JPH0693429A - Crucible for vacuum vapor deposition device - Google Patents

Abstract

PURPOSE:To provide the crucible for a vacuum vapor deposition which is usable for rapid heating by an electron beam, prevents the leakage of a molten metal, does not require preheating by the electron beam, does not require the separate provision of a heat treatment furnace and has high safety. CONSTITUTION:The crucible for the vacuum vapor deposition device which has an electron gun 2 for radiating the electron beam 1, the crucible 10 for housing the molten metal 3, a substrate 4 and a chamber 5 contg. the crucible and evacuated to a vacuum, heats the metal in the crucible by radiating the electron beam by the electron gun to melt and evaporate the metal and solidifies the evaporated metal on the surface of the substrate is constituted of a heat resistant vessel 12 having a recessed part 11 for housing the molten metal on the front surface, a casing 14 enclosing the outside surface exclusive of the upper surface of the heat resistant vessel separated a spacing therefrom, heat resistant powder 16 packed between the heat resistant vessel and the casing and a heater 18 inserted into the heat resistant powder.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vacuum vapor deposition apparatus, and more particularly to a crucible for a vacuum vapor deposition apparatus which is heated by an electron beam.

[0002]

2. Description of the Related Art Vacuum deposition is a film forming process in which a metal is heated and evaporated in a vacuum, and the evaporated metal is solidified on the surface of a substrate (material to be processed) to form a film. In such a film forming process, an electron beam is used to heat a vapor-deposited metal, and an evaporation metal in a crucible is irradiated with the electron beam to melt and evaporate the metal. The heating by the electron beam has many characteristics such as high temperature heating which is difficult with an ordinary heater and the like, and rapid heating and easy control of heating rate.

[0003]

The conventional crucible used in the above-mentioned vacuum vapor deposition apparatus is formed by molding a refractory material such as silica or alumina into a container having an open top. However, such a conventional crucible has a problem that cracks or cracks easily occur due to rapid heating by an electron beam, and molten metal leaks from the crucible.

In order to solve this problem, the conventional crucible is a separate container made of refractory material (hereinafter referred to as a crucible container).
A crucible which is housed in a conventional crucible and which prevents molten metal from leaking from the container by partially solidifying the molten metal leaking from the crucible in the crucible container is used.

However, since such a conventional crucible container contains a large amount of air and moisture inside, if it is used for vacuum deposition as it is, a large amount of gas (air and water vapor) flows into the apparatus through the crucible. There is a problem that the degree of vacuum in the apparatus cannot be maintained within a range suitable for electron beams (for example, 10 ⁻³ torr or less), and the vapor deposition metal cannot be heated. Therefore, until degassing and drying of the crucible container are completed, it is necessary to slowly heat the crucible container so that the degree of vacuum inside the device can be maintained. There was a point.

In order to avoid such problems, the crucible container is placed in another heat treatment furnace, and after degassing and drying,
The means used for vacuum vapor deposition are used. However, such a method requires a heat treatment apparatus adjacent to the vacuum vapor deposition apparatus, the equipment becomes large in size and the equipment cost is high, and a high temperature crucible container is installed so that the degassed / dried crucible container does not absorb moisture again. Since it is necessary to move into the vacuum vapor deposition apparatus in a short time, there is a problem that work is dangerous.

The present invention was devised to solve the above-mentioned various problems. That is, the object of the present invention is that it can be used for rapid heating by electron beam, does not leak molten metal, does not require preheating by electron beam, does not require a separate heat treatment furnace, and is highly safe. To provide a crucible for a vacuum vapor deposition apparatus.

