U.S. patent number 3,622,782 [Application Number 04/775,565] was granted by the patent office on 1971-11-23 for blocking apparatus and method utilizing a low-energy ion beam.
This patent grant is currently assigned to Minnesota Mining and Manufacturing Company. Invention is credited to James W. Salo, David P. Smith.
United States Patent |
3,622,782 |
Smith , et al. |
November 23, 1971 |
**Please see images for:
( Certificate of Correction ) ** |
BLOCKING APPARATUS AND METHOD UTILIZING A LOW-ENERGY ION BEAM
Abstract
Apparatus and method for producing a blocking pattern of the
crystalline structure of a solid surface using a low-energy ion
beam is shown wherein the low-energy ion beam is focused to a
predetermined cross section and directed by an extended bored
member onto a predetermined area of the solid surface at an angle
greater than 5.degree. and less than 90.degree. enabling the ions
to be scattered from the solid surface to produce a projected
blocking pattern which impinges upon a fluorescent screen
positioned substantially parallel to and spaced a predetermined
distance from the solid surface for producing as a visual image the
projected blocking pattern representing the crystalline structure
of the solid surface. The extended bored member also collimates the
focused ion beam into a smaller predetermined cross section and
produces secondary electrons while collimating the focused beam to
thereby produce a cloud of electrons which neutralize any charge at
the solid surface produced by incidence of the collimated ion
beam.
Inventors: |
Smith; David P. (Hudson,
WI), Salo; James W. (Cottage Grove Village, MN) |
Assignee: |
Minnesota Mining and Manufacturing
Company (St. Paul, MN)
|
Family
ID: |
25104796 |
Appl.
No.: |
04/775,565 |
Filed: |
September 16, 1968 |
Current U.S.
Class: |
850/43;
219/121.24; 219/121.35; 250/399; 250/492.3; 219/121.26; 219/121.33;
250/309; 250/492.1 |
Current CPC
Class: |
H01J
37/08 (20130101); H01J 37/20 (20130101); H01J
37/252 (20130101) |
Current International
Class: |
H01J
37/252 (20060101); H01J 37/20 (20060101); H01J
37/08 (20060101); H01j 037/26 () |
Field of
Search: |
;250/49.5 (1)/ ;250/49.5
(5)/ ;250/49.5 (9)/ ;219/121EB |
References Cited
[Referenced By]
U.S. Patent Documents
|
|
|
3221133 |
November 1965 |
Kazato et al. |
3277297 |
October 1966 |
Forrester et al. |
3415985 |
December 1968 |
Castaing et al. |
|
Primary Examiner: Lawrence; James W.
Assistant Examiner: Birch; A. L.
Claims
We claim:
1. Apparatus for producing a blocking pattern of a solid surface of
a sample by means of a low-energy ion beam comprising
generating means for generating a low-energy ion beam having a
predetermined mass and energy;
focusing means cooperating with said generating means for focusing
said generated ion beam into a predetermined cross section;
directing means including an extended bored member operatively
coupled with said focusing means for collimating said focused ion
beam into a smaller predetermined cross-section and directing said
collimated ion beam at an angle greater than about 5.degree. and
less than about 90.degree. onto a predetermined area of said solid
surface enabling said ions to slightly penetrate said solid surface
and be scattered from said solid surface as a function of the
crystal structure of the atoms forming said solid surface to
produce a blocking pattern representing as a projected pattern the
crystalline structure of said solid surface and formed of scattered
ions from said directed smaller predetermined cross-section ion
beam, which extended bored member has an inside cross-section
corresponding to said smaller predetermined cross-section, and the
interior of which extended bored member includes material capable
of producing secondary electrons when the extended bored member is
collimating said focused ion beam to thereby produce a cloud of
electrons to neutralize any charge at said solid surface produced
by incidence of said collimated ion beam; and means for sensing
said blocking pattern.
2. The apparatus of claim 1, wherein the extended bored member
includes a converging portion at the entry of said focused ion beam
into the extended bored member.
3. The apparatus of claim 1, wherein the extended bored member is
formed of a needle having an inside cross-section corresponding to
said smaller predetermined cross-section.
