U.S. patent number 3,609,064 [Application Number 04/878,812] was granted by the patent office on 1971-09-28 for getter pump with direct resistance heating of getter strip.
This patent grant is currently assigned to S.A.E.S. Getters S.p.A.. Invention is credited to Bruno Ferrario, Tiziano A. Giorgi.
United States Patent |
3,609,064 |
Giorgi , et al. |
September 28, 1971 |
**Please see images for:
( Certificate of Correction ) ** |
GETTER PUMP WITH DIRECT RESISTANCE HEATING OF GETTER STRIP
Abstract
A getter pump comprising a substrate of high ohmic resistance; a
nonevaporable getter material embedded in the substrate; and means
for causing an electrical current to flow through the
substrate.
Inventors: |
Giorgi; Tiziano A. (Milan,
IT), Ferrario; Bruno (Milan, IT) |
Assignee: |
S.A.E.S. Getters S.p.A. (Milan,
IT)
|
Family
ID: |
11211929 |
Appl.
No.: |
04/878,812 |
Filed: |
November 21, 1969 |
Current U.S.
Class: |
417/51; 417/53;
96/126 |
Current CPC
Class: |
H01J
7/18 (20130101); H01J 7/186 (20130101) |
Current International
Class: |
H01J
7/00 (20060101); H01J 7/18 (20060101); F04b
037/02 (); B01d 053/26 (); B01d 039/00 () |
Field of
Search: |
;417/48,49,51,53
;55/208,387,389 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Walker; Robert M.
Claims
What is claimed is:
1. A getter pump comprising a substrate of high ohmic resistance; a
particulate nonevaporable getter material embedded in the
substrate; and means for causing an electrical current to flow
through the substrate wherein the substrate is of a material having
a resistivity of 1 to 200 microhm-centimeters when measured at
20.degree. C.
2. The pump of claim 1 wherein the nonevaporable getter material is
an alloy of 5 to 30 weigh percent aluminum, balance zirconium.
3. The pump of claim 2 wherein the nonevaporable getter material is
an alloy of 16 weight percent aluminum, balance zirconium.
4. The pump of claim 1 wherein the means for causing an electrical
current to flow comprises electrodes attached to opposite ends of
the substrate.
5. The pump of claim 1 wherein the substrate is pleated.
6. The pump of claim 5 wherein the pleated substrate is circularly
formed.
7. A getter pump of claim 1 comprising:
A. a gastight envelope having a rim defining an opening attachable
to a vessel in fluid communication therewith;
B. a first retainer fixedly attached to the envelope, the first
retainer having an annular groove;
C. a second retainer fixedly attached to the envelope, the second
retainer having an annular groove facing the annular groove of the
first retainer;
D. at least one strip of planar substrate of a material of high
ohmic resistance having embedded in the substrate a particulate
nonevaporable getter material, the pleated strip being between the
retainers resting in the annular grooves of adjacent retainers;
and,
E. means for causing an electrical current to flow through the
substrate, whereby imposing a potential across the electrodes
causes current to flow through the pleated strip heating and
activating the embedded getter material thereby increasing the rate
of sorption of gas within the vessel.
8. A getter pump comprising a substrate of high ohmic resistance; a
particulate nonevaporable getter material embedded in the
substrate; and means for causing an electrical current to flow
through the substrate wherein the substrate is of a material having
a resistivity of 10 to 150 microhm-centimeters when measured at
20.degree. C.
9. A process for increasing the sorptive rate of particulate
nonevaporable getter material embedded in a substrate comprising
the step of passing an electrical current through the substrate
thereby ohmically generating heat in the substrate and conducting
the heat to the particulate nonevaporable getter material wherein
the electrical current is passed at a rate such that the
particulate nonevaporable getter material is heated to 600.degree.
to 900.degree. C. to activate the getter material.