[0008]

According to the present invention, there is provided an electron gun for emitting an electron beam, a crucible for containing a metal to be melted, a substrate and a chamber containing the crucible and evacuated to a vacuum, A crucible for a vacuum vapor deposition apparatus that heats and melts and evaporates the metal in the crucible by radiating an electron beam with an electron gun, and solidifies the evaporated metal on the surface of the substrate. In a heat-resistant container, a casing surrounding the outer surface of the heat-resistant container with a gap apart from the upper surface, a heat-resistant powder filled between the heat-resistant container and the casing, a heater inserted in the heat-resistant powder, A crucible for a vacuum vapor deposition device, comprising:

According to a preferred embodiment of the present invention, the heater is capable of heating the heat resistant powder at a temperature of at least 200 ° C. and below a temperature at which the molten metal cannot evaporate, and is further resistant to the molten metal. It is an electric resistance heater equipped with a protection tube. The heat-resistant container and the heat-resistant powder are made of a refractory material that can withstand the melting temperature of the metal to be melted, the heat-resistant container has a porosity of 20 to 30%, and the heat-resistant powder is more coarsely filled than the heat-resistant container. Further, it is preferable that the heat resistant container and the heat resistant powder are made of a refractory material containing at least oxide, carbide, nitride, boride, or ceramics as a main component.

[0010]

According to the above-mentioned structure of the present invention, the crucible for a vacuum vapor deposition apparatus according to the present invention encloses a heat-resistant container having a recess for accommodating molten metal on its upper surface and an outer surface of the heat-resistant container with a space therebetween. Since the casing and the heat resistant powder filled between the heat resistant container and the casing are provided, the molten metal leaked from the heat resistant container even when the heat resistant container is cracked or cracked by rapid heating by an electron beam. Since it penetrates into the gap of the heat resistant powder and solidifies in the gap of the heat resistant powder having a relatively low temperature, the molten metal does not leak from the crucible. Therefore, the crucible according to the present invention can be used for rapid heating by electron beam. In particular, the heat-resistant container and the heat-resistant powder are made of a refractory material that can withstand the melting temperature of the metal to be melted, the heat-resistant container has a porosity of 20 to 30%, and the heat-resistant powder is more coarsely filled than the heat-resistant container. The heat-resistant container is dense, the molten metal is unlikely to leak, and has high strength. The heat-resistant powder is soaked in the molten metal that it can be diffused in a wide range without cracking.

Further, since the crucible for the vacuum vapor deposition apparatus according to the present invention includes the heater inserted in the heat resistant powder,
The heater can be used to degas and dry the heat resistant powder in the vacuum vapor deposition apparatus. Therefore, costly preheating with an electron beam is not required, a separate heat treatment furnace is not required, and safety is high. Also, degas the electron beam.
Since it is not used for drying, degassing and drying are not restricted by pressure, and degassing and drying can be performed not only in vacuum but also at atmospheric pressure. Further, since the heating / cooling can be adjusted by adjusting the output of the heater, the heating can be performed more slowly than the heating by the electron beam, and the thermal stress generated in the crucible can be reduced. As a result, damage to the heat-resistant container can be particularly reduced, and the life of the entire crucible can be extended.

Further, if the heater is a resistance heater capable of heating the heat-resistant powder to at least 200 ° C. or more and provided with a protective tube capable of withstanding the molten metal, the molten metal leaks from the heat-resistant container. Even if there is, the heat resistant powder can be degassed and heated without damaging the heater due to contact with the molten metal.

[0013]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is an overall vertical sectional view showing a vacuum vapor deposition apparatus and a crucible for a vacuum vapor deposition apparatus according to the present invention, and FIG. 2 is a transverse sectional view of a crucible for a vacuum vapor deposition apparatus according to the present invention. Figure 1
In FIG. 1, the vacuum vapor deposition apparatus includes an electron gun 2 that emits an electron beam 1, a crucible 10 that contains a molten metal 3, and a chamber 5 that contains a substrate 4 and a crucible 10 and that is evacuated to a vacuum.

The substrate 4 is, for example, a steel plate, a stainless plate, a film or the like. The electron beam 1 is radiated in the horizontal direction, and then is irradiated by a magnetic field (not shown) applied in the chamber 5 to irradiate the metal 3 for vapor deposition in the crucible 10 to heat and melt the metal 3 for vapor deposition in the crucible 10.・ It is designed to be evaporated. The inside of the chamber 5 is normally maintained at a vacuum of 10 ⁻³ to 10 ⁻⁵ torr by a vacuum pump (not shown).