4. The apparatus of claim 1, wherein the extended bored member is
formed of a stainless steel needle having an inside cross-section
corresponding to said smaller predetermined cross-section.
5. The apparatus of claim 1, wherein the interior of said extended
bored member comprises a conductive material including
semiconductive material.
6. The apparatus of claim 1, wherein the interior of said extended
bored member comprises an insulating material.
7. The apparatus of claim 1, further comprising
a scattering gas source, to which the generating means is
operatively coupled for producing ions to be focused, directed
onto, and scattered from said predetermined area of said solid
surface; and
a sputtering gas source, to which the generating means is
operatively coupled for producing ions to be included in said
generated, focused, and directed ion beam for sputtering said
predetermined area of said solid surface.
8. Apparatus for producing a blocking pattern of a solid surface of
a sample by means of a low-energy ion beam comprising
generating means for generating a low-energy ion beam having a
predetermined mass and energy;
focusing means cooperating with the generating means for focusing
said generated ion beam into a predetermined cross-section;
directing means operatively coupled with the focusing means for
collimating said focused ion beam into a smaller predetermined
cross-section and directing said collimated ion beam at an angle
greater than about 5.degree. and less than about 90.degree. onto a
predetermined area of said solid surface enabling said ions to
slightly penetrate said solid surface and be scattered from said
solid surface as a function of the crystal structure of the atoms
forming said solid surface to produce a blocking pattern
representing as a projected pattern the crystalline structure of
said solid surface and formed of scattered ions from said directed
smaller predetermined cross-section ion beam;
sensing means for sensing said blocking pattern;
a scattering gas source, to which the generating means is
operatively coupled for producing ions to be focused, directed
onto, and scattered from said predetermined area of said solid
surface; and
a sputtering gas source, to which the generating means is
operatively coupled for producing ions to be included in said
generated, focused, and directed ion beam for sputtering said
predetermined area of said solid surface.
9. The apparatus of claim 8, wherein the first gas source is
selected to be hydrogen or helium and the second gas source is
selected to be an inert gas such as argon.
10. The apparatus of claim 8, further comprising
means for either alternatively or simultaneously operatively
coupling the sputtering gas source with the generating means.
11. A method for producing a blocking pattern of a solid surface of
a sample with a low-energy ion beam comprising the steps of
generating a low-energy ion beam having a predetermined mass and
energy;
focusing said generated ion beam into a predetermined
cross-section;
directing said focused ion beam with an extended bored member at an
angle greater than about 5.degree. and less than about 90.degree.
onto a predetermined area of said solid surface enabling said ions
to slightly penetrate said solid surface and be scattered from said
solid surface as a function of the crystal structure of the atoms
forming said solid surface to produce a blocking pattern
representing as a projected pattern the crystalline structure of
said solid surface and formed of scattered ions from said directed
ion beam, which directing step includes the steps of
collimating said focused ion beam with said extended bored member
having an inside cross-section corresponding to a smaller
predetermined cross-section to collimate said focused ion beam into
a smaller predetermined cross-section for direction onto said solid
surface, and
producing secondary electrons with the extended bored member when
the extended bored member is collimating said focused ion beam to
thereby produce a cloud of electrons to neutralize any charge at
said solid surface produced by incidence of said collimated ion
beam; and
sensing said blocking pattern.
12. A method according to claim 11, further comprising the steps
of
providing a scattering gas for producing ions to be focused,
directed onto, and scattered from said predetermined area of said
solid surface; and
providing a sputtering gas for producing ions to be included in
said generated, focused, and directed ion beam for sputtering said
predetermined area of said solid surface.
