U.S. patent number 3,878,392 [Application Number 05/425,457] was granted by the patent office on 1975-04-15 for specimen analysis with ion and electrom beams.
This patent grant is currently assigned to Etec Corporation. Invention is credited to Wyman C. Lane, Nelson C. Yew.
United States Patent |
3,878,392 |
Yew , et al. |
April 15, 1975 |
Specimen analysis with ion and electrom beams
Abstract
A method and apparatus employing ion and electron beams for
chemically analyzing a specimen. A specimen is mounted on a movable
platform in an evacuated chamber and irradiated with an ion beam
over a predetermined area of interest to liberate secondary ions.
The secondary ion spectrum is analyzed with a mass filter and
display unit to provide a spectral distribution. Ions having a
particular mass-to-charge ratio are selected for spatial
distribution analysis and the mass filter is tuned to the selected
mass-to-charge ratio. The filtered beam of secondary ions passed
through the mass filter is detected by an ion detector which
generates a signal representative of secondary ion abundance at
that mass-to-charge ratio. The ion detector output signals are used
to control the intensity or deflection of a CRT beam. An
independently generated electron beam is scanned over the specimen
area irradiated by the ion beam and the CRT beam is swept in
synchronism with the scanned electron beam. The electron beam,
scanned over the ion irradiated specimen area, modulates the
secondary ion yield at the point where both the electron beam and
the ion beam are coincident on the specimen. The resulting display
is a two dimensional spatial distribution map of the species in the
specimen to which the mass filter is tuned.
Inventors: |
Yew; Nelson C. (Hillsborough,
CA), Lane; Wyman C. (Fremont, CA) |
Assignee: |
Etec Corporation (Hayward,
CA)
|
Family
ID: |
23686655 |
Appl.
No.: |
05/425,457 |
Filed: |
December 17, 1973 |
Current U.S.
Class: |
250/306; 250/307;
250/309; 250/310 |
Current CPC
Class: |
H01J
37/256 (20130101); G01N 23/225 (20130101) |
Current International
Class: |
H01J
37/252 (20060101); H01J 37/256 (20060101); G01N
23/225 (20060101); G01N 23/22 (20060101); G01n
021/26 (); G01n 023/12 () |
Field of
Search: |
;250/306-311 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Smith; Alfred E.
Assistant Examiner: Chatmon, Jr.; Saxfield
Attorney, Agent or Firm: Townsend and Townsend
Claims
What is claimed is:
1. A method of analyzing a specimen for elemental constituents
comprising the steps of:
a. directing a beam of primary ions to a target area of said
specimen to produce secondary ions;
b. scanning said irradiated target area with an electron beam;
and
c. detecting the variation of secondary ion current with position
of said electron beam.
2. The method of claim 1 further including the step of filtering
said secondary ions to permit detection of secondary ions having
substantially the same preselected mass-to-charge ratio.
3. The method of claim 1 wherein said step (c) of detecting
includes the steps of:
i. synchronously scanning said electron beam and the imaging beam
of a cathode ray tube; and
ii. modulating said CRT beam in accordance with said variation of
said secondary ion current.
4. The method of claim 1 wherein said step (b) of scanning is
preceded by the step of determining the spectral distribution in
mass-to-charge ratios of said secondary ions emanating from said
irradiated target area.
5. The method of claim 4 wherein said step of determining includes
the steps of:
i. sweep filtering said secondary ions to permit detection of ions
having varying mass-to-charge ratios;
ii. scanning the imaging beam of a cathode ray tube synchronously
with said step of sweep-filtering;
iii. detecting the variation of said secondary ion current with
mass-to-charge ratio; and
iv. modulating said cathode ray tube beam in accordance with said
variation of said secondary ion current.
6. The method of providing a spatial distribution plot of
constituent elements of a specimen comprising:
a. generating a beam of primary ions;
b. irradiating a target area with said beam of primary ions to
liberate secondary ions from said target area;
c. generating beam position signals;
d. scanning said irradiated target area with an electron beam in
accordance with said beam position signals;
e. scanning a recording element with said beam position signals in
synchronism with said electron beam scanning;
f. generating control signals representative of the variation of
secondary ion current with position of said electron beam relative
to said target area; and
g. applying said control signals to said recording element to
record said variations.
