JPH11279746A - Vapor deposition device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enable vapor deposition even if a crucible holding a vapor depositing source is arranged above a sample. SOLUTION: This device is composed of a vapor depositing source chamber J1 arranged in a vacuum chamber 3 formed inside an outer wall 1 and formed by a wall member 13 in which vapor depositing ports 13a are formed, a sample S held at the outside of the vapor depositing source chamber J1 and also at the position lower than the vapor depositing ports 13a, a crucible 22 arranged in the vapor depositing source chamber J1, opening in the upper direction and also holding a vapor depositing source evaporating when being heated to vapor- deposit on the surface of the sample S, vapor depositing source heating apparatus (14+18+21) heating and evaporating the vapor depositing source in the crucible 22 to form into vapor depositing material A, a reflector 23 arranged above the crucible 22 and allowing the vapor depositing material A to processed to the vapor depositing ports 13a and reflector heating apparatus (17+19+24) heating the reflector 23.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for forming a vapor-deposited film on the surface of a sample to be observed and analyzed by using a charged particle beam apparatus (an electron microscope, an analyzer using an electron beam, an ion beam, etc.). To a vapor deposition apparatus.

[0002]

2. Description of the Related Art Conventionally, as the vapor deposition apparatus, the following (J.
The technology shown in 01) is known. (J01) Technology shown in FIG. 5 FIG. 5 shows an ultra-high vacuum scanning tunneling microscope (UHV-ST).
It is a schematic explanatory view of the conventional vapor deposition device used in M).
In order to facilitate understanding of the following description, in the drawings, the front-rear direction is the X-axis direction, the vertical direction is the Y-axis direction, the left-right direction is the Z-axis direction, and arrows X, -X, Y, -Y, Z,-
The direction or side indicated by Z is defined as front, rear, upper, lower, right, left, or front, rear, upper, lower, right, or left, respectively. Also, in the figure, those with “•” in “○” mean arrows pointing from the back of the paper to the front, and those with “x” in “○” indicate the arrow on the paper. From the back to the back.

[0005] In FIG. 5, a vacuum flange 02 is mounted on the lower right side of the outer wall 01, and is fixed to the outer wall 01 in a vacuum chamber 03 formed inside the outer wall 01 and held in vacuum. The base 04 of the ultra-high vacuum scanning tunnel microscope U is arranged. On the base 04, a deposition material passage hole 04a penetrating in the vertical direction (Y-axis direction) is formed, and on the base 04, on the left side (−Z side) of the deposition material passage hole 04a, XY stage 0 movable in X-axis direction (front-back direction) and Y-axis direction (up-down direction)
6 are arranged. The sample S is placed on the XY stage 06.
Is mounted. On the right side (Z side) of the sample S, on the right side of the deposition material passage hole 04a, a probe support device 09 for supporting the probe 08 is arranged.

[0004] Below the base 04 (-Y direction), a vapor deposition apparatus J for forming a vapor deposition film on the surface of the sample is disposed. The vapor deposition apparatus J has a cylindrical cover 011 fixed to the inner end side of the vacuum flange 02, and terminals 012a, 012a fixed to the vacuum flange 02. In the upper part on the left end side of the cylindrical cover 011, vapor deposition ports 011 a and 011 a are formed. Terminal 0
Reference numerals 12a and 012a denote members for electrically connecting the vacuum side, which is inside the vacuum flange 02, to the atmosphere side, which is the outside. Also, terminals 012a, 01 of the vapor deposition apparatus J
A heating power supply 013 is connected to an outer end (right end) of 2a, and a deposition filament 014 is connected to an inner end (left end). The deposition filament 014 is wound around a crucible 016. The crucible 016 is provided with the vapor deposition ports 011a, 011a whose openings are upward.
The inside of the crucible 016 holds a powder deposition source (not shown).