13. A method for producing a blocking pattern of a solid surface of
a sample with a low-energy ion beam, comprising the steps of
generating a low-energy ion beam having a predetermined mass and
energy;
focusing said generated ion beam into a predetermined
cross-section;
directing and collimating said focused ion beam into a smaller
predetermined cross-section and at an angle greater than about
5.degree. and less than about 90.degree. onto a predetermined area
of said solid surface enabling said ions to slightly penetrate said
solid surface and be scattered from said solid surface as a
function of the crystal structure of the atoms forming said solid
surface to produce a blocking pattern representing as a projected
pattern the crystalline structure of said solid surface and formed
of scattered ions from said directed and collimated smaller
predetermined cross-section ion beam; and
sensing said blocking pattern; wherein the method further includes
the steps of
providing a scattering gas for producing ions to be focused,
directed onto, and scattered from said predetermined area of said
solid surface; and
providing a sputtering gas for producing ions to be included in
said generated, focused, and directed ion beam for sputtering said
predetermined area of said solid surface.
Description
Low-energy ion scattering apparatus and method are known in the
art. Such apparatus and methods are described in an article
entitled "The Influence of Absorbed Gases On Surface Analysis For
Low-Energy Ion Scattering" by David P. Smith which appeared in the
Oct. 1966 Transactions of the Thirteenth National Vacuum Symposium
of the American Vacuum Society at pages 189 and 190 and in an
article entitled "Scattering Of Low-Energy Noble Gas Ions From
Metal Surfaces" by David P. Smith which appeared in the Jan. 1967
Journal of Applied Physics at pages 340--347.
The above-noted articles clearly and sufficiently describe the use
of low-energy ion scattering wherein the energy of a scattered
primary gas ion is used for surface compositional analysis of a
solid surface.
In a recent article entitled "Proton Scattering Microscopy" by R.
S. Nelson which appeared in the Apr. 1967 Philosophical Mag.,
Volume 15 at pages 845--854, a method and apparatus are disclosed
for producing what Nelson considers to be proton blocking patterns
on a fluorescent screen using protons having an energy in excess of
20 Kev.
The use of high-energy proton beams having energies in the order of
20 Kev. for producing proton blocking patterns to represent the
atomic structure of a crystalline surface have several inherent
disadvantages. For example, the use of high-energy protons
extracted from conventional plasma-type sources and utilized to
produce a blocking pattern representing the crystal structure of
the surface of an insulating material causes the insulating
material to store a charge thereon which has the effect of
establishing a field which repels the proton beam being directed
onto the surface thereof.
Other disadvantages of the prior art apparatus include that a mass
analyzer must be used to obtain an ion beam of desired mass and
energy and that the apparatus must operate at high voltage levels
in the order of 20 kv. or higher. In addition, when samples to be
analyzed are of an insulating material, it appears that the sample
builds up a positive surface charge which may repel the ion beam.
Also, the samples must be separately cleaned and prepared by
separate apparatus and methods for use before the solid surface
thereof can be analyzed by the prior apparatus.
The present invention overcomes the disadvantages of the prior art
apparatus and method for analysis of the crystalline structure of
the surface of material by use of a unique and unusual means for
directing an ion beam onto the surface of the material. The ion
beam directing means includes an extended bored member which is
capable of collimating a focused ion beam of a predetermined cross
section into a collimated ion beam of a smaller predetermined cross
section, of directing the collimated ion beam to a predetermined
area of the material surface, and of producing secondary electrons
while collimating the ion beam to produce a cloud of electrons
which are attracted to the material surface to prevent a surface
charge built up on the surface of the material which otherwise
would repel or interfere with the ion beam being directed upon the
material surface. The neutralizing capability is particularly
significant when producing a blocking pattern from an insulating
material.
Another advantage of the present invention is that low-energy ions
having an energy level in the order of less than 10 Kev. can be
used for producing the ion blocking pattern illustrating the atomic
structure of a solid surface.
Another advantage of the present invention is that an ion beam
generating source is disclosed which is capable of precisely
directing an ion beam of a predetermined cross section onto a
predetermined area of a solid surface which is to have an ion
blocking pattern produced illustrating the crystal structure of the
solid surface.
Yet another advantage of the present invention is that a unique and
novel method for generating an ion blocking pattern representing
the crystalline structure of a solid surface by use of low-energy
ions scattered from the surface is disclosed.
