Hydrogen evolution at 600 deg and 5 x 10 to the 7th power - 10 to the 6th power torr from AVOOO Al samples, which were pickled in 10 percent NaOH, is discussed. An H evolution kinetic equation is derived for samples of equal vol. and different surfaces (5 and 20 sq cm). The values of the H evolution coefficient K indicated an agreement with considered H diffusion mechanism through an oxide layer. The activation energy for the H evolution process, obtained from the K-temp. relation, was 13,000 2000 cal/g-atom

Andreyev, L. A.

Gelman, B. G.

Polosina, Y. Y.

Zhukhovitskiy, A. A.

English

NASA Technical Reports Server

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3 1176 00129 0882 
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NASA TECHNICAL MEMORANDUM 
THE HYDROGENATION OF METALS UPON 
INTERACTION WITH WATER 
NASA TM-75362 
L.A. Andreev , B.G. Gel lman , A . A . Zhukovitskii, 
E.E. Polis ina 
NASA-TM-75362 19790007953 
A translation of "Navodorozhivanie Metallov 
pri Vzairnodeistvii s Vodoi ," Izvestiya Vysshikh 
Uchebnykh Zavedenii : Chernaya Metallurgiya , (1), 18-21 (1972) 
JAN 1 C ,') 
LANGLEY !?:SE,IR:H CC:ilTER 
L'BR';r. (, "',AS" 
HA,\IPTO,", VIHGINIA 
NATIONAL AERONAUTICS AND SPACE ADMINISTRATI ON 
WASHINGTON , D.C. 20546 JANUARY 1979 
J 
https://ntrs.nasa.gov/search.jsp?R=19790007953 2020-03-22T01:26:09+00:00Z
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STANDARD TITLE PAG E 
I . Repo rt No. 12. Government Accession No . 3. Recip ient ' , Cotolog N<> . 
NASA TM- 75362 
4 . T i tle ond Subtitle 5. Repo rt Dote 
HYDROGEN ABSORPTION OF METALS DURING January , 1979 
THEIR INTERACTION WITH WATER 6 . Performing Drgan i zot ian Code 
7. Au thar( s) 8 . Perform ing Organ i zation Repor t No . 
Andreev, L. A. ; Gelman , B . G. , et al 10 . Work Unit No . 
II. Contract or Grant No . 
9 . Perfo rmi ng Organ i zat ion Nome and Addre .. 
Leo Kanner Associates 13. Type 01 Report and Per iod Covered 
Redwood City, California 94063 Translation 
12. Sponsoring Agency Name and Addre .. 
National Aeronautics and Space Admin . 
Wa.shington , D.C . 20546 14 . Sponsoring Age ncy Cod. 
15 . Supplementary Notes 
Hydrogen Absorption of Metlas During Their Interaction with 
Water. Andreev, L . A. ; Gelman , B. G., et al. Investiya , 
Vy ss hikh Uchebnykh Zavedeniy , Chernaya Metallurgiya I 
vol. 1 , 1972, pp . 18- 21 
16. Abstract 
107- 106torr. H evolution at 600 0 and 5 x from AVOOO Al 
samples, which were pickled in 1 0% NaOH , is dicussed . A H 
evolution kinetic equation is deri~ed for samples of equal vo 
and different surfaces (5 and20 cm ). The values of the H , 
evolution coeff . K indicated an agreement with considered H 
diffusion mechanism through an oxide layer. Teh activation 
energy for the H evolution process , obtained from the K- temp . 
relation, was 13,000 2000cal/g- atom 
17 . Ke y Word, (Selec ted by AuthOr(s») 18 . DiSlr ibut ion Statement 
Unclassified- Unlimited 
19. Secu ri ty Clau i!. (of this report) 20. Secu ri ty Clossil. (01 this page) 21. No. 01 Pages 22. Pr ice 
Unclassified Unclassified 
I 
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/ . 
I 
THE HYDROGENATION OF METALS UPON 
INTERACTION WITH WATER 
L.A. Andreev, B.G. Gel'man, A.A. Zhukovitskii, 
E.E. Polisina 
(Moscow Institute of Steel and Alloys) 
Gas Emission during Vacuum Extraction 
from Etched Metals 
A significantly greater precision and convenience of 
analysis of the hydrogen in metals is related to the elucidation 
of the nature of the so-called "surface hydrogen." A variety 
of surface treatments of aluminum, such as turning samples on 
a lathe [1], etching them, or even exposure to air at room 
temperature [2], produces the emission of large amounts of 
hydrogen during vacuum heating. 
It is of interest to study the special feature of hydrogen 