7. The method of claim 6 wherein said step (f) of generating
includes the step of passing said secondary ions through a mass
filter tuned to reject substantially all secondary ions hot having
a preselected mass-to-charge ratio so that only control signals
representative of the variation of secondary ions having said
preselected mass-to-charge ratio are generated.
8. A system for analyzing a specimen for elemental constituents
comprising:
means for directing a beam of primary ions onto a target area of
said specimen to produce secondary ions;
means for scanning said irradiated target area with an electron
beam; and
means for detecting the variation of secondary ion current with
position of said electron beam.
9. The system of claim 8 wherein said detecting means includes
filter means for preventing detection of secondary ions not having
a preselected mass-to-charge ratio.
10. The system of claim 8 wherein said detecting means includes
means for synchronously scanning said electron beam and a recording
element and means for modulating said recording element in
accordance with said variation of said secondary ion current.
11. The system of claim 8 further including means for determining
the spectral distribution in mass-to-charge ratios of said
secondary ions liberated from said irradiated target area.
12. The system of claim 11 wherein said spectral distribution
determining means includes:
means for sweep filtering said ions to permit detection of ions
having varying mass-to-charge ratios;
means for scanning said recording element synchronously with said
sweep filtering means;
means for detecting the variation of secondary ion current with
mass-to-charge ratio; and
means for modulating said recording element in accordance with said
variation of said secondary ion current.
Description
BACKGROUND OF THE INVENTION
This invention relates to specimen analysis by means of beams of
charged particles. More particularly, this invention relates to an
improved technique for investigating the chemical composition of a
specimen by secondary ion analysis.
Chemical analysis of a specimen using the technique of secondary
ion emission is known. In a typical arrangement, e.g., that
disclosed a U.S. Pat. No. 3,517,191 to Liebl issued Jan. 23, 1970,
a specimen to be investigated is placed on a platform and bombarded
with a primary beam of ions from a suitable ion source. The primary
beam is scanned in raster-like fashion over the entire area of
interest. The interaction of the bombarding beam with each
elemental area of the specimen results in the ejection of secondary
ions characteristic of the chemical composition of the specimen in
that area. These secondary ions are collected and filtered by means
of a mass analyzer which permits only ions having a specific
mass-to-charge ratio to be transmitted therethrough. The filtered
secondary ions encounter an ion detector which provides an output
signal whose magnitude is representative of the intensity of the
ion beam incident thereto. This output signal is typically used to
control the intensity of a cathode ray tube, or CRT, scanning beam
which is scanned in synchronism with the ion beam. The resulting
display on the face of the CRT thus provides a spatial distribution
plot of ion density as a function of location on the specimen.
While this conventional technique has been found to provide useful
results in some applications, it suffers from several
disadvantages. For example, the spatial resolution of the chemical
specimen constituents is a function of the fineness of the primary
ion beam. The degree of resolution of the primary ion beam is
directly dependent upon the complexity and size of the beam
generation ion optics and deflection circuitry. In general, the
finer the resolution desired, the more complicated, cumbersome and
costly the ion optics and circuitry must be. In actuality, the cost
of specimen analysis increases inordinately with the fineness of
the resolution desired and, in many cases, is so great as to render
the gathering of much-needed data economically prohibitive.
A further disadvantage inherent in known ion beam analysis
techniques is the lower limit of resolution. The minimum primary
ion beam diameter practically obtainable with known systems is
about 1 micron. Thus, where a finer resolution than that obtainable
with this lower limit is required, ion beam analysis cannot furnish
meaningful data and other techniques must be employed, usually with
less satisfactory results.
Efforts to overcome these and other disadvantages inherent in known
secondary ion analysis techniques have not met with wide success to
date.
