U.S. patent number 3,906,889 [Application Number 05/325,740] was granted by the patent office on 1975-09-23 for crystal growing apparatus.
This patent grant is currently assigned to Hitachi, Ltd.. Invention is credited to Tadao Kaneko, Itiro Omura.
United States Patent |
3,906,889 |
Omura , et al. |
September 23, 1975 |
Crystal growing apparatus
Abstract
A crystal growing apparatus comprises a Knudsen cell source of
the surface ionization type, focusing means to focus, on a crystal
substrate, an ion beam emitted from the ion source, deflection
means to deflect the ion beam, detection means to detect the
quantity of the ion beam, an electron gun to generate an electron
beam which neutralizes ions focused on the crystal substrate, and a
quadrupole mass filter to evaluate the ratio of partial pressure of
the neutralized molecules within a vacuum specimen chamber in which
the crystal substrate exists, the ion beam being scanned on the
substrate by the deflection means.
Inventors: |
Omura; Itiro (Hino,
JA), Kaneko; Tadao (Oome, JA) |
Assignee: |
Hitachi, Ltd.
(JA)
|
Family
ID: |
11670619 |
Appl.
No.: |
05/325,740 |
Filed: |
January 22, 1973 |
Foreign Application Priority Data
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|
|
|
Jan 21, 1972 [JA] |
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47-7612 |
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Current U.S.
Class: |
118/666; 118/715;
250/281; 118/690; 118/720 |
Current CPC
Class: |
C30B
23/06 (20130101) |
Current International
Class: |
C30B
23/02 (20060101); C30B 23/06 (20060101); C23C
013/12 () |
Field of
Search: |
;250/292,284,285,423,424,397 ;118/7,8,5,49.1,49.5 ;117/93.3 |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
IEEE Spectrum "The Application of Electron/Ion Beam Technology to
Micro Electronics," Brewer, G. R., (Jan. 1971), pp. 23-37..
|
Primary Examiner: Kaplan; Morris
Attorney, Agent or Firm: Craig & Antonelli
Claims
We claim:
1. A crystal growing apparatus comprising:
a vacuum chamber;
a crystal substrate located within said vacuum chamber to be
subjected to crystal growth;
a Knudsen cell source of the surface ionization type for
irradiating an ion beam onto said crystal substrate;
ion detector means for detecting the quantity of the ion beam
irradiated from said ion source;
focusing means for focusing said ion beam onto said crystal
substrate;
beam deflector means for scanning the focused ion beam on said
crystal substrate;
means for generating an electron beam for neutralizing said ion
beam on said crystal substrate;
detector means for detecting the ratio of the partial pressures of
the molecules within said vacuum chamber; and
signal generator means operatively connected to said ion detector
means and said detector means for detecting the ratio of partial
pressures for generating control signals for controlling the
crystal growth, in accordance with the output from said ion
detector means and the output from said detector means for
detecting the ratio of partial pressures,
whereby said crystal is so grown as to have a two-dimensional
distribution of concentrations of the molecules by the scanning of
said ion beam on said crystal substrate.
2. An apparatus as defined in claim 1, further comprising molecular
beam-generating means to further irradiate a neutral molecular beam
onto said crystal substrate, whereby the crystal growth is
accelerated.
3. A crystal growing apparatus comprising:
a vacuum chamber;
a crystal substrate located within said vacuum chamber to be
subjected to crystal growth;
a Knudsen cell source of the surface ionization type consisting of
a plurality of cells and for irradiating a plurality of ion beams
onto said crystal substrate;
first ion detector means for detecting the quantity of ions of each
of said plurality of ion beams;
focusing means for focusing said ion beams onto said crystal
substrate;
beam deflector means for scanning the focused ion beam on said
crystal substrate;
second ion detector means for detecting the total quantity of ions
of said plurality of ion beams;
means for generating an electron beam for neutralizing said focused
ion beam on said crystal substrate;
detector means for detecting the ratio of the partial pressures of
the molecules within said vacuum chamber;
means for receiving the outputs from said first and second ion
detector means and for evaluating the ratio between said total
quantity of ions and said quantity of ions of said each ion beam;
and
signal generator means operatively connected to said means for
evaluating the ratio between said total quantity of ions and said
quantity of ions of said each ion beam and said detector means for
detecting the ratio of the partial pressures for generating control
signals for controlling the crystal growth, in accordance with the
output from said means for evaluating the ratio between the
quantities of ions and an output from said detector means for
detecting the ratio of partial pressures,
whereby the crystal is so grown as to have a two-dimensional
distribution of concentrations of the molecules by the scanning of
said focused ion beam.