Still another advantage of the present invention is that in a
preferred embodiment one ion beam including both scattering ions
and sputtering ions can be used for producing a blocking pattern of
the solid surface being analyzed and for sputtering or eroding the
solid surface at a controlled rate. The inclusion of both
sputtering and scattering ions in the ion beam has the advantage of
providing a convenient means for preparing a surface by sputtering
to remove the atoms of any amorphous or foreign material from the
solid surface to be analyzed while the sample is mounted for
observation by the scattering ion in the beam.
These and other advantages become readily apparent in light of the
detailed description of the preferred embodiment disclosed herein
taken together with the drawing wherein:
FIG. 1 is a frontal cross-sectional view of an ion generating
source capable of producing low-energy ion beams having a
predetermined cross section;
FIG. 2 is a pictorial representation illustrating the relationship
between the end of the ion source relative to a solid surface which
is to have a projected blocking pattern of its crystalline
structure produced on a substantially parallel and fluorescent
screen spaced at a predetermined distance from the solid
surface;
FIG. 3 is a frontal sectional view of a portion of apparatus for
selectively positioning a selected one of a plurality of samples
adjacent an ion source for generating a visual blocking pattern
which can be observed by means of a window;
FIG. 4 is a graphic representation of a blocking pattern of the
crystalline structure of a gold crystal produced by a low-energy
ion beam directed at and scattered from the surface thereof;
and
FIG. 5 is a schematic diagram partially in block form illustrating
a control system for automatic control of the operation of the
apparatus of FIG. 3.
Briefly, the apparatus and method disclosed herein is capable of
producing a blocking pattern of a solid surface of a sample by
means of a low-energy ion beam. In one embodiment, the apparatus
includes a means for generating a low-energy ion beam having a
predetermined mass and energy. A means which cooperates with the
generating means is utilized for focusing the ion beam into a
predetermined cross section. A directing means is operatively
coupled with the focusing means and collimates the ion beam into a
smaller predetermined cross section. The directing means also
directs the collimated ion beam at an angle greater than about
5.degree. and less than about 90.degree. onto a predetermined area
of the solid surface enabling the ions to slightly penetrate the
solid surface and be scattered from the solid surface as a function
of the crystal structure of the atoms forming said solid surface to
produce a blocking pattern representing as a projected pattern the
crystalline structure of the solid surface and formed of scattered
ions from the smaller predetermined cross-section ion beam. A
fluorescent means is positioned substantially parallel to and
spaced a predetermined distance from the solid surface. The
fluorescent means receives ions scattered from the smaller
predetermined cross-section ion beam forming the blocking pattern
for producing as a visual image the blocking pattern which
represents as a blocking pattern the crystalline structure of the
atoms forming the solid surface.
FIG. 1 illustrates a novel and unique ion source which includes a
collimating member having an extended aperture. An ion source
support, generally designated as 10, formed of a conductive
material is utilized for supporting the ion source, generally
designated as 12, ion focusing means, generally designated as 14,
and an ion directing means, generally designated as 16. The
directing means 16 forms the collimating member having an extended
aperture, which in this embodiment is an extended bore 100. The
support 10 is grounded to a common conductor, generally designated
as 20.
The ion source 12 includes a heatable metallic filament 22 which in
the preferred embodiment is formed of a thoriated tungsten wire.
The wire filament 22 is supported by filament supports 24 and 26
which are isolated from the conductive support 10 by means of
insulators 28 and 30 respectively. The filament supports 24 and 26
are formed of a conductive material and are operatively coupled to
the secondary winding of a filament isolation transformer,
generally designated as 32. The filament isolation transformer 32
is in turn energized from a power source which may be a variac
transformer, generally designated as 34, operatively coupled to a
source of alternating current potential (not shown).
A first or scattering gas source 36 and a second or sputtering gas
source 38 are operatively coupled via a first valve 40 and a second
valve 42 respectively to a tube 43. Tube 43 in turn is connected
into an enclosed housing, generally designated as 44, which defines
a chamber 46 enclosing the wire filament 22. The tube 43 is
supported as it passes through the support 10 by means of a ceramic
insulator 48. The housing 44 defining the chamber 46 is mounted on
support 10 by means of a raised cylindrically shaped support 50
which is integral with the planar portion of the support 10.
