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Vycor Glass
C. C. Leiby Jr. and C. L. Chen
Citation: Journal of Applied Physics 31, 268 (1960); doi: 10.1063/1.1735556
View online: http://dx.doi.org/10.1063/1.1735556
View Table of Contents: http://scitation.aip.org/content/aip/journal/jap/31/2?ver=pdfcov
Published by the AIP Publishing
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IP: 129.120.242.61 On: Thu, 27 Nov 2014 01:01:37
JOURNAL
OF
APPLIED
PHYSICS
VOLUME
31,
NUMBER
FEBRUARY,
1960
The permeability of a Vycor filter (680 cm2 area and 0.25 mm thick) is given for helium at six temperatures ranging from 299K to 723K, for neon and hydrogen at 673 oK and 723K, and for nitrogen at 673K.
The observed values and their temperature dependences are in good agreement with corresponding values
for fused quartz reported elsewhere. Values of the diffusion coefficient of these gases in Vycor also were
obtained experimentally, enabling calculation of their solubilities. Helium appears to deviate from activated
diffusion in Vycor somewhere between 100 and 26C. Its permeation velocity and diffusion coefficient at
26C are larger than expected for activated diffusion, while its solubility at 26C is one-half its value at
100C. These changes suggest that some structure sensitive diffusion process begins to dominate the activated or solution process at these lower temperatures. Helium flow rates through the filter as high as 2100
mm Hg (OC)Xcc/hr at a filter temperature of 4S0C and a pressure difference of 3S cm Hg (OC) were
observed. On the basis of observed permeation rates for the above gases, it is estimated that the filtered
helium has an impurity content of less than 1/S0th of its unfiltered value.
I. INTRODUCTION
'4
aXlo
prove adequate for this purpose, providing the membrane were thin enough and of sufficient area to filter
practical amounts of gas. Since Norton's values for
helium permeation in Vycor cover a range of temperatures from -78C to 25C, it was necessary to determine whether an extrapolation of his data to higher
temperatures (where the permeation velocity should
be greatly enhanced) was valid. Also it was considered
necessary to find the permeation velocities for other
gases which might be present in commercially available
"spectroscopically pure" helium in order to determine
the possible reduction in impurity content that could
be effected by the filter. Further, since the sensitivity
of the method employed in measuring these permeation
rates was quite good, it was also decided to include
measurements of the diffusion coefficients for the above
gases in Vycor. Knowledge of the permeation velocities
and diffusion coefficients of these gases enables their
solubilities to be calculated. These measurements were
deemed worthwhile inasmuch as the only published
values for the interaction of gases with Vycor glass
known to us are the three permeation velocities for
helium (at -78,0, and 25C) reported by Norton.!
II. PRINCIPLE OF THE EXPERIMENT
O~~~~~r-~rn---~40~--~--~--~'O
t Iminu!es)
dpldt=K(AIVd)t.p.
(1)
268
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H 2, AND
N 2 269
-3
4XI0
-3
3XI0
0.
J:
W
Ir
N e,
-3
i7l 2X10
<J)
dp
ADS
dt
Vd
Ir
<Xl
-=--~p[1+
1:
Q.
(3)
ZN
>
;::
m=!
IL
-3
w IXIO
-8
10
~~--~----~10----~----~20~--~----~
-9
10
(minutes)
(6)
K=DS.
1.0
2.0
3.0
llsee)
or its transform
dp 2AS(D)t
-=- ~p
dt
V
1f"t
2
[ ( d (2m+1)2)]
exp m=O
4Dt
1:
<Xl
(4)
(5)
(7)
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C.
270
C.
LEIBY, JR.,
,I
I
I
I
I
ra;;ZZZZm?zzzzzwzwzz;;Jj
_-1
AND
C.
L.
CHEN
The high vacuum portion of the system was thoroughly baked out at 400C and the portions external
to the bakeout region were flamed. At the conclusion
of this process, an ultimate pressure of the order of 10-10
mm Hg was achieved on the "clean" side of the system,
whereas the best obtainable pressure on the "dirty"
side was of the order of 10-7 to 10-8 mm Hg. This procedure was followed prior to the admission of each gas.
The filter oven was then raised to operating temperature and baked out until residual pressure rises on both
sides of the system, when closed off from the pumps,
stabilized. This usually required several hours. (For
example, at 400C, ultimate oven bakeout was reached
when the residual pressure rise on the clean side of the
system reached approximately 10- 7 mm Hg/hr, i.e.,
the expected helium diffusion rateS through the outer
Pyrex envelope from the atmosphere.) Prior to the
admission of gas to the filter, this filter bakeout was
carried as high as 475C for as long as twenty hours to
guarantee that quantities of the previous gas which
went into solution in the filter were removed.
