KR100430410B1 - Manufacturing method of Aluminum films by ion plating - Google Patents

Abstract

The disclosed method for producing an aluminum coating includes a vacuum chamber in which a coating treatment is performed; A barrel fixed to the upper portion of the vacuum chamber and having a specimen installed therein; An electron beam evaporation source provided below the vacuum chamber opposite to the barrel; A shutter installed between the barrel and the electron beam evaporation source; A filament and an ionization electrode installed at one side of the electron beam evaporation source; A method of forming an aluminum film on a specimen mounted to the barrel by using an ion plating apparatus including a specimen heating device installed between the shutter and the barrel, wherein the initial voltage is applied to the barrel at about 300V to 600V. After the deposition for 60 minutes, the voltage was lowered by 50 to 100 V for 1 hour and 30 minutes, and a current of 40 to 60 A was flowed through the filament, a voltage of 40 to 70 V was supplied to the ionization electrode, and a current of 400 to 800 mA was applied to the barrel. It is characterized in that the ion plated by heating the specimen to 200 ℃ by the specimen heating device to flow. According to this, it is possible to shorten the cleaning time of the specimen, to improve the adhesion and corrosion resistance, and to economically produce a coating having improved coating reliability.

Description

Manufacturing method of aluminum film by ion plating {Manufacturing method of Aluminum films by ion plating}

The present invention relates to a method for manufacturing an aluminum film, and more particularly, to ion plating to improve adhesion, corrosion resistance and film reliability by adjusting a bias voltage applied to a substrate by an ion plating method using an electron beam evaporation method. It is related with the manufacturing method of the aluminum film by this.

Generally, aluminum (Al) is a silver-white, light and soft element having a specific gravity of 2.7 and a melting point of 660 ° C., and is a metal that is easy to process due to its rich stretchability and spreadability. Such aluminum has been widely applied in the industrial field due to the properties of metals, that is, a low density, and excellent workability, corrosion resistance and thermal conductivity.

In recent years, as the space development and the aviation industry have greatly developed, research has been conducted to improve the corrosion resistance and mechanical properties by coating aluminum on various materials.

For example, McDonald's Douglas, USA, uses aluminum as an ion-plating material for various parts used in airplanes as a corrosion and wear resistant material.In Germany, aluminum is vacuum-deposited on steel sheets to be used for storage can materials and home appliances. Doing. In addition, it is widely applied in various fields such as decorative coatings used for wrapping paper, various accessories, and conductive thin film materials for semiconductors.

On the other hand, the general aluminum coating was coated with an electroplating, in this case, the efficiency was low, there was a disadvantage in lowering productivity. In order to solve this disadvantage, a physical vapor deposition method is used.

Such physical vapor deposition methods include vacuum deposition, sputtering, and ion plating. In order to improve corrosion resistance, ion plating is mainly used.

The ion plating method is a kind of physical vapor deposition technology developed by Mattox in 1963, and is a coating method in which vapor evaporated in a vacuum state is ionized in a plasma layer to accelerate and attach to a cathode, which is a plated body, Not only the deposition material but also gas, ions, and the like are incident and collided with the plated body, so that the densification and adhesion of the coating layer can be improved.

The aluminum film coated by the physical vapor deposition method as described above has a disadvantage in that not only a large number of holes are formed in the coating layer, but also poor adhesion to the substrate. In order to solve this problem, the substrate is heated to a high temperature in the case of vacuum deposition. In ion plating, a larger amount of discharge gas must be introduced to increase the voltage applied to the substrate or to increase the ionization rate.

However, when the substrate is heated to a high temperature as described above, not only the substrate is damaged but also the adhesion amount decreases as the substrate becomes a high temperature, so that economic efficiency is lowered, and a method of applying a high voltage to the substrate also damages the substrate.

In addition, to increase the ionization rate by increasing the amount of discharge gas introduced as described above, the discharge gas is mixed into the film to damage the film, and scattering occurs between the discharge gas and the evaporated aluminum, resulting in a decrease in adhesion amount.

In order to solve the above problems, various methods of vacuum deposition, sputtering, ion plating apparatus or method (Japanese Patent Notification 59-28569, Japanese Patent Notification 61-59861, British Patent Publication 2141442, Japanese Country) Patent notification fire extinguishing 57095749, British Patent 2162205, Japanese Patent 7942676) has been developed, mainly to improve the uniformity of the film and the adhesion between the film and the substrate, the stability of the generated plasma, the material and structure of the evaporation source, high ionization rate, etc. It was.

