U.S. patent number 3,886,358 [Application Number 05/472,929] was granted by the patent office on 1975-05-27 for specimen transfer container for ion microprobe mass analyzer.
This patent grant is currently assigned to The United States Energy Research and Development Administration. Invention is credited to Stephen S. Cristy, John F. McLaughlin.
United States Patent |
3,886,358 |
McLaughlin , et al. |
May 27, 1975 |
Specimen transfer container for ion microprobe mass analyzer
Abstract
This invention is directed to a specimen holder for use with an
ion microprobe mass analyzer. The specimen holder provides for the
transfer of the specimen from an inert atmosphere to the analyzer
without exposing the specimen to an atmosphere reactive therewith
prior to analysis of the specimen.
Inventors: |
McLaughlin; John F. (Oak Ridge,
TN), Cristy; Stephen S. (Clinton, TN) |
Assignee: |
The United States Energy Research
and Development Administration (Washington, DC)
|
Family
ID: |
23877472 |
Appl.
No.: |
05/472,929 |
Filed: |
May 23, 1974 |
Current U.S.
Class: |
250/289; 850/18;
250/441.11 |
Current CPC
Class: |
H01J
49/0409 (20130101); H01J 37/20 (20130101) |
Current International
Class: |
H01J
49/02 (20060101); H01J 37/20 (20060101); H01J
49/04 (20060101); G01t 001/16 () |
Field of
Search: |
;313/330,363
;250/251,304-311,526,400,492,288,289,441 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Dixon; Harold A.
Attorney, Agent or Firm: Carlson; Dean E. Zachry; David S.
Larcher; Earl L.
Government Interests
The present invention relates generally to a specimen holder for
housing a reactive and/or hygroscopic specimen in an ion microprobe
analyzer, and more particularly to such a specimen holder for
transferring the specimen from an inert atmosphere to the analyzer
without exposing the specimen to a specimen-contaminating
environment. This invention was made in the course of, or under, a
contract with the United States Atomic Energy Commission.
Claims
What is claimed is:
1. A specimen holder for use with an ion microprobe mass analyzer
to provide for the transfer of a specimen to be analyzed from a
specimen-loading facility to a specimen-analyzing chamber
exhaustable to a predetermined pressure in said analyzer without
exposing the specimen to an atmosphere reactive with the specimen,
comprising an open housing having a receptacle at one end thereof
for receiving a specimen container through the opening, sealing
means at said open end of the housing disposed about said
receptacle, removable lid means adapted to be disposed over said
receptacle at said one end thereof in a contacting relationship
with said sealing means, a passageway projecting into said housing
in registry with said receptacle for placing said receptacle in
communication with a source of vacuum to a pressure corresponding
to said predetermined pressure for evacuating said receptacle and
pulling said lid means against said sealing means for enclosing
said receptacle, and valve means in registry with said passageway
for selectively opening and closing said passageway, with said lid
means being affixed to said housing upon evacuation of said
receptacle and closing of said passageway by said valve means,
whereby when said holder is positioned within the analyzer chamber
and when said chamber is at said predetermined pressure, the cover
is released from said contacting relationship with said sealing
means so that the specimen may be analyzed.
2. The specimen holder claimed in claim 1, wherein said specimen
container comprises a specimen-carrying block having a closed-end
cavity therein for receiving the specimen, a plurality of apertures
projecting through said block adjacent to said cavity, and wherein
said block is disposed fully within said receptacle with said
cavity opening towards said lid means and with said apertures
projecting between said lid means and the innermost surface of said
receptacle.
3. The specimen holder claimed in claim 2, wherein, in combination,
lid clamping means are disposed within said specimen-analyzing
chamber for receiving and securing said lid means to provide for
selective displacement of said housing from said lid means.
4. The specimen holder claimed in claim 3, wherein said
specimen-analyzing chamber has a rotatable disc disposed therein
with said disc having a receptacle therein for receiving said
specimen holder, said lid means has a flange projecting therefrom,
said lid clamping means has a pivotable arm thereon having a slot
therein for receiving said flange, and wherein clamping means
project into said slot for securing said lid means to said arm.
Description
The ion microprobe mass analyzer has proven to be a valuable
instrument for surface studies of many metallic materials and other
substances such as semiconductors and geological specimens. In the
operation of the ion microprobe a few layers of atoms are removed
from the surface of the specimen by ion bombardment sputtering. As
these atoms are removed they are simultaneously analyzed to
determine the mass-to-charge ratio of the atoms.
