KR100489301B1 - Manufacturing method for metal film by vacuum evaporation - Google Patents

Abstract

The present invention provides a buffer layer 22 having a thickness of 500 to 1500 kPa on the substrates 6, 21 and 21 'while maintaining the substrates 6, 21 and 21' at room temperature in manufacturing a metal film using vacuum deposition. 22 ') vacuum depositing; Depositing a metal film layer (23, 23 ') on an upper surface of the buffer layer (22, 22'), wherein the evaporation rate of the metal is 0.3 to 0.5 µm / min; Exposing the substrate to which the buffer layers (22, 22 ') and the metal film layers (23, 23') are attached to the atmosphere, and then keeping the substrate at a low temperature; And separating the buffer layers 22, 22 'and the metal film layers 23, 23' from the substrates 6, 21, 21 '(FIG. 2A) or the metal film layers 23, 23'. 22, 22 ') and a separation from the substrate (FIG. 2B) provides a method for producing a metal film.

When manufacturing a film using the method of the present invention, it is possible to produce a small amount of metal films of various thicknesses, it is possible to manufacture the film in an economical and environmentally friendly way because a large rolling facility is unnecessary.

Description

Manufacturing method for metal film by vacuum evaporation

The present invention relates to a metal film production method using vacuum deposition, and more particularly to a metal film production method using vacuum deposition, characterized in that for forming a buffer layer in order to facilitate separation of the substrate and the metal film. .

Vacuum deposition is a kind of physical vapor deposition technique, where physical vapor deposition is a general method for manufacturing a coating on a substrate to be coated by heating the material in a vacuum or plasma atmosphere or by evaporating the coating material by using momentum transfer. Physical vapor deposition is generally well known that it is easy to manufacture a metal film with high purity and smooth surface.

Physical vapor deposition includes vacuum deposition, sputtering, and ion plating. In the case of manufacturing a metal film, vacuum deposition is widely used except for special cases. This is because the vacuum deposition method is relatively simple and the evaporation rate is higher than other methods. Vacuum deposition methods are classified into resistance heating vacuum deposition, electron beam heating vacuum deposition, and induction heating vacuum deposition, depending on the type of heating source and heating method.There are many resistance heating and electron beam heating vacuum deposition methods except for special cases such as industrial large-scale plants. It is used.

Resistance heating vacuum evaporation is a vacuum evaporation method that melts and evaporates a substance contained in an evaporation source by directly passing a current through a refractory metal or an intermetallic compound in the form of a boat, crucible or filament, and evaporating. After the filament to which a high voltage is applied is discharged and an electron is discharged, it concentrates on the copper crucible which becomes water-cooled, and vaporizes a substance and forms a film | membrane. Resistance heating vacuum deposition is used for evaporation of materials having low reactivity and relatively low vaporization temperature, such as copper, zinc, silver, etc., because the entire heating source is heated so that the evaporant reacts with or evaporates. On the other hand, electron beam heating uses water-cooled crucibles, so that virtually all materials on the periodic table can be evaporated.

However, a film prepared by vacuum deposition generally has many pores in the film, so that the film density is different from that of a solid material. Therefore, if the film is to be peeled off with a film, it is easily torn or turned into powder, so that the use as a film is almost impossible and has not been used until now.

Since metal film production by vacuum deposition is limited in this way, in general, the manufacture of a metal film is made by rolling a plate continuously to create a desired thickness. Therefore, large-scale rolling equipment is required for the film production, which is accompanied by an increase in manufacturing cost more than necessary, and the rolled film adversely affects the environment while undergoing various types of surface processing and clean processing. In addition, the metal film by rolling has a disadvantage that there is a limit in making the thickness thin.

Accordingly, it is an object of the present invention to provide a method of manufacturing a metal film of several tens of micrometers by using a vacuum deposition method, by coating a proper peeling buffer layer to easily separate the substrate and the metal film layer.

Another object of the present invention is excellent adhesion to the substrate, but the method of forming a buffer layer having a minimum adhesion to the film to be prepared, and excellent adhesion to the film to be produced, but a minimum adhesion to the substrate It is to provide a film production method of constituting a buffer layer having, to provide a method for producing a metal film that is not torn or differentiation phenomenon.