In addition, the inventors of the present application in order to solve the above problems, the film formation method excellent in adhesion and surface properties (Korean patent application 96-71544), a high corrosion-resistant aluminum film production method for small sintered parts (Korean patent application 97-72392) And a method of manufacturing an aluminum film having improved adhesion and density (Korean Patent Application No. 99-57106), and the like, have been filed.

However, when coating the sintered parts or coating a large amount of specimens at once, and when using the product in the harsh conditions, the problem that the adhesion strength according to the surface condition and deposition conditions of the specimens has emerged.

Accordingly, the present invention has been made to solve the above problems, the ion plating method using an electron beam evaporation method, the ion to improve the adhesion, corrosion resistance and film reliability by adjusting the bias voltage applied to the substrate It is an object to provide a method for producing an aluminum film by plating.

1 is a schematic view showing an aluminum film production apparatus according to the present invention,

2 is a chart showing the variation of the bias voltage during the film production process according to the present invention,

Explanation of symbols on the main parts of the drawings

One; Vacuum chamber 2; Electron beam evaporation source

3; Ionization electrode 4; filament

5; Shutter 6; Thickness monitor

7; Specimen heating apparatus 8; Barrel

9; Vacuum gauge 10; Gas injection device

11; Psalm 12; aluminum

13; Wire feeder

Method for producing an aluminum film by ion plating according to the present invention for achieving the object as described above, the vacuum chamber in which the film treatment is performed; A barrel fixed to the upper portion of the vacuum chamber and having a specimen installed therein; An electron beam evaporation source provided below the vacuum chamber opposite to the barrel; A shutter installed between the barrel and the electron beam evaporation source; A filament and an ionization electrode installed at one side of the electron beam evaporation source; A method of forming an aluminum film on a specimen mounted to the barrel by using an ion plating apparatus including a specimen heating device installed between the shutter and the barrel, wherein the initial voltage is applied to the barrel at about 300V to 600V. After the deposition for 60 minutes, the voltage was lowered by 50 to 100 V for 1 hour and 30 minutes, and a current of 40 to 60 A was flowed through the filament, a voltage of 40 to 70 V was supplied to the ionization electrode, and a current of 400 to 800 mA was applied to the barrel. It is characterized in that the ion plated by heating the specimen to 200 ℃ by the specimen heating device to flow.

Hereinafter, with reference to the accompanying drawings will be described in more detail the configuration and operation of the apparatus and method for producing an aluminum film according to an embodiment of the present invention.

1 is a configuration diagram schematically showing an apparatus for manufacturing an aluminum film according to the present invention.

In the figure, reference numeral 1 denotes a vacuum chamber, in which one side of the vacuum chamber 1 is provided with an ionization electrode 3, and one side of the ionization electrode 3 is provided with a filament 4.

On the other side of the vacuum chamber 1, a wire supply device 13 for continuously supplying aluminum is installed, and on one side of the wire supply device 13, a gas injection device 10 for injecting gas is provided in the vacuum chamber 1. It is installed through the lower part.

Between the gas injection device 10 and the filament (4) is provided an electron beam evaporation source (2) provided with aluminum supplied from the wire supply device (13). Here, it is preferable that the electron beam evaporation source 2 uses an alumina crucible for improving the evaporation rate.

In addition, a shutter 5 is disposed across the center of one side of the vacuum chamber 1, and a vacuum gauge 9 for measuring the vacuum of the vacuum chamber 1 on the upper part of the shutter 5 communicates with the vacuum chamber 1. Is installed.

Then, the thickness monitor 6 for measuring the thickness of the aluminum film coated on the specimen is installed inside the opposite vacuum chamber 1 in which the vacuum gauge 9 is installed. In addition, a specimen heating device 7 for heating the specimen is provided on both inner walls of the vacuum chamber 1 above the thickness monitor 6 and the vacuum gauge 9. On the upper side of the specimen heating device 7 is installed a barrel 8 into which the specimen 11 is inserted across the vacuum chamber 1 horizontally. Here, the barrel 8 is also called a board | substrate.