Ceramic spacers 52 are used as supports between the raised
cylindrically shaped support 50 and a conductive shield and support
member 54 having raised outer edges 56. The shield member 54 is in
turn operatively connected to the housing 44 thereby providing a
rigid support for the housing and preventing light emanating from
the filament 22 from passing outside of the ion source.
The housing 44, which defines the chamber 46, terminates in an
annular-shaped opening 60. Interposed between the wire filament 22
and the opening 60 is a conductive wire mesh 62 which in this
embodiment is selected to be tungsten mesh.
Ions which are to be scattered from the solid surface of a sample
to be analyzed are generated within the chamber 46 by establishing
a potential difference between the wire filament 22 and wire mesh
62 to produce a localized source of electrons and by opening valve
40 and closing valve 42 to pass gas from the scattering gas source
36 via tube 43 into the chamber 46 and in the vicinity of the
heated wire filament 22. The gas molecules are bombarded by and
interact with the electrons passing between the filament 22 and
wire mesh 62 to produce the gas ions. The resulting gas ions pass
through the conductive mesh 62 and exit through the opening 60 of
housing 44.
In the preferred embodiment, the scattering gas is hydrogen. When
the hydrogen gas molecules are bombarded by the electrons from
filament 22, several ions are produced; namely H.sub.1 .sup.+,
which is an atomic ion, and H.sub.2 .sup.+, which is a molecular
ion.
It appears that about equal quantities of each ion are produced.
Therefore, mass analysis of the ions is unnecessary and the
resolution of the ion blocking pattern is not seriously affected by
the patterns produced by scattering of each type ion. Also, heavier
gas atoms could be used as the scattering ion source, such as for
example helium, where hydrogen atoms upon being ionized forming
ions would be detrimental due to chemical reactivity with the
surface being analyzed.
If desired, the second or sputtering gas source 38 can be used
either alternately or simultaneously with the scattering gas source
to clean the surface being analyzed. Typically, an inert gas is
used for sputtering, such as for example argon. The sputtering gas
can be passed from gas source 38 into chamber 46 via tube 43 by
opening valve 42. The resulting sputtering gas beam passes along
the same path as the scattering ion beam.
By using the teachings of the present invention, it is possible to
observe the crystal structure of the solid surface while the same
is being sputtered or cleaned. This is accomplished by opening both
valves 40 and 42. Such a feature has wide utility in that a
crystalline sample with a contaminated or amorphous surface layer
can be placed into the ion blocking apparatus, be sputtered and
then have its crystalline structure displayed. Also, by using the
scattering gas source and sputtering gas source concurrently, one
can observe the crystal structure of the solid surface being
developed due to cleaning during the sputtering process. By knowing
ion current densities, sputtering yields and sputtering times
required to produce a blocking pattern representative of a
crystalline surface, it is possible to measure or determine the
thickness of the amorphous or noncrystalline layer. This technique
would have wide utility, such as, for example, to measure the
thickness of destruction layers produced by mechanically polishing
of semiconductor crystals for use in an electron beam laser.
The focusing means 14 is formed of a plurality of spaced parallel
annular-shaped lens elements 70-78. Each of the annular-shaped lens
elements 70-78 has an opening of predetermined diameter, namely the
ions emanating from opening 60 to pass therethrough. The elements
70-78 are stacked in a coaxial aligned relationship and are spaced
from each other by means of a plurality of insulating spacers,
generally designated as 80. The combination of annular-shaped
members having an aperture therethrough positioned in aligned
coaxial relationship and which form an electrostatic focusing means
is generally known as an Einzel focusing lens. As is readily
apparent, the diameter of the apertures in each of the lens
elements or plates is selected so that the beam can be focused to a
predetermined cross section at the opening of the last aperture
plate 78.
In the embodiment illustrated in FIG. 1, aperture plate 74 is
electrically connected to a variable voltage dividing network,
generally designated as 84, so that an appropriate focusing
potential can be applied to the ions to form the same into an ion
beam. The other aperture plates 70, 72, 76 and 78 are electrically
connected to the common conductor 20. A high voltage source,
generally designated as 86, is operatively connected to the voltage
dividing network 84 which is in turn connected to conductor 20 for
providing the desired high voltage focusing potential. Typically,
the high voltage source 86 will provide a variable high voltage
output in the order of 0-10 kv.