10. A process for increasing the sorptive rate of a particulate
nonevaporable getter material embedded in a substrate comprising
the step of passing an electrical current through the substrate
thereby ohmically generating heat in the substrate and conducting
the heat to the particulate nonevaporable getter material wherein
the electrical current is passed at a rate such that the
particulate nonevaporable getter material is maintained at a
temperature of 250.degree. to 400.degree. C. in order to sorb
active gases at a maximum rate while avoiding evolution of
hydrogen.
11. A getter pump comprising a substrate of high ohmic resistance;
a particulate nonevaporable getter metal embedded in the substrate
and means for imposing a potential across the substrate in order to
cause an electrical current to flow through the substrate heating
it and conducting the heat to the particulate nonevaporable getter
metal embedded therein.
Description
Getter pumps employing nonevaporable getter materials embedded in a
substrate are known and have found wide acceptance for producing
and maintaining a vacuum in closed vessels and especially in
electronic tubes such as klystron tubes, image intensifier tubes
and cathode-ray tubes. Such pumps employing getter materials are
especially suited for the pumping of active gases. The substrate
coated with the getter material is generally pleated and coaxially
disposed around a separate central resistance heater. In operation
heat is radiated from the resistance heater to the getter material
on the substrate. If the getter material has a clean fresh surface
the sorptive rate of gases increases with temperature as is well
known in the art. If the surface of the getter material is
partially or fully saturated with sorbed gases, the heat drives the
gas-reaction products, through diffusion, into the center of the
particles of the getter material and exposes a fresh surface.
Unfortunately such devices suffer from a number of disadvantages.
The presence of the necessary separate resistance heater increases
production costs. Uniform heating of the getter material is
difficult or impossible to obtain for example, because varying
portions of the coated substrate are at varying distances from the
heater. While it is desirable to coat both sides of the substrate
with the getter material only the side next to the heater is heated
by radiation whereas the side away from the heater must be heated
by conduction through the substrate. Because of the above,
relatively long heating periods are required in order to activate
the getter material.
Accordingly, it is an object of the present invention to provide
getter pumps which are substantially free of one or more of the
disadvantages of prior pumps.
Another object is to provide getter pumps which require no separate
heater.
A further object is to provide getter pumps wherein the getter
material can be easily and uniformly heated.
A still further object is to provide getter pumps employing a
substrate having a getter material on both sides which is heated
uniformly and simultaneously.
Still another object is to provide a getter pump which requires
only a short period of time to activate the getter material.
Still another object is to provide a novel process for activating a
nonevaporable getter material which is embedded in a substrate.
Additional objects and advantages of the present invention will be
apparent to those skilled in the art by reference to the following
detailed description and drawings wherein:
FIG. 1 is a sectional view of a getter pump of the present
invention taken along line 1--1 of FIG. 2; and,
FIG. 2 is a sectional view of a getter pump of the present
invention taken along line 2--2 of FIG. 1.
The above and other objects are accomplished by providing a getter
pump having a nonevaporable getter material embedded in a substrate
of high ohmic resistance and means for causing an electrical
current to flow through the substrate to heat the getter
material.