emission during vacuum heating from samples whose surfaces have 
been etched with a 10% aqueous solution of NaOH at room temper-
ature. Experiments were conducted in parallel, using two 
samples of equal volume of pure aluminum ABOOO wire of differ-
ent surface area. The samples with the smaller (5 cm 2 ) surface 
were prepared from wire 0.8 mm in diameter, while those of the 
larger (20 cm 2 ), from 0.2 mm diameter wire. 
When the wire samples were vacuum heated directly upon 
delivery, they emitted large amounts (0.5-0.7 cm 3 /lOO g) of 
hydrogen with poor consistency, so all samples were given pre-
liminary heating in a vacuum for 3 hours at 600°C. 
In order to conduct the analysis, the samples were placed 
in a vacuum system. The quartz tubes used for the extraction 
* Numbers in the margin indicate pagination in the foreign text. 
1 
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were first heated to 700-S00°C, then allowed to cool to 600°C; 
when the vacuum had reached 10- 6 - 5 X 10- 5 rom Hg , the samples 
were placed by turns into a tube. The water inevitably emitted 
during the annealing of the samples was caught by a system of 
liquid nitrogen traps. The instantaneous hydrogen emission was 
recorded by an automatic pen, and the total amount of hydrogen 
was determined by integrating the area under the curve [3]. 
The results of the analysis of three pairs of samples after 
3 hours of preliminary heating in a vacuum and etching with a 
10% NaOH solution are as follows: 
Experiment number: 1 2 3 
Total hydrogen content, cm 3 /1OOg: 0.166 0.139 0.125 
O.lSl 0.155 0.18S 
Gas emission coefficient, K, min- 1 : 0.35 0.35 0.33 
l.2 ~ l.2 
(Note: values in the numerators refer to the 5 cm 2 
samples, the denominator to the 20 cm 2 samples.) 
The hydrogen content after etching exceeded by some 6 times 
the solubility of hydrogen in aluminum at 1 atrn pressure and 
600 °C. Note that there is only a small increase in the total 
hydrogen content with a four-fold increase in the sample surface 
area at constant volume. 
There is no doubt that the source of the hydrogen is the /19 
oxidation reaction of aluminum with water (or OH- groups) held 
on the oxide layer which was created by the etching of the 
metal in local sections, probably close to the grain boundaries. 
The density of the oxide layer is less in the 0.2 rom diameter 
samples than the 0.8 rom diameter samples, but the observed 
kinetics of hydrogen emission during vacuum heating of the 
2 
samples (see Figure 1) do not immediately contradict the kinetics 
of the reaction 
h ,M.'! 
15J Ln::------ ------- --- - ----, 
fDO 
~------,.--\ \ 
:---'--~::__--~-.-__:_-L---:..-...L----''--____'1.\ r-:-- i 
2 ~ b t5 fD 30 [ .ilY .'! 
Figure 1: Curves of hydrogen emission, h, over time, t, in 
minutes, during 600°C heating of etched aluminum samples of 
surface area: 1) 20 cm 2 ; 2) 5 cm 2 • The points indicate 
calculated values. 
The coefficient of hydrogen diffusion at room temperature 
in aluminum is very small [4J, and the accumulation of signifi-
cant amounts of hydrogen during etching is not possible . The 
formation of hydrogen occurs immediately during vacuum heating 
as a result of the oxidation of aluminum by water at the oxide-
metal interface. The initial oxide layer is not very permeable, 
and large amounts of hydrogen can accumulate during the ox ida-
tion of the sample. This, in turn, creates conditions which 
change the condition of the layer, increasing its permeability 
over the entire sample surface area. 
The slowest stage of the emission of hydrogen fr om heated 
samples is the passage of the hydrogen through the dense oxide 
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- - - --- - - - - _ ._ .. _- - - - - - - - -- - - - - - -- - - -- - - -