The manufacturing method of the aluminum film by the aluminum film production apparatus according to the present invention configured as described above will be described.

First, prior to loading the specimen 11 into the barrel (substrate) 8, pretreatment is performed using sand blasting to remove contaminants from the specimen 11. When the pretreatment of the specimen 11 is completed in this way, the specimen 11 is charged into the barrel 8. After filling the electron beam evaporation source 2 with aluminum, the vacuum chamber 1 is exhausted to a desired degree of vacuum using a vacuum pump (not shown). Here, the degree of vacuum of the vacuum chamber (1) is less than approximately 10 ^-5 Torr (torr). When the vacuum degree of the vacuum chamber 1 is 10 ⁻⁵ torr or less, argon gas is injected into the gas injection device 10 to clean the specimen 11, and a negative voltage is applied to the specimen 11. To clean the specimen (11).

Here, the cleaning of the specimen 11 is intended to remove not only impurities such as organic matter present in the specimen 11 but also naturally occurring oxide films, and argon having a degree of vacuum of about 10 ⁻² torr (torr). In a gas atmosphere, a negative voltage of 400 to 1000 V is applied to the specimen to induce glow discharge. In this way, when a negative voltage is applied to the specimen 11 to induce a glow discharge, the argon ions present in the discharge region collide with the specimen 11 to remove impurities present in the specimen 11.

As described above, when the cleaning of the specimen 11 is finished, the vacuum degree of the vacuum chamber 1 is maintained at 10 ⁻⁵ Torr or less again, and then a voltage of 40 to 70 V is applied to the ionization electrode 3. Then, a current of 40 to 60 A is applied to the filament 4 to increase the current of the evaporation source 2 to evaporate aluminum. The temperature of the evaporation source 2 rises and aluminum is evaporated. In this way, aluminum is evaporated and ion plating is performed on the specimen 11 charged in the barrel 8. As such, when ion plating is completed in a vacuum state, the specimen 11 is taken out of the vacuum chamber 1, and then polished using sand blasting to remove surface roughness and make a surface for metallic luster. This completes the manufacture of the aluminum film.

Hereinafter, the present invention will be described in more detail with reference to Examples.

Example 1

According to the general performance mode of the Al film forming method of the present invention described above, the evaporation rate is 0.5 μm / min, the initial voltage applied to the barrel (substrate) is 400 V, and the initial voltage is applied for about 30 minutes, and finally the substrate A voltage of 100 V was applied to the aluminum film. The adhesion, corrosion resistance, and reliability of the Al film thus calculated to the substrate are shown in detail in Table 1 below.

Example 2

An Al film was prepared in the same manner as in Example 1 except that the evaporation rate was 1.0 μm / min, the initial applied voltage was 500 V, the voltage applied time was 1 hour, and the final applied voltage was 50 V. The adhesion to the substrate, the corrosion resistance, and the reliability thereof are shown in detail in Table 1 below.

Example 3

An Al film was prepared in the same manner as in Example 1 except that the evaporation rate was 0.3 μm / min, the initial applied voltage was 500 V, the voltage application time was 30 minutes, and the final applied voltage was 100 V. The adhesion to the substrate, the corrosion resistance, and the reliability thereof are shown in detail in Table 1 below.

Example 4

An Al film was prepared in the same manner as in Example 1 except that the evaporation rate was 1.2 μm / min, the initial applied voltage was 300V, the voltage application time was 1 hour, and the final applied voltage was 50V. The adhesion to the substrate, the corrosion resistance, and the reliability thereof are shown in detail in Table 1 below.

Example 5

An Al film was prepared in the same manner as in Example 1 except that the evaporation rate was 1.2 μm / min, the initial applied voltage was 600 V, the voltage applied time was 30 minutes, and the final applied voltage was 50 V. The adhesion to the substrate, the corrosion resistance, and the reliability thereof are shown in detail in Table 1 below.

Comparative Example 1

An Al film was prepared in the same manner as in Example 1 except that the evaporation rate was 0.5 μm / min, the initial applied voltage was 200 V, the voltage application time was 30 minutes, and the final applied voltage was 100 V. The adhesion to the substrate, the corrosion resistance, and the reliability thereof are shown in detail in Table 1 below.