A second lower voltage source, generally designated as 88, is
operatively connected between the housing 44 and one of the
filament supports 26. The high voltage source 88 is used to control
the amount of bias applied to the wire filament 22.
In the preferred embodiment, the aperture plate 74 is formed of
stainless steel having a thickness in the order of about one-half
inch (about 12 mm.) while the other aperture plates 70, 72, 76 and
78 are formed of stainless steel having a diameter in the order of
about one-quarter inch (about 6 mm). The spaces between each of the
aperture plates 70-78 are selected to be about three-fourths inch
(about 18 mm). The voltage dividing network 84 is formed of four
4.7--megohm resistors and a potentiometer having a rating of 5
megohms. The voltage source 88 is selected to have a voltage in the
order of 100 to 150 volts DC. The high voltage source 86 is
selected to be in the order of 5 kv. However, in some experiments,
a voltage in the order of 1 kv. was operative.
At the outlet of the focusing means 14 is mounted the directing
means 16 or collimating member having an extended aperture which in
the preferred embodiment is in the form of an extended bored member
100. The bored member 100 is attached to the aperture plate 78 in
alignment with the axis thereof. The bored member 100 may be formed
of a stainless steel needle having an inside diameter in the order
of about .030 inch (about .75 mm). It is contemplated that a
conductive material, which includes semiconductive material, can be
used as the directing means. If desired, an insulating material can
be used as the directing means, such as, for example, a thin layer
of aluminum oxide on an aluminum surface.
In this manner, the focusing means 14 can focus the ions emanating
from opening 60 of housing 44 into an ion beam of predetermined
cross section at a focal point located on the outer surface of
annular plate 78 and in alignment with the aperture thereof. The
ion beam of predetermined cross section then passes through the
bored member 100 and is collimated into an ion beam having a cross
section which is precisely determined by the inside cross section
of the bored member 100.
It has been determined that the outer portion of the ion beam
contacts the inner surface of the bored member 100 and results in
the creation of secondary electrons which in turn build up a space
charge of electrons near the outlet of bored member 100. The
so-generated space charges are attracted to any positive surface
charges located on the surface of the sample being bombarded. By
this technique, the space charges of electrons neutralize the
positive surface charges enabling the ion beam to bombard the
surface of the sample and be scattered from the surface of the
sample without the ion beam being repelled or deflected.
FIG. 2 pictorially represents the end of the bored member 100
positioned adjacent a crystalline surface 110 which is mounted onto
a support 112. The ion beam, generally designated by line 114,
emanates from the outlet of bored member 100 which is positioned
just adjacent the surface of solid 110. The ion beam 114 is
directed at a predetermined angle .theta. relative to the surface
of the support 112. It has been determined that the angle .theta.
should be greater than 5.degree. and less than 90.degree. such that
the ions from the ion beam 114 are scattered into a pattern,
generally designated as 116. During scattering, some of the
scattered ions are neutralized by the electrons in the sample. The
scattered ions and other particles including the neutralized ions
or atoms bombard a fluorescent means 120 which converts the ion
blocking pattern into a visual ion blocking pattern. The
fluorescent means 120 may be a fluorescent screen 120 which is
positioned substantially parallel to and spaced a predetermined
distance from the solid surface 110.
When a post accelerating negative voltage was applied to the
fluorescent phosphor screen to accelerate positive scattered ions,
no detectable increase in brightness of the fluorescent phosphor
was observed as would be expected if the scattered ions were not
efficiently neutralized. Thus, it appears that the blocking pattern
is formed substantially of neutralized ions which, of course, is a
blocking pattern formed of scattered ions from the smaller
predetermined cross section ion beam.
The so-produced visual ion blocking pattern is a projected image of
the crystallographic directions in the bombarded sample. The
prominent dark areas of the visual ion blocking pattern represent
the directions of rows of atoms in the crystal which inhibit
scattering of ions.