In order to achieve the above object, the present invention provides a method for manufacturing a metal film using vacuum deposition, comprising: vacuum depositing a buffer layer having a thickness of 500 to 1500 있어서 on the substrate while maintaining the substrate at room temperature; Depositing a metal film layer on an upper surface of the buffer layer, wherein the evaporation rate of the metal is 0.3 to 0.5 µm / min; Exposing the substrate on which the buffer layer and the metal film layer are formed to the air, and then keeping the substrate at a low temperature; And separating the metal film layer having the buffer layer attached thereto from the substrate, or separating the metal film layer from the substrate having the buffer layer attached thereto.

In addition, the present invention is that the substrate is an aluminum plate having an aluminum oxide film formed on the surface, the metal film layer is deposited using a gadolinium (Gd) or dysprosium (Dy) as a source, the buffer layer is deposited by using aluminum as a source It provides a method for producing a metal film characterized by. In addition, the substrate is an iron plate, the metal film layer is deposited using a gadolinium (Gd) or dysprosium (Dy) as a source, the buffer layer is manufactured by using a chromium (Cr) as a source of the manufacture of a metal film Provide a method.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

The present invention utilizes the physical vapor deposition method described above.

FIG. 1 is a manufacturing system for producing a film by the method of the present invention, and FIG. 2 schematically shows a coating layer constituted for producing the present metal film. 3 is a photograph of a gadolinium film produced by the method of the present invention.

As shown in Figure 2, the metal film according to the present invention can be produced by the method of Figures 2a and 2b. In the case of Fig. 2A, the buffer layer 22 and the metal film layer 23 are separated from the substrate 21, so that the metal film to which the buffer layer 22 is attached is manufactured. In the case of Fig. 2B, the metal film layer 23 'is separated from the substrate 21' and the buffer layer 22 ', so that a metal film made of only the metal film layer 23' is produced.

Referring to the method of manufacturing a metal film using vacuum deposition according to the present invention.

The substrates 6, 21, 21 'were kept at room temperature, and the substrates 6, 21, 21' were vacuum-deposited with buffer layers 22, 22 'having a thickness of 500-1500 Å. When the vacuum deposition is performed without maintaining the substrates 6, 21, 21 'at room temperature, latent heat is generated to increase the temperature of the substrates 6, 21, 21'. At this time, if the elevated temperature of the substrates 6, 21, 21 'is not maintained at room temperature, metal-to-metal mixing may occur.

Therefore, when vacuum deposition is performed without maintaining the substrates 6, 21, 21 'at room temperature, in the case of FIG. 2A, the buffer layer 22 is in close contact with the substrate to separate the buffer layer 22 from the substrate 21. Since it may be difficult, there is a fear that it is difficult to manufacture a metal film to which the buffer layer 22 is attached. In addition, when vacuum deposition is performed without maintaining the substrates 6, 21, and 21 'at room temperature, in the case of FIG. 2B, the buffer layer 22' and the metal film layer 23 'are brought into close contact with each other to form the metal film layer 23. ') May be difficult to separate from the buffer layer 22', which may make it difficult to manufacture a metal film composed of only the metal film layer 23 '.

The buffer layers 22 and 22 'have a thickness of 500 to 1500 kPa, more preferably 700 to 1500 kPa. If the thickness of the buffer layers 22 and 22 'is less than 500 mm, complete coating may be difficult, and when the buffer layers 22 and 22' are separated from the substrate 21 or the metal film layer 23 ', The buffer layers 22 and 22 'may be torn or may cause differentiation.

In the case of FIG. 2A when the thickness of the buffer layers 22 and 22 'exceeds 1500 mm, the substrate 21 and the buffer layer 22 may be in close contact with each other, which may make it difficult to separate the buffer layer 22 from the substrate 21. There is a fear that the production of the metal film with (22) becomes difficult. In addition, when the thickness of the buffer layers 22 and 22 'exceeds 1500 mm, in the case of FIG. 2B, the buffer layer 22' and the metal film layer 23 'are brought into close contact with each other, and the metal film layer 23' is brought into contact with the buffer layer 22 '. Since it may be difficult to separate the metal film from the metal film, it may be difficult to manufacture the metal film composed of the metal film layer 23 'only. Therefore, the buffer layers 22 and 22 'outside the thickness range may not serve as buffer layers.

After the deposition of the buffer layers 22 and 22 'is completed, the metal film layers 23 and 23' are deposited on the top surfaces of the buffer layers 22 and 22 ', and the evaporation rate of the metal is 0.3 to 0.5 µm / min. Be sure to If the evaporation rate is less than 0.3㎛ / min it may be uneconomical to increase the deposition time.