A current of about several A flows from the heating power supply 013 to the vapor deposition filament 014 to heat it, thereby heating the powder vapor source in the crucible 016.
The evaporation material A evaporated from the evaporation source by heating passes through the evaporation holes 011a and 011a of the front cylindrical cover 011 and passes through the evaporation material passage hole 04a of the base 04 fixed diagonally above the evaporation holes 011a and 011a. And the base 04
It deposits on the surface of the sample S held above. When the deposition source is a powder, a crucible is necessary, but when the deposition source is a wire or a lump, it is common to not use a crucible.

[0006]

(Problem of (J01)) In the prior art (J01), when the deposition source is a wire or a lump, the crucible 016 is not used and the deposition port 011 is not used.
a can be attached downward, and vapor deposition can be performed on the sample from above. However, when a powder deposition source is used, the crucible 016 cannot be directed downward.
Can be deposited only from below. Therefore, the sample S
In addition, it is necessary to dispose the crucible 016 and the member supporting the crucible below the member supporting the same, and there is a problem that vapor deposition cannot be performed with the reverse arrangement.
For example, in the case of the ultra-high vacuum scanning tunneling microscope U as in the prior art (J01), the crucible 016 is located below the base 04 supporting the XY stage 06 holding the sample S.
When the vapor deposition device J supporting the crucible 016 is not enough, there is a small space below the base 04 and the vapor deposition device J supporting the crucible 016 cannot be disposed below. Further, even when there is a space below, the base material 04 must be provided with a vapor-deposited material passage hole 04a for allowing the vapor-deposited material A to pass through. For this reason,
There is a problem that the conventional vapor deposition apparatus J using a crucible can be used only when there is a space for disposing the vapor deposition apparatus below the sample holding position.

In view of the above circumstances, the present invention provides the following (O01)
Is the subject of the description. (O01) To enable vapor deposition even if a crucible holding a vapor deposition source is arranged above a sample.

[0008]

Next, a description will be given of the present invention which has solved the above-mentioned problems. In the description of the present invention, reference numerals in parentheses added after constituent elements of the present invention denote constituent elements of the present invention. Reference numerals of corresponding components of the embodiment described later. The reason why the present invention is described in correspondence with the reference numerals of the components of the embodiments described later is to facilitate understanding of the present invention, and not to limit the scope of the present invention to the embodiments.

(A present invention) In order to solve the above problems, a vapor deposition apparatus of the present invention has the following requirements: (A01) A space formed inside an outer wall (1), A vapor deposition source chamber (J1) which is disposed in a vacuum chamber (3) maintained in vacuum and is formed by a wall member (13) in which vapor deposition ports (13a, 13a) are formed, (A02) the vapor deposition source chamber The sample (S) held outside the (J1) and below the vapor deposition ports (13a, 13a), (A03) is placed in the vapor deposition source chamber (J1) and has a crucible opening upward ( 22), (A04) the crucible (22) holding an evaporation source which becomes an evaporation material (A) which evaporates when heated to be evaporated on the surface of the sample (S), (A05) the crucible (2)
2) An evaporation source heating device (14 + 18 + 21) which heats and evaporates the evaporation source in (2) to form an evaporation material (A), (A06) which is disposed above the crucible (22), and
The evaporation material (A) evaporated from 2) is transferred to the evaporation port (13).
(A07) Reflector heating device (17 + 19) for heating the reflector (23).
+24; 17 + 19 + 24-28).