SUMMARY OF THE INVENTION
The invention comprises a method and apparatus for providing a
spatial map of secondary ion emission which provides a resolution
which is substantially finer than that hitherto obtainable. In the
preferred embodiment, a beam of primary ions from a source is
directed onto the surface of a specimen, with the primary ion beam
covering the entire area of interest. An electron beam from an
electron-optical column is line scanned over the same area to
interact with the secondary ions liberated from the specimen area
by the primary ion beam. The secondary ions are passed through a
mass filter tuned to ions of a preselected mass-to-charge ratio,
and the ions transmitted therethrough are detected by an ion
detector, the output of which is used to control the intensity or
deflection of the beam of a CRT display. The CRT beam is scanned
synchronously with the electron beam to provide a spatial
distribution map of secondary ion intensity as a function of
electron beam position.
As the electron beam scans those regions of the specimen which
contain unconcentrated amounts of the element corresponding to the
preselected secondary ions, a substantially constant background
level of secondary ion current is produced which is attributable to
the steady state emission of secondary ions from the total area
irradiated by the primary beam. However, as the electron beam scans
those regions of the specimen containing concentrations of the same
element, a pronounced modulation in secondary ion current is
produced. The resulting spatial distribution map exhibits regions
of markedly different intensity corresponding to those portions of
the specimen containing concentrations of the species under
investigation. By tuning the mass filter to secondary ions having
different mass-to-charge ratios, both qualitative and quantitative
data relating to several different elements may be obtained from
the same or different specimens. Since the spatial resolution of
the resulting distribution map is dependent upon the size of the
scanned electron beam, which is typically two orders of magnitude
smaller than the smallest obtainable ion beam, maps exhibiting an
extremely fine resolution are obtained with the invention.
For a fuller understanding of the nature and advantages of the
invention, reference should be had to the ensuing detailed
description taken in conjunction with the accompanying
drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagramatic view of a preferred embodiment of a system
constructed according to the invention;
FIG. 2 is a schematic diagram illustration the distribution
frequency of elements of a specimen; and
FIG. 3 is a schematic diagram illustrating the principle of the
invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Turning now to the drawings, FIG. 1 illustrates a preferred
embodiment of a system constructed according to the invention. A
housing 10 shown partly broken away provides a main specimen
chamber 11 which can be evacuated by means of a vacuum pump 12 and
valved conduit 13. Mounted within chamber 11 is a specimen platform
14, commonly termed a stage, which provides a support surface for a
specimen 15 to be investigated. Stage 14 is provided with suitable
mechanical connections indicated by broken lines 16-20 for enabling
independent movement of stage 14 in the x, y, and z directions, and
tilting and rotation of stage 14 about the x-y plane and the z
axis, respectively, in response to the manipulation of control
elements 21-25. Elements 16-25 may comprise any suitable known
mechanical arrangement for imparting the desired motion to stage
14. Since several such arrangements are known, details thereof have
been omitted for clarity.
Mounted within chamber 11 is a source of primary ions 26, which may
comprise a duo plasmatron ion source, a diode source, an RF source,
or the like. Ion beam source 26 is powered by a conventional ion
gun power supply 27 which provides beam generation, focusing and
alignment control signals. Ion gun 26 is so arranged in chamber 11
that the beam of primary ions 28 generated by gun 26 is emitted an
an angle .alpha. between the beam axis and the x-y reference plane.
If desired, ion gun 26 may be provided with a suitable mechanical
arrangement for adjusting the angle .alpha..
The optimum value for the angle a depends primarily on the primary
ion beam energy, the nature of the specimen under investigation and
the type of analysis desired, and can best be determined on an
empirical basis for a given application. In general, shallow angles
are preferred to a minimum of about 10.degree., although values of
a up to a limit of about 85.degree. can provide good results.
The nature of the primary ion beam used in practicing the invention
also depends upon the nature of the sample under investigation, the
desired ion beam energy and the type of analysis desired. Some
examples of suitable primary ion beams are argon, cesium, the
halogens, helium, nitrogen and oxygen. Other types will occur to
those skilled in the art.