With such a configuration, the illustrated vacuum vapor deposition apparatus radiates the electron beam 1 by the electron gun 2 to the crucible 10
The vapor deposition metal 3 therein can be heated to melt and evaporate, and the vaporized metal can be solidified on the surface of the substrate 4. In the crucible 10, various metals such as aluminum (Al),
Zinc (Zn), Nickel (Ni), Alumina (Al
₂ O ₃ ), etc. The number of crucibles 10 may be one, or may be two or more. Further, the same metal may be housed in a plurality of crucibles, or different metals may be housed. By using different metals at the same time, alloys such as Al—Zn alloys can be deposited on the substrate 4.

1 and 2, a crucible 10 for a vacuum vapor deposition apparatus according to the present invention has a recess 1 for containing a molten metal 3.
1, a heat-resistant container 12 having an upper surface 1, a casing 14 surrounding the outer surface of the heat-resistant container 12 excluding the upper surface with a space, a heat-resistant powder 16 filled between the heat-resistant containers 12, and a heat-resistant powder 16 And a heater 18 inserted in the.

The heat resistant container 12 and the heat resistant powder 16 are made of a refractory material that can withstand the melting temperature of the metal to be melted. In particular, the heat-resistant container and the heat-resistant powder should be resistant to the high melting temperature.
It is preferable that the refractory material contains at least oxide, carbide, nitride, boride, or ceramics as a main component. Thereby, for example, aluminum (Al, melting point 660 °
C), zinc (Zn, about 420 ° C), nickel (N
The crucible according to the present invention can be used for vapor deposition of i, 1453 ° C).

The porosity of the heat-resistant container is 20 to 30%,
The heat resistant powder is filled so as to be coarser than the heat resistant container. A refractory material having a porosity of 20 to 30% has high thermal shock resistance,
And the strength is great. Therefore, with such a structure, the heat-resistant container is dense, the molten metal is hard to leak, and the strength can be increased. Further, the heat-resistant powder, which is coarser than the heat-resistant container, can penetrate the molten metal and diffuse into a wide range, and since it is made of powder, it does not crack due to heat.

The casing 14 is a recess 1 of the heat-resistant container 12.
The outer surface other than the upper surface having the number 1 is surrounded with a space. This interval should be set so that the temperature of the casing itself does not become excessively high. As a result, overheating of the casing can be prevented and the life of the casing can be extended. The casing 14 is made of a heat-resistant metal such as SUS310 or SUS.
316 or SUS304 or the like is preferable. The casing 14 is preferably made watertight by welding or the like except for the through holes through which the electric cables of the heater 18 are passed. Thereby, even if the molten metal leaks to the casing through the heat resistant powder, the molten metal can be prevented from leaking from the crucible 10.

The heater 18 is preferably capable of heating the heat resistant powder 16 to at least 200 ° C. or higher, preferably 500 ° C. or higher. Further, it is preferable that the heat resistant powder 16 is heated by the heater 18 to a temperature below which the molten metal cannot be evaporated. Thereby, the heat resistant powder can be sufficiently heated, degassed and dried. Further, the heater 18 is an electric resistance heater provided with a protection tube 18a that withstands molten metal. For example, the protective tube 18a may be a sealed tube made of heat-resistant metal such as Inconel, Hastroy, and SUS310. Thereby, even when the molten metal comes into contact with the heater 18, the protection tube 18a can prevent the heater from being damaged.

Further, as shown in FIG. 2, the heater 18 has a length shorter than that of the casing 14, is entirely housed in the casing 14, and is connected to each other by a heat-resistant electric cable (not shown). The electric cable is taken out. With this configuration, the lower portion of the casing can be made watertight, and even if molten metal may leak to the casing through the heat resistant powder, the molten metal can be prevented from leaking from the crucible 10.