(Operation of the present invention) In the vapor deposition apparatus of the present invention having the above configuration, the crucible (22) opening upward is formed by the wall member (13) in which the vapor deposition ports (13a, 13a) are formed. The evaporation source chamber (J1) holds an evaporation source that becomes an evaporation material (A) that evaporates when heated and evaporates on the surface of the sample (S). Evaporation source heating device (14
In (+ 18 + 21), the evaporation source in the crucible (22) is heated and evaporated to be the evaporation material (A). The vaporized substance (A) which evaporates from the crucible (22) opening upward and is directed toward the reflector (23) above the crucible (22) comes into contact with the reflector (23). The reflector (23) is a reflector heating device (17 + 19 + 24; 17 + 19 + 24 to 28).
Therefore, the deposition material (A) in contact with the reflection plate (23) is separated without being deposited on the reflection plate (23), or is re-evaporated and separated immediately after the deposition. The reflecting plate (23) contacts the vapor deposition material (A) separated from the reflector (23) with the vapor deposition ports (13a, 13a).
To go to. The vapor deposition material (A) passing through the vapor deposition ports (13a, 13a) is applied to the sample (S) held outside the vapor deposition source chamber (J1) and below the vapor deposition ports (13a, 13a). Evaporate. Accordingly, it is possible to deposit the evaporation material (A) heated and evaporated from the inside of the crucible (22) disposed above the sample (S) on the sample (S).

When the sample (S) is held on a sample stage (6) such as an ultra-high vacuum scanning tunneling microscope (U), the vapor deposition apparatus (J) of the present invention uses the sample (S) The sample (S) can be vapor-deposited even if it is disposed above the sample stage (6) that holds the sample stage (6), so that the ultra-high vacuum scanning tunneling microscope ( In U) and the like, vapor deposition can be performed. The sample stage (6)
Even when there is a space below the member for supporting the sample (S), since the vapor deposition apparatus (J) of the present invention is arranged above the sample stage (6) holding the sample (S), it is arranged below the sample (S). There is no need to provide a passage hole for allowing the deposition material (A) to pass through the member supporting the sample stage (6).

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION

EXAMPLES Next, examples (embodiments) of the embodiments of the vapor deposition apparatus of the present invention will be described with reference to the drawings, but the present invention is not limited to the following examples. (Embodiment 1) FIG. 1 is a schematic explanatory view when a vapor deposition apparatus of Embodiment 1 of the present invention is used in an ultra-high vacuum scanning tunnel microscope. In FIG. 1, a vacuum flange 2 is mounted on the upper right side (Z side) of the outer wall 1. A base 4 of the ultra-high vacuum scanning tunneling microscope U fixed to the outer wall 1 is disposed below (−Y side) inside the vacuum chamber 3 formed by the outer wall 1 and held in vacuum. ing. An XY stage 6 that can move in the X-axis direction (front-back direction) and the Y-axis direction (up-down direction) is disposed on the left side (−Z side) of the base 4. Is mounted.

A probe support device T is disposed on the right side of the sample S. The probe support device T has a Z-direction drive mechanism 8 disposed on the base 4, and an XYZ-direction piezoelectric scanning element 9 is supported on the left end side of the Z-direction drive mechanism 8. . A probe holder 11 is supported on the left end side of the XYZ-direction piezoelectric scanning element 9. The probe holder 11 supports the probe 12, and the tip of the probe 12 faces the surface of the sample S. Above the ultra-high vacuum scanning tunnel microscope U, a vapor deposition device J is disposed.

In FIG. 1, the vapor deposition apparatus J has a cylindrical cover (wall member) 13 fixed to a left end surface (a surface in the −Z direction) of the vacuum flange 2. The left and lower portions of the cylindrical cover 13 are provided with evaporation ports 13a and 13a.
3a is formed, and an evaporation source chamber J1 is provided in the cylindrical cover 13. The cylindrical cover 13 is a member for preventing the deposition material from spreading in directions other than the direction of the sample S. Further, crucible heating terminals 14, 14 of the vapor deposition apparatus J are fixed to the lower portion of the vacuum flange 2, and the crucible heating terminals 14, 14 are fixed to the upper portion. The reflector support member 16 and the reflector heating terminals 17, 17 are fixed respectively. Crucible heating power supplies 18 and reflector heating power supplies 19 are connected to outer ends of the crucible heating terminals 14 and the reflector heating terminals 17 and 17, respectively.
An evaporation filament 21 is connected to the inner ends of the crucible heating terminals 14, 14, and the evaporation filament 21 is wound around a crucible 22. The opening of the crucible 22 is directed upward, and a powder deposition source (not shown) is held inside.