4. An apparatus as defined in claim 3, further comprising molecular
beam-generating means to further irradiate a neutral molecular beam
onto said crystal substrate, whereby the crystal growth is
accelerated.
5. An apparatus as defined in claim 3, further comprising display
means receiving as its input, the output from said means for
evaluating the ratio between the quantities of ions, the output of
said display means being swept in synchronism with the scanning of
said focused ion beam by said beam deflector means.
6. A crystal growing apparatus comprising:
a vacuum chamber within which a crystal substrate to be grown may
be disposed;
first means for irradiating a crystal substrate disposed within
said chamber with particles of opposite charge by at least one ion
beam;
second means, coupled to said first means, for detecting the
magnitude of said at least one ion beam;
third means, coupled to said chamber, for detecting the ratio of
the partial pressures of molecules within said chamber; and
fourth means, coupled to said second and third means, for
controlling the irradiation of said at least one ion beam by said
first means in accordance with the outputs of said second and third
means, whereby a resulting neutralized particle is grown upon the
surface of said substrate.
7. An apparatus according to claim 6, wherein said first means
further includes means for focusing said at least one ion beam onto
said substrate and for scanning the focused ion beam on said
crystal substrate.
8. An apparatus according to claim 6, wherein said first means
comprises means for irradiating said substrate with a plurality of
ion beams.
9. An apparatus according to claim 8, wherein said second means
detect the respective magnitudes of each of said ion beams of said
plurality, and said apparatus further comprises fifth means for
detecting the total quantity of ions of said plurality of beams,
and
sixth means, coupled to the outputs of said second and fifth means,
for providing a signal representative of the ratio between said
total quantity of ions and the quantity of ions of each ion
beam,
wherein said fourth means is coupled to said third and sixth means
for controlling the irradiation of said ion beams by said first
means in accordance with the outputs of said third and sixth
means.
10. An apparatus according to claim 6, wherein said first means for
irradiating said crystal substrate commprises a Knudsen cell source
of the surface ionization type having a plurality of cells therein
for irradiating said substrate with a plurality of ion beams.
11. An apparatus according to claim 7, further comprising display
means, responsive to the output of said second means, and being
synchronized with said scanning means, for displaying the output of
said second means, whereby the ion beam concentration can be
observed.
12. An apparatus according to claim 6, further comprising means
responsive to the output of said fourth means, for controlling the
temperature of said crystal substrate.
13. An apparatus according to claim 6, further comprising seventh
means, coupled to said first and fourth means, for controlling the
quantity of said at least one ion beam, and
eighth means, coupled to said crystal substrate and said fourth
means, for controlling the temperature of said substrate,
wherein said fourth means applies a signal to at least one of said
seventh and eighth means as a function of the outputs of said
second and third means such that crystal growth on said substrate
proceeds in accordance with the crystal growth conditions of
quantity of said at least one ion beam and temperature of said
substrate.
14. An apparatus according to claim 9, further comprising seventh
means, coupled to said first and fourth means, for controlling the
quantity of said plurality of ion beams, and
eighth means, coupled to said crystal substrate and said fourth
means, for controlling the temperature of said substrate,
wherein said fourth means applies a signal to at least one of said
seventh and eighth means as a function of the outputs of said third
and sixth means such that crystal growth on said substrate proceeds
in accordance with the crystal growth conditions of quantity of
said plurality of ion beams and temperature of said substrate.
15. An apparatus according to claim 9, wherein said first means
further includes means for focusing said ion beams onto said
crystal substrate scanning for acanning said focused beams in said
crystal substrate.
