JPS6130663A - Surface coating device of powdery solid - Google Patents

Abstract

PURPOSE:To cover the surface of powdery solid with coating film in uniform thickness when covering the surface of powdery solid with vaporized coating material in a vacuum container, by vapor depositing the coating material while rolling the powdery solid. CONSTITUTION:A holder 11 in which metal 5 such as Zn etc. for vapor deposition is contained is placed in a glass container 1 and surrounded by a heater for evaporation and connected to a heating power source 4. Opposite to this, a sample 6 of powsery solid such as thin flaky glass, active alumina beads etc. is placed on a mechanical vibration generating device 8. Inside of the container 1 is evacuated by a vacuum pump 2, and the metal 5 for vapor deposition is heated and evaporated by the heater 3 and vapor deposited on the sample of powdery solid 6. At this time, electrical oscillation generated by an oscillator 9 is amplified by an amplifier 10, and the sample of powdery solid is rolled by the device 8 using the oscillating electric power, and uniform film of Zn etc. is formed on whole face of the sample 6.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to an improvement in an apparatus for applying a coating substance to the surface of a powdered solid in a vacuum vessel.

More specifically, the present invention provides powder coating using vacuum evaporation, ion blating, sputtering, etc., such as when coating the surface of an inorganic photonic material powder with a metal or coating the surface of a glass microsphere with an inorganic compound. The present invention relates to an apparatus capable of forming a uniform coating on the surface of a powdery solid by rolling the entire powdery solid when a coating material is applied to the surface of the solid.

Conventional technology Until now, methods for coating the surface of powdered solids include coating metals such as nickel by dispersing mica in a plating solution with a special composition and performing electroless plating; Methods are known in which pyrolytic carbon is deposited on the surface of a powdered solid while it is fluidized, but these methods are limited in the coating materials and thus have a limited range of application.

On the other hand, as a method for coating the surface of a substrate with metal or other substances, the coating material is gasified or ionized under vacuum conditions such as vacuum evaporation, ion blating, or sputtering, and the gas is collided with the surface of the substrate. A method of coating is known. These methods can be applied to a relatively wide range of coating substances and produce products of good quality, so these methods have recently been used for watch cases, bands, and various accessories.
1. These methods have become widely used for coating electronic components, etc., but in these methods, it is necessary to expose the surface to be coated so that it can come into contact with the gas or ions of the coating substance. It has the disadvantage that it cannot be used to coat powdered solids that are processed without being exposed in multiple layers. To overcome these drawbacks, it is sufficient to constantly roll the solid particles by stirring, shaking, fluidizing, etc., so that each surface can come into uniform contact with the above gas or ions. However, all of the above methods must be carried out in a vacuum container, and stirring, shaking, and fluidization by normal mechanical means used in the atmosphere cannot be applied.

Until now, it has not been possible to coat powdered solids using these methods.

Problems to be Solved by the Invention The purpose of the present invention is to apply a uniform coating to the surface of a powdery solid using a surface coating method performed in a vacuum container such as a vacuum evaporation method, an ion blasting method, or a sputtering method. The purpose is to provide a device for rubbing.

, 1., 1 Another object of the present invention is to provide a transfer means for effectively coating the surface by rolling a powdery solid placed in a vacuum container. be.

Means for Solving the Problems According to the present invention, in an apparatus for depositing a coating substance on the surface of a powdery solid in a vacuum container, the powdery solid mounting table is formed into a mechanical vibration generator. At the same time, this device is connected to an oscillation device separately provided outside the vacuum container via an amplifier device, and a powdery solid surface coating device is used.
That purpose can be achieved.

Next, one example of the apparatus of the present invention will be specifically explained with reference to the accompanying drawings. 1 is a vacuum container, usually made of glass, which is connected to a vacuum pump 2 so that the contents can be brought to a vacuum when necessary. Reference numeral 11 denotes a metal holder for deposition, in which a coating material, for example, a metal for deposition 5 is housed, and is heated and gasified by a surrounding heater for deposition 3 and a heating power source 4 connected to it. . The powder solid sample 6 is stored in a suitable container and placed on a mounting table 8. This mounting table is formed into a mechanical vibration generator, and is connected to an oscillating device 9 via an amplifier 10 outside the vacuum container by a conductive wire.

