JPH05171412A - Production of material for vapor-depositing silicon monoxide - Google Patents

Abstract

PURPOSE:To produce a material for vapor-depositing silicon monoxide while suppressing splash. CONSTITUTION:Silicon is mixed with silicon dioxide and evaporated by heating in vacuum. The resulting vapor is condensed on a cooled recovering plate and the resulting condensate is heated to >=1000 deg.C in inert gas under >=10<-1>Torr pressure or the vapor is condensed on a recovering plate kept at >=1,000 deg.C.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a material for vapor deposition of silicon monoxide used for forming an optical component, a hard coating for protection or a plastic film for gas permeable resistance packaging.

[0002]

2. Description of the Related Art Conventionally, a material for vapor deposition of silicon monoxide is a mixture of silicon and silicon dioxide, which is heated to 1200 to 1400 ° C. in a vacuum of 10 ^-2 Torr or less and evaporated on a recovery plate cooled. It was manufactured by condensing.

[0003]

When silicon monoxide produced by the conventional method is used as an evaporation material for vacuum evaporation, a diameter of 0.01 μm to 2 mm called a splash from the evaporation material at the time of temperature rise and at the beginning of evaporation. Lumps of
It has come to the surface of the vapor-deposited substrate to reduce the surface gloss and cause pinholes in the film. In severe cases, when the vapor deposition substrate is a plastic film having a thickness of several tens of μm, through holes may be formed in the substrate.

Therefore, there are drawbacks that the yield of the evaporation material is low and the operating rate of the vapor deposition apparatus is low, such that the temperature raising time is lengthened and the vapor deposition temperature must be maintained for a certain time or more before the vapor deposition is started. It was

In view of the above-mentioned state of the art, the present invention aims to provide a method for producing a silicon monoxide vapor deposition material in which the problems of the vapor deposition material produced by the conventional method are eliminated.

[0006]

According to the present invention, (1) a substance obtained by mixing silicon and silicon dioxide, heating in a vacuum and evaporating is condensed on a cooled recovery plate,
A method for producing a material for vapor deposition of silicon monoxide, comprising heating the obtained condensed substance to 1000 ° C. or higher in an inert gas of 10 ⁻¹ Torr or higher.

(2) A material for vapor deposition of silicon monoxide, characterized in that a substance obtained by mixing silicon and silicon dioxide, heating in a vacuum and evaporating is condensed on a recovery plate kept at 1000 ° C. or higher. Production method. Is.

The first aspect of the present invention is to use silicon monoxide obtained by the conventional method in an inert gas atmosphere of 10 ^-1 Torr or more.
This is a method of heating to 000 ° C or higher, but here, 10 ^-1 T
oror is silicon monoxide 45 at 1000 ℃
Since it has an equilibrium vapor pressure of 0.75 Torr at 1 × 10 ⁻³ Torr and 1400 ° C., if it is lower than this value, the evaporation becomes remarkable and the yield is poor. The inert gas is silicon monoxide and the atmosphere gas. To prevent the reaction of 10
The temperature of 00 ° C or higher is 1000 ° C as described in Examples below.
This is because there is no effect if less than.

The second invention of the present invention is the same as the conventional method in terms of means. However, only the temperature of the recovery plate is heated to 1000 ° C. or higher, and the heat recovery plate is cooled. It is a method of condensing a material for vapor deposition of silicon oxide. 1000 ° C
The reason for the above is that there is no effect below 1000 ° C. as in the examples described later.

[0010]

According to the present invention, the reason why the splash can be remarkably reduced is not clear, but silicon monoxide obtained by condensing a conventional SiO vapor on a cooled recovery plate is amorphous and has internal stress, and While it is considered that there are many internal defects and cracks are likely to occur, by heating the recovery plate during subsequent heating or condensation as in the method of the present invention, the internal stress is small and the silicon monoxide has few internal defects. It is thought that splash can be prevented because cracks are less likely to occur.

[0011]

EXAMPLES Examples of the first invention and the second invention of the present invention will be given below together with comparative examples to prove the effects of the present invention.

Examples and Comparative Examples of the First Invention [0012] Silicon monoxide, which is obtained by mixing silicon and silicon dioxide and evaporating by heating to 1200 to 1400 ° C in a vacuum of 10 ^-2 Torr or less, is condensed on a cooled recovery plate. After that, the obtained silicon monoxide was heated to each temperature in an inert gas at each pressure.

Example of the Second Invention and Comparative Example Silicon monoxide, which was obtained by mixing silicon dioxide with silicon dioxide and evaporating by heating to 1200 to 1400 ° C. in a vacuum of 10 ⁻² Torr or less, was held at each temperature. It was condensed onto a collection plate.

The silicon monoxide vapor deposition material prepared in the above was heated to 1380 ° C. at a pressure of 1 × 10 ⁻⁴ Torr by the vacuum vapor deposition apparatus shown in FIG. 1 to vapor deposit silicon monoxide on a glass plate, and scanning electron Five fields of view were observed with a microscope at a magnification of 5000, and the average value of the number of deposits on the coating surface was obtained. Also,
Since the absolute value of the production rate of silicon monoxide is determined by the capacity of the production apparatus, the production rate under standard conditions is set to 1 and shown as a relative value.

In the vacuum vapor deposition apparatus of FIG. 1, 1 is a vacuum tank, 2 is a film substrate, 3 is a material for vapor deposition, and 4 is a chimney type evaporation source.

The above results are shown in Table 1 below.

[Table 1]

The silicon monoxides produced in Comparative Examples 1 and 2 have heating temperatures of 800 and 900 ° C., and the production rate is a value under the standard conditions, but the number of splashes is large and it is unsuitable as a vapor deposition material.

The silicon monoxide produced in Examples 1 to 4 is good in the production rate and the number of splashes at a heating temperature of 1000 to 1300 ° C., and is a good vapor deposition material.

In Examples 5 to 8, the heating temperature was 1000 ° C.,
There are few splashes for all four pressures of 10 ^-1 , ¹ , 10, 760 Torr, but 10 ^-1 , 1 Torr is a good evaporation material although the production rate is slightly low. Further, when the pressure is raised to 10,760 Torr, the production rate is improved and it is a good evaporation material.

The silicon monoxide produced in Comparative Examples 3 and 4 has a large amount of splash at heating temperatures of 800 and 900 ° C. and is unsuitable as an evaporation material.

Heating temperature of Examples 9-11: 1000-13
00 ° C has a small splash, a good production rate, and is a good evaporation material.

[0022]

According to the present invention, silicon monoxide having a small internal stress and a small number of internal defects can be obtained, and since cracking is less likely to occur, splash can be prevented, and the silicon monoxide obtained by the present invention can be used as an evaporation material. When used as, the yield of the evaporation material is improved and the operation rate of the vapor deposition apparatus can be improved.

[Brief description of drawings]

FIG. 1 is a schematic view of a vapor deposition apparatus for confirming the effect of a silicon monoxide vapor deposition material obtained by the method of the present invention.

Claims (2)

[Claims] 1. A substance obtained by mixing silicon and silicon dioxide, heating in a vacuum and evaporating, is condensed on a cooled recovery plate, and the obtained condensed substance is then an inert gas of 10 ⁻¹ Torr or more. A method for producing a material for vapor deposition of silicon monoxide, which comprises heating to 1000 ° C. or higher in the atmosphere. 2. A method for producing a material for vapor deposition of silicon monoxide, characterized in that a substance obtained by mixing silicon and silicon dioxide, heating in a vacuum, and evaporating is condensed on a recovery plate kept at 1000 ° C. or higher. Method.