16. An apparatus according to claim 6, said first means further
includes means for accelerating crystal growth of said substrate by
irradiating said substrate with a neutral molecular beam.
17. An apparatus according to claim 8, wherein said first means for
irradiating said crystal substrate with a plurality of ion beams
comprises a Knudsen cell source of the surface ionization type
having a plurality of cells therein.
18. An apparatus according to claim 15, further comprising eighth
means, responsive to the output of said sixth means, and being
synchronized with said scanning means, for displaying the output of
said sixth means, whereby the ion beam concentration can be
observed.
19. An apparatus according to claim 9, further comprising means
responsive to the output of said sixth means, for controlling the
temperature of said crystal substrate.
Description
BACKGROUND OF THE INVENTION
The present invention relates to a crystal growing apparatus, and
more particularly to an apparatus which can control crystal growth
two-dimensionally and precisely by scanning the surface of a
crystal with an ion beam.
DESCRIPTION OF THE PRIOR ART
Prior-art crystal growing apparatus conduct crystal growth by the
use of a molecular beam. However, where the surface of a crystal
substrate to be grown is irradiated during crystal growth by the
molecular beam, the following disadvantages are involved. The
quantity of molecules to be supplied to the crystal is controlled
only by the control of the temperature of the crystal substrate.
Moreover, growth cannot be so controlled as to form a
two-dimensional molecular concentration distribution in the
crystal.
SUMMARY OF THE INVENTION
An object of the present invention is to provide crystal growing
apparatus which can provide a two-dimensional concentration
distribution in a crystal.
Another object of the present invention is to provide a crystal
growing apparatus which can perform a precise crystal growth.
In order to accomplish such objects, the present invention employs
an ion beam, and deflects it to scan the surface of a crystal
substrate and to control the quantity of the ion beam itself,
thereby forming a two-dimensional concentration distribution in the
crystal to grow it.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic view showing the construction of a prior-art
crystal growing apparatus;
FIGS. 2a and 2b are schematic views for explaining the subject
matter of the present invention, respectively;
FIG. 3 is a schematic view showing the construction of an
embodiment of crystal growing apparatus according to the present
invention; and
FIG. 4 is a block diagram showing a control unit suitable for the
crystal growing appratus according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to the accompanying drawings, the present invention
will be described hereunder in comparison with an example of prior
art.
FIG. 1 is a view shows prior-art crystal growing apparatus using
neutral molecular beams. In the figure, numeral 1 designates a
vacuum chamber in which crystal growth is carried out, 2 Knudsen
cells (in the illustrated case, two cells) used as a molecular beam
source, 3 a crystal substrate to be grown, 4 mass analyzing means
(for example, a quadrupole mass filter) for evaluating the ratio of
partial pressures within the vacuum chamber 1, and 5 an electron
gun. Neutral molecular beams emitted from the Knudsen cells 2 are
caused to fall on the crystal substrate 3, to grow a single crystal
on the substrate 3. It is a common practice in this case that,
using an electron beam e generated from the electron gun 5,
electron-diffraction patterns of the growing crystal are
sequentially observed on a fluorescent screen 6. The control of the
crystal growth is effected by a temperature control for the
substrate 3. The ratio of partial pressures of the molecules within
the vacuum chamber 1 is therefore evaluated by the mass analyzing
means 4. In order that the ratio of partial pressure and the
crystal growth may hold a predetermined relation, the temperature
of the substrate 3 is suitably controlled in response to the
magnitude of the ratio of partial pressure. Heating means is
omitted from the illustration.
In accordance with such prior-art apparatus, although the crystal
growth depends severely on the temperature of the substrate, the
quantity of the molecular beams, etc., an extremely thin (for
example, in the order of 100 A) multi-layer film can be
produced.
Since, however, the prior-art crystal growing apparatus uses
neutral molecular beams, it has disadvantages as stated below. The
use of the neutral molecular beams makes it impossible to form a
two-dimensional molecular concentration distribution on the
substrate. Further, the control of the crystal growth is performed
only with the substrate temperature. More specificially, the ratio
of partial pressure as evaluated by the mass analyzing means is
based on those molecules among the total neutral molecular beams
being supplied to the substrate which are not absorbed on the
substrate, in other words, the quantity of the molecules absorbed
on the substrate. The control of the crystal growth with only
changes in the quantity of the molecules does not provide a precise
control.