The angle limits of greater than 5.degree. and less than 90.degree.
set forth above are practical limits on the angle between the ion
beam of smaller predetermined cross section and the solid surface.
Generally, an angle in the order of 20.degree. is preferred.
In the preferred embodiment, the fluorescent screen comprises a
thin optically transparent layer of tin oxide deposited on Pyrex
glass and which is coated with a uniform thin layer of Pl type
phosphor. The predetermined distance between the fluorescent screen
120 and the support 112 is in the order of one-fourth inch to 1
inch (about 6 mm. to 25 mm).
FIG. 3 illustrates an apparatus adapted for producing an ion
blocking pattern of the crystalline structure of a solid surface.
The apparatus includes a vacuum chamber, generally designated as
200, which includes an ion gun chamber 204 and a sample support
chamber 206. The ion gun chamber 204 is positioned at a
predetermined angle relative to the sample support chamber 206 such
that the ion beam can be directed at a predetermined angle onto the
surface of the solid which is to have the ion blocking pattern of
its crystal structure produced on a fluorescent screen. A support
208 bearing a disk-shaped sample holder 210 provides a means for
positioning any one of several samples and materials for
bombardment by the ion beam for generating the ion blocking
patterns of the atomic structure of its surface. The support shaft
212 extends to the outside of vacuum chamber 200 and is capable of
rotating the sample holder 210. A geared positioning member 214 is
mounted in a support 215 having a plurality of openings therein.
The geared positioning member 214 is operatively attached to
rotatable shaft 226 and is capable of being rotated to position
screen support 232 a predetermined distance relative to the sample
holder 210. Rotatable shaft 226 extends to the outside of the
apparatus so that it can be rotated.
A fluorescent screen 230 is supported by a screen support 232 a
predetermined distance from the sample holder 210. By rotating
shaft 226, this distance can be selectively changed to vary the
magnification of the blocking pattern. A window 236 is located on
the exterior portion of vacuum chamber 200 in alignment with the
fluorescent screen 230 and the disk-shaped member 210. The window
236 enables a viewer to observe the ion blocking pattern formed on
the fluorescent screen 230 when the ion beam from the bored member
220 is scattered from the surface of a sample located on the sample
support 208. The sample support vacuum chamber 206 is evacuated via
a pumping port 217 and support 215 to a pressure in the order of
10.sup.-.sup. 5 Torr during operation. Samples within the pumped
vacuum of the sample support chamber 206 can be selectively
positioned by rotating the sample support shafts 212 and 226
thereby enabling a viewer to observe ion blocking patterns from a
plurality of samples without interruption of the vacuum. Samples
can be removed and placed onto the sample support 208 by admitting
atmospheric pressure into the sample support chamber 206 and by
removing a cover 238 which is located in alignment with the ion gun
chamber 204. After the samples have been positioned onto the sample
support 208, the cover 238 can be repositioned onto the sample
support chamber 206 and the entire chamber can then be repumped to
the desired vacuum level and operation of the apparatus
reestablished.
FIG. 4 illustrates a typical ion blocking pattern produced from a
single crystal gold surface. The pattern is formed by the ions from
the scattering gas source penetrating a few atomic layers into the
solid surface and being scattered back out of the solid. Depending
on the crystalline structure of the sample, which for gold is face
centered cubic, the rows of atoms block or interrupt some of the
scattered ions in a manner analogous to an object interrupting a
light beam to produce a shadow. This results in the scattered ions,
neutralized ions and other particles being scattered in a pattern
of varying density wherein some of the particles are blocked. Thus,
the scattered particles impinge fluorescent screen 230 which
results in a visual pattern which is a projection of the
crystalline structure of the sample.
If desired, the visual ion blocking pattern can be used as a means
for identifying crystalline surfaces. For example, it is possible
to utilize a computer to determine calculated ion blocking patterns
by means of a mathematical model. Known output devices can be used
to plot the calculated ion blocking pattern. By comparing the
calculated ion blocking pattern to the observed ion blocking
patterns, a crystalline identification process or technique can be
obtained.