layer. Thus, the loss in hydrogen content of the sample during 
the time dt is 
qo dq = - D Vs dt. 
where q is the amount of hydrogen in the volume of the 
sample, in atm-cm 3 ; 
(1 ) 
D is the diffusion coefficient for hydrogen in oxide, 
in cm 2 /minj 
a is the surface area of the sample, in cm 2 ; 
V is the volume of the metallic interior of the 
sample, in cm 3 ; 
~ is the thickness of the oxide layer, in cm. 
If we ignore the resistance of the extraction tube and the 
ion source box of the omegatron to gas conduction, then, accord-
ing to [3], the change of pressure dP in the latter can be 
expressed as 
I SP dP = v dt - II dt ; 
where I is the rate of gas emission from the metal, 
atm-cm 3/min; 
V is the pumped volume, in cm 3 j 
S is the pump speed, in cm 3 /min. 
After integrating equation (1), a simple transformation 
and use of the notation K = Da/V~ produces 
dq -1\.1 1 = -- kqoe dt - • 
where qo is the initial hydrogen content of the sample. 
( 2) 
(3 ) 
After taking into account the linear relation between the 
omegatron index h and the partial pressure of hydrogen, P ~ mh 
(where m is the coefficient of proportionality), we solve 
4 
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equation (2) by substituting equation (3) in it, obtaining 
where 
B = K.q o . A = ~ . 
V ' V 
The ratio of coefficients of gas emission for models of dif-
ferent diameter in this case should be ~ 4. 
(4 ) 
h,M8.-_____ --, 
150 
100 
The coefficients of K and 
A were selected in such a manner 
that the curves of gas emission 
corresponding to the time t do 
not deviate from the experimen-
tal values of h by more than 
5 rnrn. See Figure 2. A prelim-
inary value for A can be obtained 
by solving the transcendental 
equation relating the time, to, 
and the height, h o, of the signal 
of maximum gas emission. At 
that point Figure 2: Curves of hydro-
gen emission, h, at 600 DC, 
for models of surface area: 
1), 3) 20 ern 2; 2), 4) 5 ern 2 • After the completion of 
gas emission during heating, we 
observe a small elevation of the level of the null line (see 
Figure 1). This is obviously related to the heterogeneous 
process which occurs during heating of the samples in the pres-
e nce of water vapor adsorbed on quartz walls, leading to the 
formation of molecular hydrogen. Therefore, the null line at 
large times of heating was extrapolated back to the beginning /21 
of gas emission and considered as the true null line. 
The results of processing the curves of gas emission from 
etched samples are presented in Figure 2. In all cases, 
5 
[gl(----
o 
-0,5 o 
Figure 3: Temperature 
dependence of the coef-
ficient, K, of gas 
emission. 
coefficient A remains within the 
limits 0.60 to 0.65. Figures 1 
and 2 show that equation (4) fol-
lows the kinetics of hydrogen 
emission sufficiently well. The 
values of K which have been obtained 
agree excellently with the mechanism 
considered for the diffusion of 
hydrogen across the oxide layer. 
The activation energy, which is 
calculated from the temperature 
dependence of K (see Figure 3), 
is 13,000 ±2,OO O cal/g-atom, 
satisfactorily close to the value obtained earlier [4]. 
6 
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REFERENCES 
1. Danalkin, V.A., in: Metody Opredeleniya i Issledovaniya 
Sostoy aniya Gazov v Metallakh ("Methods ~f Determining 
and Studying the C~nditions of Gases in Metals"), Nauka, 
1968, p. 24. 
2. Kostron, H., !. Metallkunde, !l (8), 268 (1952). 
3. Andreev, L.A., and B.G. Gellman, Izv. Vusov: Chernaya 
Metallurgiya, (5),19 (1971). 
4. Eichenauer, W., and A. Pebler, z. Metallkunde, 48 (7), 
373 (1957). 
7 
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The hydrogenation of metals upon interaction with water

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