In view of such problems, the present invention employs a Knudsen
cell source of the surface ionization type in order to generate ion
beams, and effects crystal growth with the ion beams.
Here, the Knudsen cell source of the surface ionization type is an
ion source which has hitherto been well known. When the atoms are
passed through a tungsten porous material, they are ionized
according to the Saha-Langmuir's equation at their departure from
the surface of the material.
The Knudsen cell source of the surface ionization type is at a
temperture of approximately 1,000.degree.C and can efficiently
generate ions by increasing the porosity of the tungsten
material.
In conformity with the Saha-Langmuir's equation, one of the most
important factors for the probability of surface ionization is the
relation between the ionization potential of the specimen atom and
the work function of the porous material. Where the work function
of the employed material is about 5.5 eV, about 50% of the atoms
which come into contact with the material are ionized as for indium
(In) whose ionization potential is 5.79 eV. About 1 to 50% of atoms
are ionized, as for an element whose ionization potential is
approximately 10 eV. In accordance with these quantitative
calculations, ion beams of 10.sup.10 atoms/sec-cm.sup.2, as
required on the substrate for the crystal growth, can be
sufficiently obtained.
FIGS. 2a and 2b are views for explaining the subject matter of the
present invention which makes use of the Knudsen cell source of the
surface ionization type. Referring to FIG. 2a, ion beams from the
Knudsen cell 7 source of the surface ionization type pass through
focusing electrostatic lenses 8, and are focused on a substrate 3.
While, in the illustration, the Knudsen cell source of the surface
ionization type consists of two cells, it may be similarly composed
of a single cell. The case of using a plurality of cells, however,
is advantageous in that the control of the crystal growth is more
precise.
The magnitude of the ion beams is detected by means of mesh
electrodes and ion detectors 9 which are arranged between the
focusing electrostatic lines 8 and the substrate 3. On the other
hand, the ion beams focused on the substrate 3 are neutralized by
the interaction with low energy-electron rays emanating from an
electron gun 11.
As a result, the crystal based on the neutral molecular beams is
grown on the substrate 3. Further, if necessary, the growing
process is successively observed in such way that
electron-diffraction patterns of the crystal by high
energy-electron rays emanating from an electron gun 5 are formed on
a fluorescent screen 6.
FIG. 2b is a view for explaining the state in which the ion beam is
scanned on the crystal by a deflecting electrode. The ion beam
ejected from the Knudsen cell source 7 of the surface ionization
type is focused by the focusing electrostatic lens 8, to reach the
surface of the substrate 3. The ion beam having reached the
substrate 3 scans the surface of the substrate 3 as, for example,
shown by dotted lines in the figure by virtue of the deflecting
electrode 10. In this case, the scanning speed is freely changed,
whereby the distributed state of a multi-layer film gradually
growing on the substrate 3 can be varied as desired.
FIG. 3 is a schematic view showing the construction of an
embodiment of the present invention. The same symbols as in FIGS.
2a and 2b represent the same or equivalent parts. The Knudsen cell
source of the surface ionization type 7 consists of three cells.
Reference numerals 1 and 4 designate the same vacuum chamber and
mass analyzing means as illustrated in FIG. 1, respectively.
Numeral 12 indicates a total ion beam detector by which, in case of
utilizing a plurality of ion source cells, an ion beam with the
respective ion beams focused into a single one is detected.
With such a construction, specimen atom ions ejected from the
Knudsen cell source of the surface ionization type 7 are focused on
the substrate 3 by the focusing electrostatic lens 8.
Simultaneously therewith, ion beams generated from the cells of the
Knudsen ion source of the surface ionization type are respectively
detected by the ion detectors 9-1, 9-2 and 9-3. The total quantity
of the ion beams is detected by the total ion beam detector 12. A
signal from the total ion beam detector 12 is fed back to the
electron gun 11, to control the magnitude of an electron beams so
as to neutralize the ion beam on the substrate 3 by the electron
beam. Thus, the phenomenon in which the surface of the crystal
growing on the substrate 3 is charged is perfectly eliminated.