Comparative Example 2

The Al film was manufactured in the same manner as in Example 1 except that the evaporation rate was 0.5 μm / min and the initial voltage was not applied, and the final applied voltage was 100 V. Thus, the Al film thus obtained was subjected to adhesion, corrosion resistance, and reliability. Is shown in detail in Table 1 below.

Comparative Example 3

An Al film was prepared in the same manner as in Example 1 except that the evaporation rate was 0.5 μm / min, the initial applied voltage was 400V, the voltage application time was 15 minutes, and the final applied voltage was 100V. The adhesion to the substrate, the corrosion resistance, and the reliability thereof are shown in detail in Table 1 below.

Comparative Example 4

The Al film was manufactured in the same manner as in Comparative Example 2 except that the evaporation rate was 1.2 μm / min and the initial voltage was not applied, and the final applied voltage was 50 V. Thus, the Al film thus obtained was subjected to adhesion, corrosion resistance, and reliability to the substrate. Is shown in detail in Table 1 below.

Comparative Example 5

An Al film was prepared in the same manner as in Example 1 except that the evaporation rate was 0.5 μm / min, the initial applied voltage was 400 V, the voltage application time was 3 hours, and the voltage was not changed. The adhesion to the substrate, corrosion resistance, and reliability are shown in detail in Table 1 below.

Table 1

NO Evaporation rate (㎛ / min) Initial Board Voltage (V) Initial voltage application time Final substrate voltage (V) Adhesion Corrosion resistance Reliability Example 1 0.5 400 30 minutes 100 Prize Prize Prize Example 2 1.0 500 1 hours 50 Prize Prize Prize Example 3 0.3 500 30 minutes 100 Prize Prize Prize Example 4 1.2 300 1 hours 50 Prize Prize Prize Example 5 1.2 600 30 minutes 50 Prize Prize Prize Comparative Example 1 0.5 200 30 minutes 100 medium Ha medium Comparative Example 2 0.5 - - 100 medium medium Ha Comparative Example 3 0.5 400 15 minutes 100 medium medium medium Comparative Example 4 1.2 - - 50 Ha Ha Ha Comparative Example 5 0.5 400 3 hours 400 Prize Ha medium

In Table 1, characteristics such as adhesion, corrosion resistance, and film reliability were compared in three steps through the following test.

The adhesive force is tested by using a tape test and a scratch tester, and the comparative examples 1 to 5, the case of the very excellent adhesion to the 'phase', the middle case 'mid', the case where the Al film falls even with the tape 'Ha' is indicated.

In addition, the corrosion resistance of the film is tested by the PCT (Pressure Humidity Test) test at a test temperature of 121 ° C., a relative humidity of 100%, and a pressure of 2 atm, with observing rust, bubble generation, plating cracking, Investigate plating peeling, etc., and the case of no abnormality within 20 hours is set to 'high'. Indicated.

In addition, the reliability of the film is a comparison of the ratio of defective products produced by the inspection and evaluation of the coating layer after coating to coat 1000 disc-shaped permanent magnets having an outer diameter of 23mm at once, the rate of occurrence of defective products Less than 1% is indicated as 'up', between 1 and 5% is indicated as 'medium', and more than 5% as 'low'.

As described above, according to the present invention, it is possible to shorten the clean time of the test piece, improve adhesion and corrosion resistance, and have an advantage of economically manufacturing a film having improved film reliability.

Claims (2)

A vacuum chamber in which the film treatment is performed; A barrel fixed to the upper portion of the vacuum chamber and having a specimen installed therein; An electron beam evaporation source provided below the vacuum chamber opposite to the barrel; A shutter installed between the barrel and the electron beam evaporation source; A filament and an ionization electrode installed at one side of the electron beam evaporation source; In the method for forming an aluminum film on the specimen mounted to the barrel by using an ion plating apparatus including a specimen heating device installed between the shutter and the barrel, An initial voltage of about 300V to 600V was applied to the barrel for 30 to 60 minutes, and then the voltage was lowered to 50 to 100V for 1 hour and 30 minutes, and a current of 40 to 60 A flowed to the filament, and 40 to the ionization electrode. A method of producing an aluminum coating by ion plating, wherein a voltage of 70 V is applied to the barrel and a current of 400 to 800 mA flows, thereby heating the specimen to 200 ° C. with the specimen heating device. The method of manufacturing an aluminum film by ion plating according to claim 1, wherein the electron beam evaporation source is an alumina crucible.