Also mounted within chamber 11 is a conventional quadrupole mass
filter 33 powered by a mass filter control unit indicated by
reference numeral 34 which comprises a conventional RF generator 35
and DC power supply 36.
Mass filter 33 may be operated in two modes: a narrow filter mode
in which filter 33 is turned by the combination of control signals
from control unit 34 to transmit only ions having a given
mass-to-charge ratio, and a spectral mode in which the narrow
transmission window normally provided during narrow filter mode is
cyclically varied over a preselected range of mass-to-charge
ratios.
A secondary ion detector 38 which may be a conventional electron
multiplier, is mounted at the secondary ion beam output of mass
filter 33, and is powered by a conventional ion detector power
supply 39.
The output of ion detector 38 is coupled via an amplifier 40 to the
beam intensity control element 41 of a standard cathode ray tube 42
and also to fixed contact 43 of a switch 44. A conventional CRT
power supply 45 provides beam generator signals to CRT 42.
Mounted on housing 10 is a conventional electron-optical column 46
powered by a standard column control unit 47. Column control unit
47 provides beam generation, beam focusing and beam alignment
control signals to electron optical column 46.
A sweep generator 48 provides raster type beam deflection scanning
signals which are coupled to the deflection coils of
electron-optical column 46. The deflection scanning signals from
sweep generator 48 are also coupled to a first pair of contacts 51,
52 of a double-pole, double-throw switch 50. The alternate pair of
contacts 53, 54 are coupled to the output signals from RF generator
35 and the blade contact 55 of switch 44. As indicated by broken
line 56, blade 55 of switch 44 is mechanically linked to a pair of
moveable blades 57, 58 of switch 50 so that blade 55 closes when
blades 57, 58 are moved to the left-hand position of FIG. 1. Blades
57, 58 are coupled to the deflection control elements of CRT 42.
Thus, the deflection of the display beam of CRT 42 is alternately
controlled by sweep generator 48, and the output signals from RF
generator 35 and ion detector 38, depending on the position of
switch 50.
Preferably, the elements designated by reference numerals 10-14,
16-25, 42, 45, 46, 47 and 48 comprise conventional scanning
electron microscope (SEM) elements, such as those found in the
AUTOSCAN model Scanning Electron Microscope available from Etec
Corporation of Hayward, Calif. Since these elements, and the other
elements noted above as conventional, are all well-known, further
details thereof have been omitted to avoid prolixity.
In operation, a specimen 15 is mounted on stage 14 and maneuvered
to the desired target position by elements 16-25, after which
chamber 11 is evacuated by pump 12 and valve 13. Ion gun power
supply 27 is then activated to cause ion gun 26 to generate a beam
of primary ions 28 of the desired size and intensity. Mass filter
control unit 34 and ion detector power supply 39 are energized to
activate mass filter 33 and ion detector 38. CRT power supply 45 is
activated and switch 50 is placed in the left-hand position (not
illustrated).
Mass filter 33 is now operated in the spectral mode and the filter
control signals generated by RF generator 35 and the output signals
from ion detector 38 are coupled via switch contacts 43, 53, 54 and
blades 55, 57, 58 to the deflection elements of CRT 42 so that the
CRT beam is swept in the horizontal direction as a function of
mass-to-charge ratio and in the vertical direction as a function of
the beam intensity.
The resulting display shown in FIG. 2 is a spectral plot of
intensity vs. mass-to-charge ratio of the secondary ions emitted
from the area of specimen 15 subjected to the primary ion beam. The
location and the intensity of peaks 59 i give the relative
distribution of various species of elements or compounds in the
sample 15. From this display, a particular species of interest is
selected for spatial distribution analysis.
To begin the spatial distribution analysis, mass filter control
unit 34 is adjusted to operate mass filter 33 in the narrow filter
mode. In this mode only those ions, whether positive or negative,
having the preselected mass-to-charge ratio are permitted to pass
to ion detector 38. Switch 50 is next moved to the right-hand
position illustrated in FIG. 1 and synchronous beam scanning is
initiated by actuating sweep generator 48 and column control unit
47. Thus, in the spatial distribution mode, the electron beam
generated by electron-optical column 46 and the CRT beam
simultaneously scan the target area of interest and the CRT face,
respectively, while the output of secondary ion detector 38
modulates the intensity of the CRT beam.