The ion beam can scan the surface of the substrate 3 by varying the
drive voltage of the deflecting electrode 10. The scanning can be
made by signals, such as saw-tooth waves, introduced from
deflection voltage-supplying means (not shown). On the other hand,
signals from the ion detectors 9-1, 9-2 and 9-3 are compared with
the signal from the total ion beam detector 12 (no comparator being
shown) so as to evaluate the proportions occupied by the ions of
the individual beams relative to the total ions. Simultaneously
therewith, the ratio of partial pressure of molecules within the
vacuum vessel or specimen chamber 1 is detected by the mass
analyzing means, for example, a quadrupole mass filter 4.
In this way, according to the present invention, a two-dimensional
concentration distribution of the molecules can be formed in
addition to the three-dimensional growth of the crystal in the
process of the crystal growth by the scanning of the ion beam.
Furthermore, according to the present invention, both the ratio of
partial pressure and the proportions occupied by the quantities of
the ions of the individual beams (where the Knudsen cell source of
the surface ionization type consists of a single cell, the quantity
of the ions from the single ion cell corresponds to the above
proportions) are produced as output signals. Using the output
signals, a precise control for the crystal growth may be made in
such a way that the output signals of both the quantities and the
substrate temperature as well as the ionic amount are calibrated
beforehand, or that the electron-diffraction patterns are
observed.
More specifically, let it now be supposed that the ratio of partial
pressure of the molecules within the vacuum chamber 1 has changed.
Then, it can be known whether the change is attributable to a
change in the coefficient of absorption of the substrate 3 due to a
change in the temperature of the substrate 3, or it is attributable
to a change in the quantity of the ejected ion beam from the
Knudsen cell source of the surface ionization type 7. Therefore,
the temperature of the substrate and/or the quantity of the ejected
ion beam from the ion source may be appropriately controlled so as
to effect the desired crystal growth. In order to control the
temperature of the substrate, the heating temperature of a heater
may be increased or decreased, while in order to control the
quantity of ions ejected from the ion source, the tungsten porosity
of the Knudsen cell source of the surface ionization type may be
increased or decreased.
FIG. 4 is a block diagram of a control unit which, using both the
proportions occupied by the quantities of the ions and the ratio of
partial pressure as control signals, controls the quantities of the
ions and the temperature of the crystal substrate in the apparatus
of the embodiment shown in FIG. 3. In FIG. 4, the same symbols as
in FIG. 3 indicate the same or equivalent parts. Reference numeral
13 designates a comparator which compares outputs from the ion
detector 9 and the total ion detector 12. A computing device 14
receives, as its inputs, an output from the comparator 13 and an
output from the quadrupole mass filter 4 (the ratio of partial
pressure as referred to above), and generation a control signal for
controlling the quantity of emission of the ions or the temperature
of the substrate, namely, for controlling the crystal growth. A
deflecting voltage-generator 15 generates a deflection voltage
(saw-tooth wave voltage) for the deflecting electrode 10. Numerals
17 and 18 represent an ion beam-controller (for example, a current
amplifier) and a substrate temperture-controller (for example, a
current amplifier), respectively, each of which receives as its
input an output from the computing device 14. Shown at 19 is a
memory means. Display means 20 is composed of, for example, a Braun
tube and displays the concentration of the ion beam. Numeral 21
indicates a heater for heating the crystal substrate 3.
With such a construction, the ion beams generated from the Knudsen
cell source of the surface ionization type 7 are respectively
detected by the ion detector 9. Each output of the detector 9 is
one of the inputs of the comparator 13. The focused ion beam is
detected by the total ion beam detector 12, whose output is the
other input of the comparator 13 and a control signal for the
electron gun 11. The electron gun 11 has its grid potential
controlled by the control signal from the total ion beam detector
12, and generates an electron beam sufficient for the total ion
beam to be neutralized on the crystal substrate 3. Since the
deflecting electrode 10 has the saw-tooth wave voltage applied
thereto from the deflection voltage-generator 15, the ion beam
having passed through the focusing electrode means 10 is scanned on
the crystal substrate 3. On the one hand, since the outputs from
the total ion detector 12 and the ion detector 9 are applied to the
comparator 13, the proportions occupied by the ions of the
individual beams with respect to the total ions are evaluated
therein. One of the output signals indicating the proportion is one
of the inputs to the computing device 14, while the other output
signal is an input to display means 20. On the other hand, a change
in the ratio of partial pressures within the vacuum chamber 1 is
evaluated by the mass analyzing means 4. The output of the mass
analyzing means 4 is the other input of the computing device 14.