For use in power shuttles: 1 The present invention is constructed as described above, and the oscillator 9 generates an electrical signal due to the electrical connection vibration of 0, 1 to 100 OH2, and the amplifier 10 converts the electrical signal into an output voltage of a required thickness. This output voltage is used to operate a mechanical vibration generator 8, for example, the most common electromagnetic vibrator consisting of an electromagnetic coil and a permanent magnet vibrator, while holding the powdered solid sample 6 in a transferred state by vibration. , metal vapor during evaporation 7
contact with.

It performs the required vapor deposition.

In this case, the rolling of the powdery solid sample 6 is caused by dry friction acting between each particle, and the start time of this rolling is considered to be determined by the shape of the powdery solid sample and the particle size of the material. The required amplitude varies depending on the frequency of the electrical connection vibration that operates the vibration generator. For this reason, the oscillation device 9 needs to be able to change its generation frequency significantly depending on the properties and shape of the powdery solid sample 6, and therefore an amplification device 10 is required to amplify the generated electrical signal. come.

Effects of the Invention As explained above, in this invention, the powdery solid sample 6 on the mechanical vibrator 8 is rolled by vertical, horizontal, horizontal, forward and backward vibrations, so that the entire outer surface is exposed. It is extremely efficient because it allows uniform coating to be applied to the entire surface.

Example Next, the present invention will be explained in more detail with reference to Examples.

Example 1 In the apparatus shown in the above drawing, a glass vacuum vessel (diameter 4201111, height 630111) was used to generate zinc using an oscillation device to coat the surface of flaky glass. After amplifying a weak sine wave with a frequency of 200 Hz to 3 W using an amplification device, it was added to a mechanical vibration generator, and while rolling a glass flake 109 with an average diameter of 105 μm placed on top of it, % I × 10
0.52 zinc for about 1 minute under a vacuum of -5 Torr.
It was found that the zinc-coated flaky glass thus prepared was coated with a zinc layer without any gaps on both sides of the glass flake.

Comparative Example 1 Using the same equipment as in Example 1, zinc was vapor-deposited on flaky glass of the same shape without operating the mechanical vibration generator, and as a result, a film was formed on the lower surface of the flaky glass. Moreover, even on the upper surface, it was not possible to completely form a film on the areas shaded by the overlapping glass flakes. In other words, it was found that the entire film could be formed only on the upper surface, and only on the portion facing the evaporation source.

Example 2 Using exactly the same equipment as in Example 1, activated alumina beads with an average diameter of 3.5 mm were coated with zinc.

That is, after a weak sine wave with a frequency of 50 Hz generated by an oscillation device is amplified to 0.3 W by an amplification device, in addition to a mechanical vibration generator, while rolling activated alumina beads 51, I Zinc was deposited downward by heating to 600°C for 1 minute under a 'Torr vacuum. It was found that the zinc-coated activated alumina beads prepared in this manner were coated with a zinc layer on all surfaces thereof without any gaps.

Comparative Example 2 Using the same equipment as in Example 2, without operating the mechanical vibration generator, and under exactly the same procedures and conditions, zinc was applied to activated alumina beads of the same shape as used in Example 2. Vapor deposition was performed. As a result, we were able to form a film with no gaps on the surface of the activated alumina beads facing the zinc evaporation source, but a slight coating was formed on the opposite surface due to the penetration of zinc vapor. However, it was not possible to form a film on the bottom surface or the part that came into contact with adjacent beads.

[Brief explanation of drawings]

The drawings are explanatory diagrams of the invention. 9... Oscillation device, 10... Amplifying device, 11... Metal holder for vapor deposition.

Claims (1)

[Claims] 1. In a device for depositing a coating substance on the surface of a powdery solid in a vacuum container, the mounting table for the powdery solid is formed into a mechanical vibration generator, and this device is separately provided outside the vacuum container. A powdery solid surface coating device connected to an oscillator via an amplifier.