In order to obtain an accurate analysis of the specimen surface, it
is imperative that a specimen which is reactive and/or hygroscopic
with atmospheric gases and substances be appropriately shielded
from the atmosphere from the time it is mounted in the specimen
holder through the specimen analysis. This shielding of the
specimen from the atmosphere has limited the applicability of the
analyzer since, by design, the sample-holding chamber in the
analyzer is vented to atmosphere each time a specimen is placed in
the chamber. Further, there has previously been a problem in
transferring the specimen from an inert environment such as a dry
box where the specimen is loaded in the specimen holder to the
specimen-analyzing chamber in the analyzer without exposing the
specimen to the atmosphere. Such exposures which result in
reactions between the specimen and the atmosphere cause the
analysis of the specimen to be inaccurate.
Accordingly, it is the primary aim or objective of the present
invention to provide a specimen holder for use in an ion microprobe
mass analyzer whereby the holder shields the specimen from reactive
atmosphere constituents during transfer of the specimen from a
specimen-loading chamber having an environment inert to the
specimen into the specimen-analyzing chamber. The specimen holder
also shields the specimen while it is in the analyzing chamber
until the atmosphere containing reactants therein is evacuated. The
specimen holder capable of accomplishing these goals comprises a
housing having a receptacle at one end thereof for receiving a
specimen container, sealing means at said end of the housing
disposed about said receptacle, lid or cover means adapted to be
disposed over said receptacle at said one end thereof in a
contacting relationship with said sealing means, a passageway
projecting into said housing so as to place the receptacle in
registry with a source of vacuum for evacuating said receptacle and
pulling said cover means against said sealing means for enclosing
said receptacle, and valve means in registry with said passageway
for selectively opening and closing the latter, with said cover
means being affixed to said housing upon evacuation of said
receptacle and closing of said passageway by said valve means.
Other and further objects of the invention will be obvious upon an
understanding of the illustrative embodiment about to be described,
or will be indicated in the appended claims, and various advantages
not referred to herein will occur to one skilled in the art upon
employment of the invention in practice.
A preferred embodiment of the invention has been chosen for the
purpose of illustration and description. The preferred embodiment
illustrated is not intended to be exhaustive or to limit the
invention to the precise form disclosed. It is chosen and described
in order to best explain the principles of the invention and their
application in practical use to thereby enable others skilled in
the art to best utilize the invention in various embodiments and
modifications as are best adapted to the particular use
contemplated.
In the accompanying drawings:
FIG. 1 is an exploded perspective view partially sectioned showing
the specimen holder of the present invention;
FIG. 2 is a schematic plan view of the specimen chamber in the ion
microprobe analyzer showing details of the mechanism employed for
clamping and removing the lid from the specimen holder; and
FIG. 3 is an elevated view of the FIG. 2 structure showing further
details of the specimen holder and the lid clamping mechanism.
Described generally, the present invention is directed to a
specimen or sample holder for housing a specimen to be examined in
an ion microprobe analyzer. The specimen holder provides for the
transfer of the specimen from an inert environment where the
specimen is placed in the holder to the specimen chamber in the
analyzer where the specimen is analyzed without exposing the
specimen to atmosphere, which exposure may introduce deleterious
contaminants in the specimen due to reactions with the atmospheric
gases and/or substances. The holder also provides for isolating the
specimen from atmosphere in the specimen chamber of the analyzer
until the specimen chamber is evacuated. These features are
achieved by loading the specimen into the holder while the latter
is in a dry box or other suitable inert environment, placing a lid
on the holder over the specimen and then evacuating the internal
cavities of the holder for clamping the lid against the holder.
This vacuum is then maintained within the holder during the
transfer and the evacuation of the specimen chamber in the
analyzer. When the pressure in the analyzer is reduced to a value
lower than that in the holder, the lid is released and a lid
clamping mechanism holds the lid in place while the remainder of
the specimen holder is rotated away.