The computing device 14 calculates, from the ratio of partial
pressures of the molecules wiithin the vacuum chamber 1 and the
ratio of the quantity of each ion beam to the quantity of all the
ion beams, whether a change in, for example, the ratio of partial
pressures is due to a change in the temperature of the substrate or
due to a change in the quantity of the ion beam ejected from the
Knudsen cell source of the surface ionization type 7. In dependence
on the calculated result, the output of the computing device 14
becomes the control signal to the ion beam-controller 17 and/or the
substrate temperature-control means 18, and is applied thereto. In
consequence, an output signal from the ion beam-controller 17 or
from the substrate temperature-control means 18 adjusts the
quantity of the emitted ion beam from the Knudsen cell source of
the surface ionization type 7 or the output of the heater 21,
accordingly, the temperature of the crystal substrate. As stated
above, the output of the comparator 13 is applied to display means
20. It is, therefore, possible that the ratio of the quantity of
the emitted ions of each beam to the total quantity of the emitted
ions, namely, the ion beam concentration is displayed by sweeping
the applied output signals with the saw-tooth wave voltage from the
deflection voltage-generating means 15. Thus, the ion beam
concentration can be observed while the crystal is being grown.
Further, the sequence of radiation of the radiated ion beams
effecting the crystal growth, the kinds of ions constituting the
beams, etc. are stored in the memory means 19. The crystal growth
is carried out with the deflection voltage-generating means 15 and
the computing device 14 controlled by outputs from the memory means
19. Then, any desired multi-layer film can be manufactured.
Although, in the above description, the employment of a plurality
of Knudsen ion source cells of the surface ionization type has been
stated, it is a matter of course that the crystal growth can also
be controlled in case where the Knudsen cell source of the surface
ionization type consists of a single cell. In this case of the
single cell, the total ion beam detector 12 shown in FIG. 4 is
unnecessary. In the computing device 14, the quantity of the ion
beam from the Knudsen cell source of the surface ionization type
and the ratio of partial pressure fed from the quadrupole mass
filter 4 are merely compared and operated, to calculate the control
output to be applied to the ion beam-controller 17 and the
temperature control means 18.
In the foregoing explanation, description has been made of the
crystal growing apparatus which employs only the Knudsen cell
source of the surface ionization type. Needless to say, however, in
case where the scanning by the deflection is not required, for
example, where a single crystal or the like is merely grown on the
substrate, a Knudsen cell can be used jointly with the Knudsen cell
source of the surface ionization type. In this case, the
three-dimensional growth of the crystal is promoted by neutral
molecular beams.
In the above explanation, the control of the quantity of the
emitting ion beams of the Knudsen cell source of the surface
ionization type has been stated as being conducted by the use of
the analyzed result obtained from the mass filter and the detected
results obtained from the ion detector means and the total ion
detector means. However, where the requested precision of the
control for the ion source is not very severe, the analyzed result
need not be used. In this case, the arithmetic unit 14 shown in
FIG. 4 performs operations on condition that the temperature of the
substrate 3 is invariable.
As described above in detail, according to the present invention,
two-dimensional of three-dimensional control of crystal growth as
has hitherto been impossible becomes possible by employing ion
beams. Simultaneously therewith, the control of crystal growth,
more precise than has heretofore been possible, becomes possible by
making use of the ratio between the total emitted ion beam and each
ion beam and the ratio of partial pressure of molecules floating
within a specimen chamber and not absorbed on a crystal substrate,
or by making use of the quantity of an emitted ion beam and the
ratio of partial pressure of the molecules.
* * * * *