Above the crucible 22 (Y direction), a reflector 23 supported by the reflector support member 16 is disposed. The reflector 23 has a small thickness and is made of a high melting point material. The reflection plate 23 is efficiently formed of the deposition material A.
Is desirably concave to reflect light.
On the upper surface side of the reflection plate 23, a reflection plate heating filament 24 is disposed, and the reflection plate heating terminal 17,
17 is connected to the inner end. The reflector 23 is heated by the radiation of the reflector heating filament 24. The crucible heating terminal 1
4, 14, the crucible heating power supply 18 and the vapor deposition filament 21 are used to produce the vapor deposition source heating device (14 + 18 +
21), and the reflection plate heating terminals 17, 17,
The reflector heating device (17 + 19 + 2) of the first embodiment is supplied from the reflector heating power supply 19 and the reflector heating filament 24.
4) is configured.

(Effect of Embodiment 1) In FIG. 1, a current of about several A is passed from the crucible heating power supply 18 to the vapor deposition filament 21 to heat it, and the powder vapor deposition source contained in the crucible 22 is heated. Heat. The evaporation material A evaporated from the evaporation source by heating is applied to the reflector 2 above the crucible 22.
3 contacts the lower surface. Along with the heating of the vapor deposition source, a current of about several A flows from the power supply 19 for heating the reflector to the filament 24 for heating the reflector, and heats the reflector 24 below the filament 24 for heating the reflector. .
When the reflection plate 23 is heated, the reflection plate 23
The deposition material A in contact with the lower surface separates without being deposited on the reflection plate 23 or re-evaporates immediately after the deposition. The re-evaporated deposition material A jumps out of the reflection plate 23 as if the reflection plate 23 becomes a so-called crucible, and passes through the deposition ports 13a, 13a.
3a Vapor deposition is performed on the surface of the sample S held diagonally below the XY stage 6 of the ultra-high vacuum scanning tunnel microscope U.

Accordingly, the evaporation material A, which has been heated and evaporated from the crucible 22 of the vapor deposition apparatus J disposed above the sample S, is placed on the sample S below the crucible 22 of the vapor deposition apparatus J.
Can be deposited. Further, since the vapor deposition apparatus J according to the first embodiment of the present invention can vapor-deposit the sample S even when it is disposed above the XY stage 6 holding the sample S, the base 4 supporting the XY stage 6 can be used. Vapor deposition can be performed even in the ultra-high vacuum scanning tunnel microscope U having a small space below. The XY stage 6
Even when there is a space below the base 4 for supporting the sample S, the vapor deposition apparatus J according to the first embodiment of the present invention is capable of holding the sample S
Since the XY stage 6 is disposed above the Y stage 6,
There is no need to provide a passage hole for allowing the deposition material A to pass through the base 4 that supports the substrate. Further, since the reflector 23 is heated by the radiation of the reflector heating filament 24, the vapor deposition apparatus J of the first embodiment is suitable for a substance having a melting point of about several hundred degrees Celsius.

(Embodiment 2) FIG. 2 is a schematic explanatory view of a vapor deposition apparatus according to Embodiment 2 of the present invention. In the description of the second embodiment, components corresponding to the components of the first embodiment are denoted by the same reference numerals, and detailed description thereof will be omitted.
The second embodiment differs from the first embodiment in the following points, but has the same configuration as the first embodiment in other points. In FIG. 2, in the second embodiment, a high voltage application terminal 26 is fixed to the vacuum flange 2 instead of the reflection plate support member 16 of the first embodiment. The high voltage application terminal 2
A power supply 27 for applying high voltage is connected to the outer end of 6.
A lead rod 28 is fixed to the inner end of the high-voltage application terminal, and the reflector 23 is fixed to the tip of the lead rod 28. In the second embodiment, a high voltage of several hundred volts or more is applied to the reflector 23 from the power supply 27 for applying high voltage, and a current is supplied from the power source 19 for heating the reflector to the filament 24 for heating the reflector. Electrons are generated, and the thermal electrons are applied to the reflector 23 to heat the reflector 23 by electron impact heating. In addition, the reference numerals 17, 19, 24, 26, 27, 2
8 to the reflector heating device of the second embodiment (17
+ 19 + 24 to 28).