Referring now to the drawings and in particular to FIG. 1 there is
shown a nonlimiting preferred embodiment of the present invention
in the form of a getter pump 10 comprising a glass, gastight
envelope 11 having a rim 12 which defines an opening 13. By means
of the rim 12 the getter pump 10 is rendered attachable to any
vessel in which it is desired to maintain a vacuum. Fixedly
attached to and extending through the envelope 10 are three support
members 14, 15 and 16 (See FIG. 2). The support member 14 has near
the end nearest to the envelope 11 a first flanged washer 17
electrically spot welded to the support member 14 and acting as a
stop. Near the end of the support member 14 which is furthest from
the point of attachment of the support member 14 and the envelope
11 is a second flanged washer 18. A cylindrical sleeve 19 of heat
and electrical insulative material surrounds the portion of the
support 14 between the first flanged washer 17 and the second
flanged washer 18. As shown in FIGS. 1 and 2 the support members 15
and 16 have similar flanged washers and sleeves. Within the
envelope 11 is a first retainer 20 having a hole through which the
support member 14 passes, the diameter of the hole being less than
the diameter of the sleeve 19 such that the retainer 20 is fixedly
clamped on the support 14 between the first flanged washer 17 and
the sleeve 19. The retainer 20 has a flat portion 21 attached to an
outer rim 22 and an inner rim 23. The flat portion 21 in the inner
and outer rims 22 and 23 together form an annular groove. Within
the envelope 11 is a second retainer 24 identical to the first
retainer 20 but with its annular groove facing the annular groove
of the retainer 20. The second retainer 24 is fixedly held on the
support member 14 by the second flanged washer 18 and the sleeve
19. Slidably mounted on the sleeve 19 is an intermediate retainer
25 having annular grooves on opposite faces. Between adjacent
retainers 20 and 25 is a pleated strip 26 comprising a substrate 27
having thereon a particulate nonevaporable getter material 28. A
similar pleated strip 29 is between the second retainer 24 and the
intermediate retainer 25.
A first electrode 30 extends through the envelope 11 and is
electrically spot welded to the pleated strip 26 forming an
electrical contact therewith. Also extending through the envelope
11 is a second electrode 31 which is likewise spot welded to the
pleated strip 29. Surrounding the second electrode 31 in that
portion of the electrode between the first retainer 20 and the
intermediate retainer 25 is an insulative sleeve 32. As shown in
FIG. 2 conductor 33 connects the end of the pleated strip 26 with
the beginning of the pleated strip 29. Thus the pleated strips 26
and 29 comprise two electrical resistances connected in series with
electrodes 30 and 31. The strips 26 and 29 can be connected in
parallel but series is the preferred arrangement because of the
lower current required for equivalent heating. The retainers 20, 24
and 25; and the sleeves 19 and 32 can be of any heat resistant
dielectric material but are preferably ceramic.
The substrate 27 can be any material of high ohmic resistance such
that passage of current therethrough heats the getter material 28
to within the desired temperature range. However the substrate 27
is generally formed of a material having a resistivity of 1 to 200
and preferably 10 to 150 microhm-centimeters when measured at
20.degree. C. Within these limits of resistivity practical current
values can be employed. Examples of suitable substrate materials
include among others stainless steel containing 18 percent chromium
and 8 percent nickel, balance consisting essentially of iron; as
well as the widely used high resistance material available under
the trade name "Nichrome." Other suitable materials will
immediately be apparent to those skilled in the art.
In the broadest aspects of the present invention any nonevaporable
getter material can be employed such as titanium, zirconium,
tantalum or niobium as well as alloys and/or mixtures of two or
more of the above. The preferred nonevaporable getter material is
an alloy of 5 to 30 weight percent aluminum, balance zirconium, and
especially that alloy of 16 weight percent aluminum, balance
zirconium, available as "St 101 " from S.A.E.S. Getters S.p.A.,
Milan, Italy.
The getter material 28 is applied to the substrate 27 in the form
of a powder in order to have a high surface area to mass ratio
facilitating gas sorption. The powder is preferably one which
passes through a U.S. Standard screen of 140 mesh/inch. The powder
is attached to the strips 26 and 29 by any suitable means such as
rolling or pressing which does not materially reduce the total
surface area of the powder.
In operation the getter pump 10 is attached to a vessel to be
evacuated by sealing the rim 12 to the vessel. The vessel is then
evacuated by any convenient means such as a mechanical pump or a
zeolite pump. Then the electrodes 30 and 31 are connected to a
source of alternating or direct current whereby current flows
through the pleated strip 26 and the pleated strip 29 activating
the getter material, ohmically generating heat in the substrate 27,
conducting the heat to the particulate nonevaporable getter
material 28 and driving the sorbed gases into the interior of each
particle of getter material. Current is passed through the strips
26 and 29 such that the temperature of the getter material 28 is
held at 600.degree. to 900.degree. and preferably 700.degree. to
800.degree. C. At temperatures below this range activation is too
slow to be practical whereas at temperatures above this range
sinterization of the particles of the getter material 28 begins to
occur together with diffusion of the metal of the strips 26 and 29
into the getter material 28 and vice versa. Both sinterization and
diffusion tend to reduce the gas sorptive capacity of the getter
material 28.
