies the data. Techniques of surface preparation are also given.

The temperature region of primary interest was that below 100° K;

therefore, only those metals for which data were available in this region

are presented. However, for comparison and completeness, selected

data on these materials at room temperature are also given if available.

Theory predicts that the reflectance of a metal in the infrared

region will increase with decreasing temperature and increasing wavelength. Also, surface preparation is known to have a significant effect

on reflectance values obtained. Results of this survey indicate that

reflectance increases for preparation techniques in the following order:

mechanical polishing, high vacuum vapor deposition, electropolishing,

and ultra-high -vacuum deposition. Oxidation or impurities on the surface layer generally decrease reflectance, but the effect seems much

smaller for oxidation than previoasly believed. Alloys have lower

reflectances than pure metals. Although data available on any metal

listed are not complete enough for a quantitative check, reflectances

given tend to follow the aforementioned expectations.
2. Spectral Reflectance

Of particular current interest are data on reflectance as a function of wavelength (spectral reflectance, p,). Effects on reflectance of

surface preparation, temperature, and alloy composition may also be

observed in the graphs and tables which follow. Results show that, to

obtain reproducible results, care must be taken to define surface preparation as well as other experimental techniques.

2 . 1 Aluminum

Variation of normal spectral reflectance (p^ ) with temperature,

A,

deposition vacuum, and wavelength is well illustrated for aluminum in

figure 2. 1. As is seen, reflectance of ultra-high vacuum (~10 mm Hg)

evaporated films [Bennett, et al. 1963] is significantly higher than those

values obtained using the usual high vacuum (~10 mm Hg) techniques.

Room temperature reflectances of high- vacuum deposited films calculated from the optical constants of Golovashkin, et al. [I960] and measured directly by Bennet, et al. [1962] show excellent agreement.

Bennett, et al. [1962] state that, contrary to popular belief, the

oxide layer formed on aluminum has almost no effect on the infrared

reflectance. Calculations on oxide layers from 10 to 100 A thick show

the change in reflectance to be less than 0. 1% for X > 1. 5 (i. A 22 Athick film is reported formed after several weeks' exposure.
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13
2. 4 Copper

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at

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to

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999$

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1.000

0.996

0.992

0.988

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0.980

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D

0.972

T = 90°K

T = 300°K

Figure 2.4 Spectral reflectance of copper

Roberts A T = 4.2°K Biondi (1956) |

|T<100°K

(I960)

V T = 82°K .f-Shklyarevskii

Padalka and

O T = 295°K y(1962) IHT = 100°K

Rayne (1959)

Frequencyband:

X - 1. 8 to 4gt

17
2. 5 Gold

In view of the high reflectance values of gold obtained in the

infrared at room temperature by Bennett and Ashley [ 1965] using ultrahigh-vacuum deposition, it would be interesting to make these measurements at cryogenic temperatures using the same sample preparation

technique. Such a result would be extremely useful in view of the potential use of gold as a standard of reflectance and in view of the wide application of gold plating in dewar construction.

18
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19
1.000

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ft.o

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A

O

4 8 12

Figure 2. 5 Spectral reflectance of gold

T = room temperature (10~9 mm Hg deposited) Bennett and Ashley (1965)

T= 8 2° TC ~1 - ^ T - 295° K M*° mm HS deposited) Padalka and Shklyarevskii (1961)

20
2. 6 Lead

Measurements of optical constants of lead made by Golovashkin

[ 1965] immediately after deposition and after several days in vacuum

gave identical results. No effect of oxidation on results was found after

one day in air; although, after several days in air, noticeable changes

in optical constants (of unstated magnitude) were observed by the original author.

21
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22
.000

0.960

0.920

x.o

0.880

0.840

0.800

0.760

Figure 2. 6 Spectral reflectance of lead

O T = 4°K >> A T= 78°K iGolovashkin (1965)

T = 293°K J

23
w

fnO

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U

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24
.000

0.900

0.800

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0.700

0.600

0.500

0.400

Figure 2. 7 Spectral reflectance of nickel

O T = 88°K

A T = 298°K

Roberts (1959)

25
2. 8 Silver

Ultra-high-vacuum deposited silver is seen in figure 2. 8 to have

a reflectance significantly higher than that of a film deposited using the

usual high-vacuum techniques. It is noteworthy that Biondi's results for

electropolished samples at 4. 2°K show even higher reflectance than

ultra -high-vacuum room temperature values. As in the case of gold,

the reflectance at cryogenic temperatures of ultra-high -vacuum deposited

silver would be an extremely useful result.

26
w

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Shklyarevskii

[1961] Biondi [1956]

O

(1) 2

3

cq

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so

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u

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S

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at

10

mm

of

Hg.

Purity

>

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to

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o

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9956

(limiting

value

A.,

for

X>

1.5

u.)

(T

=

4.

2°K)(See

figure

2.8)

o o* o o © o o o o o o

i

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27
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^ o o o o O O O O O i-H i-H p-l n fo ^ in ^o

28
1.000

0.996

0.976

0.972

Figure 2. 8 Spectral reflectance of silver

A T = 4. 2°K Biondi(1956) D T = 82°K 1 Padalka and

T = room temp Bennett and Ashley ( 1965) <> T = 29 5° K J Shklyarevskii [ 1961

29
2. 9 Sodium

At the time this publication went to press, additional work of

Mayer and Hietel [ 1966] on the alkali metals, potassium and cesium,

became available. Wavelength range investigated was essentially that

here reported for sodium. For details, consult the original reference,

30
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31
.000

0.980

0.960

^X,0

0.940

0.920

0.900

0.880

2.5

Figure 2.9 Spectral reflectance of sodium

A T = 90°K > O T = 195°K I Hiotel (1965)

D T = 293°K J

32
2. 10 Tin

Optical constants of tin were measured by Golovashkin and

Motulevich [1965] immediately after vapor deposition and after one day

in vacuum with identical results. After a 48-hour exposure to atmosphere, the change in n was 2 to 3% and k < 1%. This variation in optical

constants affected the reflectance by less than 0. 002% for X >5p, (present

authors' calculation).

33
I—

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m 2 a

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cd bi

ffi o •H B

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(1) 1 o

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1

34
.000

0.960

0.920

^o

0.880

0.840

0.800

0.760

Figure 2. 10 Spectral reflectance of tin

A T = 4. 2°K -s O T= 78°K ^Golovashkin and Motulrvich (1965)

D T = 293°K J

35
2. 11 Brass

Results of spectral reflectance measurements on various electropolished or-br asses at 4. 2°K by Biondi and Rayne [ 1959] using Method 2

are presented in figure 2. 11 compared with pure copper.

36
o

.1-1 No

CO

0)

03

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0)uu

I—

<4-l <u

1—1uo

<1> en

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a pi • iH -1-1 SI N

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37
3. Total Reflectance

Until recently, nearly all the reflectance data reported in the

literature were total normal reflectance (p ) or total hemispherical

reflectance (p ). For this reason, many of the results below have been

presented in previous surveys but are given here for completeness.

Results of Betz, Olson, Schurin, and Morris [ 1958] are for total normal

emittance (e ) and are reported as such.

1 1 \J

38
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4. References

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