(Operation of Embodiment 2) A current of about several A is passed from the crucible heating power supply 18 to the vapor deposition filaments 21 and 21 to heat the vapor deposition filaments 21 and 21, and the vapor deposition source in the crucible 22 is heated and evaporated to deposit vapor deposition material. Generate. At the same time, a high voltage of several hundred volts or more is applied from the high voltage applying power supply 27 to the reflector 23, and a current of about several A flows from the reflector heating power supply 19 to the reflector heating filament 24, thereby generating thermoelectrons. Is generated, and the thermoelectrons are applied to the reflection plate 23 to heat the reflection plate 23 by electron impact heating. When the reflection plate 23 is heated, the deposition material A that has been in contact with the lower surface of the reflection plate 23 separates without being deposited on the reflection plate 23 or re-evaporates immediately after the deposition, and
Move away from The deposition material A that has separated from the reflector 23 is deposited on the sample S obliquely below the evaporation ports 13a, 13a through the evaporation ports 13a, 13a of the front cylindrical cover 13.

Therefore, the evaporation material A, which is heated and evaporated from the crucible 22 of the vapor deposition apparatus J disposed above the sample S, is placed on the sample S below the crucible 22 of the vapor deposition apparatus J.
Can be deposited. Further, since the vapor deposition apparatus J according to the second embodiment of the present invention can vapor-deposit the sample S even when it is disposed above the XY stage 6 holding the sample S, the base 4 supporting the XY stage 6 can be used. Vapor deposition is possible even in the ultra-high vacuum scanning tunnel microscope U having a small space below. Even when there is a space below the base 4 supporting the XY stage 6, it is not necessary to provide a passage hole for allowing the deposition material A to pass through the base 4 supporting the XY stage 6. In addition, since the reflective plate 23 is heated by applying the thermoelectrons to the reflective plate 23 and heating the reflective plate 23 by electron impact heating, the vapor deposition apparatus J of the second embodiment has a melting point of 1000 ° C. or more. Suitable for high melting point materials.

(Embodiment 3) FIG. 3 is a schematic explanatory view of a vapor deposition apparatus according to Embodiment 3 of the present invention. In the description of the third embodiment, components corresponding to the components of the first embodiment are denoted by the same reference numerals, and detailed description thereof will be omitted.
The third embodiment differs from the first embodiment in the following points, but has the same configuration as the first embodiment in other points. In FIG. 3, in the third embodiment, a heater (not shown) connected to the reflector heating power supply 19 is disposed so as to adhere to the reflector 23, and heats the reflector 23. Further, a lead rod 29 is connected to the inner ends of the reflector heating terminals 17 instead of the reflector heating filament 24 of the first embodiment.

(Effect of Embodiment 3) A current of about several A is passed from the crucible heating power supply 18 to the vapor deposition filaments 21 and 21 to heat it, and the powder vapor deposition source contained in the crucible 22 is heated. I do. The evaporation material A evaporated from the evaporation source by heating comes into contact with the lower surface of the reflection plate 23 above the crucible 22. Along with the heating of the vapor deposition source, a current is supplied from the reflector heating power supply 19 to a heater (not shown) to heat the reflector, thereby heating the reflector 23. When the reflector 23 is heated, the deposition material A that has been in contact with the lower surface of the reflector 23 separates without being deposited on the reflector 23 or re-evaporates immediately after the deposition, and is removed from the reflector 23. Leave. The deposition material A that has separated after coming into contact with the reflection plate 23 passes through the vapor deposition ports 13 a of the front cylindrical cover 13 and passes through the vapor deposition port 13.
a and 13a are deposited on the surface of the sample S obliquely below. Therefore, also in the third embodiment, the evaporation material A heated and evaporated from the crucible 22 of the evaporation apparatus J disposed above the sample S is deposited on the sample S below the crucible 22 of the evaporation apparatus J. Becomes possible.