The seal on the gas bottle containing the gas to be
filtered was then broken, and the gas slowly admitted to
the filter. This procedure occupied (roughly) two
minutes. The Alpert valve to the pumps was then closed
and "snap" pressure readings taken at specific time
intervals. Because of the strong (ion) pumping action
of the WL 5966 ion gauge, it was necessary to make
these readings in as short a dme as possible. After some
practice, this reading interval was shortened to approximately two seconds. Shorter reading periods proved impossible because of the inertia of the microammeter.
Repeated pressure readings were made until the
pr~ssure reached approximately 2X 10-3 mm Hg. At
thIS pressure, the gauge became nonlinear and it was
necessary to pump out the "clean" side of the system
and commence anew. This process was repeated until
two or three successive runs gave the same rate of increase of pressure with time. To identify each gas
(except nitrogen), a high-frequency discharge was
established in the filtered gas and its characteristic
color observed.
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DIFFUSION, SOLUBILITY,
AND
PERMEABILITY OF
15
x
x'"
E
E
Z
w
"0
0:
0
)0-
TABLE
Gas
T(ee)
He
26
100
Ne
H2
N2
He,
Ne,
2 ,
AND
N2
271
V(cc)
dp/ dt (atmos/sec)Qee
1830
1830
200
300
400
46.2
29.4
38.4
38.4
21.2
20.2
Hg)Oee
450
455
19.1
35.0
1590
1830
2.48XlO-9
6.59
8.94
4.09XlO- 8
7.08
1.60 X 10- 7
1.67
2.24
4.20
0.036
0.151
0.157
0.873
2.26
4.65
4.86
6.88
8.07
400
17.4
1830
450
17.1
1830
1.22 X 10-9
1.27
1.23
2.24
2.24
0.048
0.050
0.048
0.090
0.090
400
17.4
1830
450
17.1
1830
400
17.4
1830
3.36X 1()--9
3.50
3.53
8.06
7.40
8.43
1.6 XlO- 11
0.132
0.138
0.139
0.324
0.298
0.339
0.00063
1830
1830
1590
K (XIO')
...0
VI. EXPERIMENTAL RESULTS
0:
::>
!/)
!/)
Q.
0:
Z'"
UJ
>
;::
<.)
...~
UJ
O~~--~~~-5~~t(-m~,nu-te-S~)~--I~O~~~
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C.
272
C.
LEIBY,
JR.,
AND C.
CHEN
10'
f-
L.
106
.:J
Activation energy
(calories/deg C)
Glass
- - VYCOR
FUSED QUARTZ
>
Qo
ttw
5600
Fused quartz
5390
5700
4900
Vycor
5900
:2
Observer
Cl:
~IO-IO
~
Q
(!)
...J 10-11
1612
LO
20
30 103
40
not<)
800
700
500
600
450
400'C
800
600
500
400
300
200 C
>=
t::
g 10
..J
W
>
t5
!;i
10
2!
a:
,..
!!:
t-
~
o
U
0
..J
.-J -10
10
0.,
"'2
Cl
...J
10
10
,II
10~--'--~~~--'--~~~~~~~~~~
1.0
3
10
1.5
2.0
T("K)
O.B
1.0
1.2
1000
TI"K)
FIG. 7. Permeation velocity K of neon in Vycor and fused quartz
glasses vs reciprocal of the absolute temperature. K is in units of
cm3 (NTP)/sec/cm" area/mm thickness/cm Hg press. diff. (OC).
+, T'Sai and Hogness" (fused SiD.); ., our values (Vycor).
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DIFFUSION,
SOLUBILITY,
AND
PERMEABILITY
950
800
850
750
700
400"C
650
-II
10
ie
0.8
0.9
1.0
1.2
1.1
1.3
1.4
1.5
10
Tl"Kl
VII. DISCUSSION
J.
OF
He,
Ne,
H2,
AND
N2
273
Gas
26
He
100
400
400
400
D (cm'j sec)
6.3
5.9
XIO- s
X10- s
5 (cc/cc/atmos)
0.0043
0.0046
0.0094
0.006
0.007
10- 5-10-4
Llp(cm Hg)OC
Q(mm HgXcc/hr)OC
26
100
46.2
29.4
38.4
31.4
21.2
20.2
20.2
19.1
35.0
12.3
33.0
49.0
256
465
696
730
1410
2100
200
300
400
450
455
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274
C.
C.
LEIBY,
JR.,
AND
C.
L.
CHEN
10
VIII. ACKNOWLEDGMENTS
t T'Sai and Hogness14 postulated a channel diffusion mechanism, in which channel size increased with increasing temperature,
in order to explain their observations, but were unable to explain
how these channels could expand over fortyfold as their data
required. Alty [T. Alty, Phil. Mag. 15, 1035 (1933) ] later proposed
the overlapping wall potential concept to explain such a channel
widening effect, but he did not agree with the idea of a channel
diffusion process.
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