Described more specifically and with reference to the accompanying
drawings, the specimen holder of the present invention as generally
shown at 10 comprises a cylindrical base portion 12 containing a
centrally-disposed, cup-shaped recess or receptacle 14 extending to
approximately the middle of the base portion and having a flat
inner surface 15. A specimen-carrying block 16, which is of a
cylindrical configuration of a diameter slightly less than the
diameter of the receptacle 14, is adapted to be housed within the
receptacle 14 in a loose-fitting, easily removable manner. This
block 16 is, in turn, provided with a closed-end cavity 18 for
receiving a specimen as generally indicated at 20. With the block
16 placed within the cavity 14, the upper surface 21 of the base
portion is above the upper surface of the block 16. The upper
surface 21 is essentially flat about the entire circumference
defining this surface for receiving a lid or cover 22 which is of a
cross section generally corresponding to the outer diameter of the
base portion 12. With the specimen-carrying block 16 disposed
within the receptacle 14, the lid 22 is placed on surface 21 and a
vacuum is coupled to the base portion for evacuating the receptacle
14. This vacuum is applied by providing the base portion 12 with a
throughgoing passageway 24 which is in registry with the lower
surface 15 of the receptacle as shown. The communication with the
receptacle through the passageway is selectively interrupted by a
simple valve mechanism shown at 26 which is a threaded structure
receivable in a threaded aperture 31 in the base portion and
provided with longitudinally spaced-apart seals 28 and 30 for
blocking the passageway 24 so as to maintain the interior of the
receptacle at a pressure less than atmospheric pressure. To assure
that the receptacle 14 can be adequately evacuated, the block 16 is
provided with a plurality of throughgoing apertures such as the six
shown at 32. Thus, with a vacuum being drawn from a suitable vacuum
source (not shown) through passageway 32, the lid 22 is pulled
against the surface 21 of the base portion. To assure that the lid
is secured to the base portion by the differential pressure caused
by the vacuum within the receptacle, a suitable seal such as an
O-ring 34 is disposed in the surface 21 of the base portion about
the receptacle 14.
With the specimen 20 loaded in the specimen holder and the lid
clamped in place by evacuating the receptacle to a pressure in the
range of 10 to 50 millitorrs, the specimen is transferred to the
ion microprobe analyzer sample chamber generally shown at 37 in
FIG. 2. This specimen chamber 37 is provided with a rotatable disc
39 which is provided with a number of receptacles 41 of a diameter
sufficient for receiving the specimen holder 10. The specimen
holder is disposed in a suitable receptacle 41 and the lid 22 of
the specimen holder is fastened to a suitable lid clamping
mechanism 43 for removing the lid when the pressure in the chamber
is reduced to a pressure lower than that within receptacle 14 so as
to release the clamping action provided by the aforementioned
differential pressure. This lid clamping mechanism comprises a
pivotable arm 45 having an elongated slot 47 therein for receiving
a flange 49 on the lid 22. As shown, this flange 49 is off-set from
the major portion of the lid but, if desired, this flange can be
straight or disposed in any other satisfactory orientation. When
the arm 45 is pivoted so that the flange 49 projects into the slot
47, a suitable lid-retaining mechanism, such as shown by screws 51,
is activated to lock the lid in the clamping mechanism 43. A
sliding key 52 held by screw 53 slides into a slot 54 in the
pivotable arm 45 to hold the arm in position when the lid is
clamped. With the lid properly clamped, the pressure within the ion
microprobe specimen chamber is reduced to a pressure in the range
of about 10.sup.-.sup.6 to 10.sup.-.sup.7 torr. Inasmuch as this
pressure is less than the vacuum within the holder, the lid is
released from the surface 21 of the specimen holder but held in
place in the chamber 37 by the clamping mechanism 43. When this
release becomes effective or any other suitable time thereafter,
the disc 39 is selectively rotated to position the specimen in the
proper location within the analyzer so as to undergo the desired
testing.
In a typical operation of an ion microprobe analyzer using the
specimen holder of the present invention, a sample of anhydrous
lithium hydroxide (LiOH) was examined for water content. The LiOH
powder was transferred from a sealed container to the cavity 18 in
block 16 of the holder while in an argon-filled dry box containing
less than 1.5 ppm water. The block 16 carrying the powder was then
mounted in the receptacle of the holder and the lid 22 placed over
the receptacle 18. The specimen holder was then evacuated to 5
.times. 10.sup.-.sup.2 torr pressure for securing and sealing the
lid to the holder base 12. The mounted LiOH sample was then
transferred in the vacuum atmosphere of the specimen holder to the
ion microprobe sample chamber 37 where the lid was fastened to the
lid clamping mechanism 43 by the screws 51. After the pressure in
the instrument was reduced to 5 .times. 10.sup.-.sup.7 torr, the
specimen holder was rotated from under the lid into the position
required for examining the powder sample.
It will be seen that the present invention provides a relatively
simple solution to the problems of specimen contamination as
heretofore encountered since the sample or specimen holder readily
provides for the transfer of the specimen from an inert atmosphere
to the ion microprobe analyzer without the exposure of the specimen
to the surrounding environment. This isolation of the specimen from
the surrounding environment is maintained during the evacuation of
the analyzer to assure that no air-borne contaminant contacts the
specimen prior to analysis by the instrument.
As various changes may be made in the form, construction, and
arrangement of the parts herein without departing from the spirit
and scope of the invention and without sacrificing any of its
advantages, it is to be understood that all matter herein is to be
interpreted as illustrative and not in a limiting sense.
* * * * *