FIG. 3 illustrates the variation of detected secondary ion current
with the electron beam position as the electron beam scans a line
element 60 of the specimen target area. In this figure, the portion
of specimen 15 subjected to the primary ion beam is indicated by
the closed path denoted by reference numeral 61. The shaded regions
denoted by reference numerals 62, 64 represent regions having a
concentration of the species of interest while the remaining
unshaded area bounded by 61 is devoid of such concentrations.
Assuming the electron beam is swept from left to right as viewed in
the figure, as the electron beam scans along line 60 from point a
to point b, the intensity of the secondary ion current is
substantially constant. As the electron beam crosses the boundary
of concentrated region 62 at point b of line 60, the intensity of
the detected secondary ion current rapidly decreases to a minimum
and remains at this minimum level until the beam emerges from
concentrated region 62 at point c of the line. As the electron beam
completes the sweep of line 60 from point c to point d, the level
of the secondary ion current increases to the original level and
remains substantially uniform.
As the electron beam scans along line 60 of the specimen, the CRT
beam is synchronously swept by sweep generator 48 along a
corresponding line 60 (FIG. 1) and modulated in intensity in
accordance with the output from ion detector 38 amplified by
amplifier 40. The result is a swept line element 60' whose
intensity varies as a function of the concentration of the species
of interest in the corresponding scanned line 60 of the specimen.
Thus, as the electron beam is rastered over the entire target area
of the specimen 15, CRT 42 displays a pictorial representation of
the target area, which exhibits those regions having a
concentration of the species under investigation as well-defined
dark regions 62', 64' on a lighter background. If desired, this
intensity variation may be reversed by providing an inverter at the
output of amplifier 40, so that regions 62, 64 appear light on a
dark background.
In the above discussed example, regions 62, 64 are assumed to have
a substantially uniform concentration of the particular species
under investigation. As will be apparent to those skilled in the
art, if the concentration is not uniform, the resulting display
will exhibit intensity variations in regions of concentration which
correspond identically to the variation in concentration over the
specimen target area.
Once the spatial distribution of the particular species of interest
has been obtained, mass filter 33 may be tuned to pass secondary
ions of a different mass-to-charge ratio and the process may be
repeated.
Since the resolution of spatial distribution maps obtained in
accordance with the invention is primarily a function of the
scanning electron beam size, extremely fine resolution on the order
of 100 Angstrom units can be obtained herewith. Further, since the
primary ion beam need only be focused to the maximum width of the
target area, typically on the order of 100 microns, extremely
simple and inexpensive primary ion beam generation and focussing
circuits can be employed without sacrificing the resolution of the
system.
While the above provides a complete disclosure of the preferred
embodiment of the invention, various modifications, alternate
constructions and equivalents may be employed without departing
from the true spirit and scope of the invention. For example, if
desired, mass filter 33 may be operated in a combined spectral and
narrow filter mode in which the narrow pass band of the filter is
shifted at a slow rate compared to the synchronous scanning rate of
the electron beam and the CRT beam to provide a composite image of
the spatial distribution of two or more species of interest.
Similarly, mass filter 33 may be operated in a discrete combined
spectral-narrow filter mode in which the narrow pass band of this
element is shifted discretely in accordance with the initially
obtained spectral plot of intensity versus mass-to-charge ratio of
the specimen under investigation, with the stepping rate being
substantially less than the scanning rate of the electron beam.
Further, if desired, the various analog data signals obtained with
the preferred embodiment, such as the sweep signals from mass
filter control unit 34 and sweep generator 48 and the intensity
control signals from ion detector 38 and amplifier 40 may be
converted to digital form and recorded or stored in a computer
memory for further quantitative and qualitative analysis.
Therefore, the above description and illustrations should not be
construed as limiting the scope of the invention which is defined
by the appended claims.
* * * * *