[0022]

As described above, the crucible for a vacuum vapor deposition apparatus according to the present invention comprises a heat-resistant container having a concave portion for accommodating molten metal on its upper surface, and a casing surrounding the outer surface of the heat-resistant container with a space therebetween. Since the heat-resistant powder filled between the heat-resistant container and the casing is provided, even if the heat-resistant container is cracked or cracked by rapid heating by an electron beam, the molten metal leaked from the heat-resistant container is heat-resistant. The molten metal does not leak from the crucible because it penetrates into the gap of the powder and solidifies in the gap of the heat resistant powder having a relatively low temperature. Therefore, the crucible according to the present invention can be used for rapid heating by electron beam. In particular, the heat-resistant container and the heat-resistant powder are made of a refractory material that can withstand the melting temperature of the metal to be melted, and the heat-resistant container has a porosity of 20 to 30%.
If the heat-resistant powder is filled more coarsely than the heat-resistant container, the heat-resistant container is dense, the molten metal is hard to leak, and the strength is high.
The heat-resistant powder can penetrate the molten metal and diffuse into a wide range without cracking.

Further, since the crucible for the vacuum vapor deposition apparatus according to the present invention has the heater inserted in the heat resistant powder,
The heater can be used to degas and dry the heat resistant powder in the vacuum vapor deposition apparatus. Therefore, costly preheating with an electron beam is not required, a separate heat treatment furnace is not required, and safety is high. Also, degas the electron beam.
Since it is not used for drying, degassing and drying are not restricted by pressure, and degassing and drying can be performed not only in vacuum but also at atmospheric pressure. Further, since the heating / cooling can be adjusted by adjusting the output of the heater, the heating can be performed more slowly than the heating by the electron beam, and the thermal stress generated in the crucible can be reduced. As a result, damage to the heat-resistant container can be particularly reduced, and the life of the entire crucible can be extended.

Further, the heater may be an electric resistance heater capable of heating the heat resistant powder to at least 200 ° C. or higher and below the temperature at which the molten metal cannot evaporate, and equipped with a protective tube resistant to the molten metal. For example, even if the molten metal leaks from the heat-resistant container, the heat-resistant powder can be degassed and heated without the heater being damaged by the molten metal.

Therefore, in summary, according to the present invention, it can be used for rapid heating by electron beam, there is no leakage of molten metal, and preheating by electron beam is unnecessary,
It is not necessary to separately provide a heat treatment furnace, and it is possible to provide a highly safe crucible for a vacuum evaporation apparatus.

[Brief description of drawings]

FIG. 1 is an overall vertical cross-sectional view showing a vacuum vapor deposition apparatus and a crucible for a vacuum vapor deposition apparatus according to the present invention.

FIG. 2 is a cross-sectional view of a crucible for a vacuum vapor deposition device according to the present invention.

[Explanation of symbols]

 1 Electron Beam 2 Electron Gun 3 Molten Metal 4 Substrate 5 Chamber 10 Crucible 11 Recess 12 Heat-Resistant Container 14 Casing 16 Heat-Resistant Powder 18 Heater

Claims (4)

[Claims] 1. A crucible for emitting an electron beam by an electron gun, comprising: an electron gun for emitting an electron beam; a crucible for containing a molten metal; and a chamber containing a substrate and the crucible and evacuated to a vacuum. The metal inside is heated and melted.
A crucible for a vacuum vapor deposition apparatus for evaporating and solidifying evaporated metal on the surface of a substrate, wherein a heat-resistant container having a concave portion for accommodating molten metal on the upper surface and an outer surface other than the upper surface of the heat-resistant container are spaced apart from each other. A crucible for a vacuum vapor deposition apparatus, comprising: a surrounding casing; a heat resistant powder filled between the heat resistant container and the casing; and a heater inserted in the heat resistant powder. 2. The heater comprises at least 2 heat resistant powders.
2. An electric resistance heater capable of being heated to a temperature not lower than 00 ° C. and lower than a temperature at which molten metal cannot evaporate, and further provided with a protective tube resistant to the molten metal. A crucible for a vacuum vapor deposition device as described. 3. The heat resistant container and the heat resistant powder are made of a refractory material capable of withstanding the melting temperature of a metal to be melted, the heat resistant container has a porosity of 20 to 30%, and the heat resistant powder is more coarsely filled than the heat resistant container. The crucible for a vacuum vapor deposition device according to claim 2, wherein 4. The heat resistant container and the heat resistant powder are oxides,
The crucible for a vacuum vapor deposition apparatus according to claim 3, wherein the crucible is made of a refractory material containing at least a carbide, a nitride, a boride, or a ceramic as a main component.