(Embodiment 4) FIG. 4 is a schematic explanatory view of a vapor deposition apparatus according to Embodiment 4 of the present invention. In the description of the fourth embodiment, the same reference numerals are given to the components corresponding to the components of the first embodiment, and the detailed description thereof will be omitted.
The fourth embodiment differs from the first embodiment in the following points, but has the same configuration as the first embodiment in other points. In FIG. 4, the reflector 23 of the fourth embodiment and the crucible 22 above the reflector 23 are integrated, and the reflector 23 and the crucible 22 are heated by the vapor deposition filament 21 wound around the crucible 22. It is supposed to be. For this reason, the reflector heating power supply 19 and the reflector heating filament 24 of the first embodiment are omitted. In the fourth embodiment, similarly to the first embodiment, the evaporation material A heated and evaporated from the inside of the crucible 22 of the evaporation apparatus J can be evaporated on the sample S below the crucible 22 of the evaporation apparatus J.

(Modifications) Although the embodiments of the present invention have been described in detail, the present invention is not limited to the above-described embodiments, but falls within the scope of the present invention described in the appended claims. Thus, various changes can be made. Modified embodiments of the present invention will be exemplified below. (H01) Although the crucible 22 is heated by the vapor deposition filament 21 in each of the above-described embodiments, a method using electron impact heating in which a thermoelectron is applied to the crucible 22 can be adopted. (H02) The vapor deposition apparatus of the present invention can be used in a charged particle beam apparatus other than the ultrahigh vacuum scanning tunneling microscope U.

[0025]

The vapor deposition apparatus according to the present invention has the following effects. (E01) Even if a crucible holding an evaporation source is arranged above the sample, evaporation can be performed.

[Brief description of the drawings]

FIG. 1 is a schematic explanatory diagram when a vapor deposition apparatus according to a first embodiment of the present invention is used in an ultra-high vacuum scanning tunnel microscope.

FIG. 2 is a schematic explanatory view of a vapor deposition apparatus according to Embodiment 2 of the present invention.

FIG. 3 is a schematic explanatory view of a vapor deposition apparatus according to Embodiment 3 of the present invention.

FIG. 4 is a schematic explanatory view of a vapor deposition apparatus according to a fourth embodiment of the present invention.

FIG. 5 is an ultra-high vacuum scanning tunneling microscope (UH)
FIG. 2 is a schematic explanatory view of a conventional vapor deposition device used in (V-STM).

[Explanation of symbols]

A: evaporation material, J1: evaporation source chamber, S: sample, 1: outer wall,
3: vacuum chamber, 13: wall member, 13a, 13a: vapor deposition port, 2
2: Crucible, 23: Reflector, (14 + 18 + 21) ... Evaporation source heater, (17 + 19 + 24; 17 + 19 + 24)
~ 28) Reflector heating device.

Claims (1)

[Claims] 1. A vapor deposition apparatus having the following requirements, (A01) a space formed inside an outer wall,
An evaporation source chamber which is disposed in a vacuum chamber maintained in a vacuum and is formed by a wall member having an evaporation port formed therein, (A02) which is held outside the evaporation source chamber and below the evaporation port; A sample, (A03) a crucible arranged in the evaporation source chamber and opening upward, (A04) a crucible holding an evaporation source which becomes an evaporation material to be evaporated on the surface of the sample when heated, A05) An evaporation source heating device that heats and evaporates the evaporation source in the crucible to form an evaporation substance, (A06)
(A07) a reflector disposed above the crucible and directing a vapor deposition material evaporated from the crucible to the vapor deposition port;
A reflector heating device for heating the reflector.