If the sample to be observed on the fluorescent screen 230 of the
apparatus of FIG. 3 is an insulating material, the secondary
electrons produced in bored member 100 are accelerated to any
positive surface charge on the insulating surface to eliminate the
build up of positive surface charge on the insulating material. By
reducing the build up of positive surface charges, the low-energy
ion beam is not repelled by charges on the surface of the
insulating material and thereby permits ions to scatter from the
surface of the insulating material and to produce an ion blocking
pattern of the atomic structure of the insulating material on the
fluorescent screen 230. This clearly is an unexpected and novel
result in that the patterns produced by scattering of low-energy
ions are not a function of electrical conductivity of the
samples.
FIG. 5. is a schematic diagram illustrating control circuitry for
automatic operation of the apparatus of FIG. 3. The apparatus is
energized from a conventional alternating current source by means
of a plug member 300 which when energized from the alternating
current source and when a main switch 302 is in its ON position
energizes a master relay 304. Relay 304 energizes a cooling fan 306
and a main control relay 308. The control relay 308 in turn is
operatively coupled to vacuum gauges located within the sample
support chamber 206 and performs the function of automatically
controlling the vacuum pumping within the sample support vacuum
chamber 206 to obtain the desired vacuum in the order of
10.sup.-.sup.5 Torr. The control relay 308 controls in a
predetermined sequence operation of various valves as the desired
vacuum is obtained in the sample support vacuum chamber 206. Also,
if it is desired to vent the sample support vacuum chamber 206 to
atmosphere for addition of various samples, the control relay 308
selectively controls the rate at which venting occurs by means of
relays, generally designated as 312. Vacuum and pressure
indications are displayed on the control panel of the apparatus of
FIG. 3 by indicating means 314. The portion of the cycle for both
pumping the vacuum and venting of the vacuum is indicated by a
cycle indicator, generally designated as 316. In this manner, the
entire operation as to pumping the sample support chamber 206 to an
appropriate vacuum and the venting thereof to permit easy and quick
insertion of the samples for subsequent generation of its ion
blocking pattern is completely under control of the automatic
vacuum circuit. In this manner, misoperation or interruption of the
operation during the time the vacuum is ON can be precisely
controlled.
In addition to the aforementioned embodiment in which the blocking
pattern is sensed by viewing the projected pattern produced by
scattered ions impinging a fluorescent means, another means of
sensing this pattern may be employed with this invention. For
example, a screen array which channels secondary emission of
electrons upon bombardment of ions and other particles can be
positioned to be impinged upon by the scattered ions. Used with the
said aforementioned embodiment, the array can be positioned between
the solid surface 110 and the fluorescent means 120. Such a screen
array is described in the articles "The Channel Electron
Multiplier, A New Radiation Detector," by J. Adams and B. W.
Manley, which appeared in the 1967 Philips Technical Review, Vol.
28, page 156, and "Electron Multipliers Utilizing Continuous Strip
Surfaces," by W. C. Wiley and C. F. Hendee, which appeared in the
1962 Proceedings of the IEEE, Transaction of Nuclear Science, Vol.
9, page 103. With this screen array so positioned, the blocking
pattern defined by the scattered ions impinging thereupon can be
transformed into an electron emission defining the blocking
pattern. Such secondary electrons can then be accelerated to
impinge a fluorescent means. Upon such electron emission impinging
the fluorescent means, the blocking pattern can be visualized.
By interposing such a screen array between the sample from which
ions are scattered and the fluorescent means, there can be also
provided means which appreciably retard the relatively rapid
deterioration of the fluorescent means caused by impingement of the
ions and like particles conveying the intelligence to be discerned
and to retard contamination of the fluorescent means by deposition
of atoms sputtered thereon.
This screen array can be prepared to impart a high gain to the
intensity of the bombardment, thereby providing a sensing means of
higher sensitivity. As a result, a lower primary ion current
density beam can be used to scatter the ions from the sample.
Another alternative embodiment for sensing the ion blocking pattern
comprises scanning the projected pattern with a single channel
electron multiplier. The output signal from such scanning means can
be fed into a suitable display device such as a recorder or an
oscilloscope.
* * * * *