Once activation is accomplished the getter material 28 is gas
sorptive at room temperature but the rate of gas sorption can be
increased by heating the getter material 28 as described above or
more preferably at temperatures of 250.degree. to 400.degree. C. in
order to avoid the evolution of hydrogen, which can be present in
the getter material 28 as a solid solution due to previous hydrogen
sorption. The getter material 28 remains gas sorptive after heating
is terminated and continues to sorb active gases evolved during the
life of the vessel. Should an undesirable increase in gas pressure
in the vessel occur, it is only necessary to connect the electrodes
30 and 31 to a source of power in order to reactivate the getter
material 28. In this manner, a very high vacuum can be maintained
in a vessel throughout its life and until the getter material 28
becomes saturated with gases.
The getter pumps of the present invention find utility as
supplements to sputter ion pumps and diffusion pumps and can be
used to create and maintain vacuum in continuously pumped vacuum
systems and in sealed off vacuum systems. These pumps can be
permanently installed for example in klystron tubes and image
intensifier tubes as so called appendage pumps.
The invention is further illustrated by the following nonlimiting
examples which are designed to illustrate the best mode of the
present invention.
Example I
This example illustrates the construction of a substrate having
embedded therein a nonevaporable getter material which substrate is
useful in the present invention.
Finely ground St101 nonevaporable getter material is passed through
a screen having 140 mesh/inch and is retained on a screen having
600 mesh/inch. This material is then placed on the center of a
strip of 18- 8 stainless steel 8 mm. wide and 0.2 mm. thick leaving
a getter material free margin near the edges of the strip. On top
of the powder is placed a strip of common soft iron of the same
dimensions. The two strips with the St101 alloy between them are
then pressed together by a roller whereupon the strip of soft iron
is removed leaving the St101 alloy adhering to the strip of
stainless steel. A plurality of slits are then made at intervals of
6 mm. across the strip and extending into the margin which is free
of St101 alloy. The strip is then folded adjacent to the slits to
form a pleated strip which is then circularly curved to be employed
in the getter pump of the present invention.
EXAMPLE II
A substrate having a getter material embedded thereon is produced
as described in U.S. application Ser. No. 527,906, filed Feb. 16,
1966. The substrate is then pleated as in example I.
EXAMPLE III
A substrate coated on both sides with St101 alloy is purchased from
S.A.E.S. Getters S.p.A. of Milan, Italy, under stock number
St101/Ct/8.times.6/D60 and pleated as described in example I.
EXAMPLE IV
A substrate coated on both sides with St101 alloy is purchased from
S.A.E.S. Getters S.p.A. of Milan, Italy under stock number
St101/Ct/15 .times.6/D150.
EXAMPLE V
The pleated strip of example III is circularly formed as shown in
FIGS. 1 and 2, attached to electrodes 30 and 31 and placed in a
getter pump 10 as shown in FIGS. 1 and 2. The getter pump 10 is
then attached to a glass vessel of about 1 liter in volume whose
pressure is reduced to 10.sup..sup.-3 torr using zeolites whereupon
a current of 7 amps is passed through the electrodes 30 and 31 for
a period of 10 minutes activating the getter material and reducing
the pressure of active gases in the vessel to 10.sup..sup.-8 torr
in an overall time of 20 minutes. Similar results are obtained with
the pleated strips of examples I, II and IV.
Although the invention has been described in considerable detail
with reference to certain preferred embodiments thereof, it will be
understood that variations and modifications can be effected within
the spirit and scope of the invention as described above and as
defined in the appended claims.
* * * * *