In addition, when the evaporation rate is more than 0.5㎛ / min, the temperature of the buffer layer (22, 22 ') may increase due to latent heat. Therefore, in the case of FIG. 2A, since the substrate 21 and the buffer layer 22 are in close contact with each other, it may be difficult to separate the buffer layer 22 from the substrate 21. Therefore, it is difficult to manufacture the metal film with the buffer layer 22. There is a risk of loss. In addition, in the case of FIG. 2B, since the buffer layer 22 ′ and the metal film layer 23 ′ are in close contact with each other, it may be difficult to separate the metal film layer 23 ′ from the buffer layer 22 ′. It may be difficult to manufacture a metal film made of only ').

After the deposition of the metal film layers 23 and 23 'is completed, the substrate on which the buffer layers 22 and 22' and the metal film layers 23 and 23 'are formed is exposed to the air and then kept at a low temperature. The buffer layer 22 and the metal film layer 23 are separated from the substrate 21 by using the stress generated at this time, or the metal film layer 23 'from the buffer layer 22' and the substrate 21 '. To separate.

When the metal film layers 23 and 23 'are separated from the substrates 21 and 21' after the deposition of the metal film layers 23 and 23 'is completed, the buffer layers 22 and 22' and the metal film layers are separated. The substrates 21 and 21 'on which the (23, 23') are attached are exposed to the air, and then kept at a low temperature. Preferably, the substrates 21 and 21 'are attached to a temperature below the normal temperature.

In the case of FIG. 2A, since the buffer layer 22 has minimal adhesion to the substrate 21 and excellent adhesion to the metal film layer 23, when the stress is generated at a low temperature, the substrate 21 has less adhesion. The silver buffer layer 22 is separated from the attached metal film.

In the case of FIG. 2B, since the buffer layer 22 ′ has excellent adhesion with the substrate 21 ′ and minimal adhesion with the metal film layer 23 ′, the metal has little adhesion when stress occurs at low temperatures. The film layer 23 'is separated from the substrate to which the buffer layer 22' is attached.

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

As the film production apparatus used in the above embodiment, as shown in Fig. 1, a deposition system equipped with a conventional electron beam evaporation source 2 was used. The electron beam evaporation source 2 used a copper crucible consisting of four pockets to form a base layer.

A metal film to which the buffer layer 22 was attached was prepared by the method of FIG. 2A, but a gadolinium film having a thickness of 15 μm was prepared. The substrates 6 and 21 used in the embodiment of FIG. 2A were aluminum plates having a thickness of 1 mm and width and length of 200 mm, respectively, and an aluminum oxide film was formed on the surface thereof. The surface on which the buffer layer is formed in the aluminum plate was mirrored through buffer polishing. The reason why the substrate was mirrored was to even out the growth of the film and to allow the film to peel off easily from the substrate.

The substrate was subjected to ultrasonic cleaning using acetone and alcohol for cleaning, and then mounted on the substrate holder 7 in the vacuum chamber 1. Next, aluminum and gadolinium, which are the film forming materials 3, were placed in the electron beam evaporation source 2, and then the vacuum chamber 1 was closed and evacuated using a vacuum pump (not shown). When the degree of vacuum became 10 ⁻⁵ Torr or less, aluminum metal used as the buffer layer 22 was deposited to a thickness of 700 kPa to facilitate the peeling of the film and to control the growth mode.

The reason why aluminum is used as the buffer layer 22 is as follows. First of all, aluminum is deposited relatively easily even at low temperatures.

It is possible and good ductility makes it possible to deposit evenly. In addition, since the substrate 21 is an aluminum plate on which an aluminum oxide film is formed, the aluminum buffer layer 22 is easily separated from the aluminum oxide present on the substrate 21. The thickness of the aluminum buffer layer 22 is preferably 500 to 1500 kPa, and more preferably 700 to 1500 kPa, because when the thickness of the aluminum is too thin or too thick, the aluminum buffer layer 22 does not function properly as a buffer layer.

When the aluminum buffer layer 22 is deposited, the power of the electron beam evaporation source 2 is adjusted to 8 kV and 140 mA so that the evaporation rate is about 400 kW per minute, which is a condition in which aluminum can evaporate most efficiently.

After the deposition of the aluminum buffer layer 22 was completed, the gadolinium film layer 23 was prepared in earnest. After the deposition of the aluminum buffer layer 22 was completed, the pocket was moved to the place containing gadolinium, and then a gadolinium film layer 23 was deposited on the upper surface of the buffer layer 22 to a thickness of 15 μm. When the gadolinium film layer 23 was deposited, the power of the electron beam evaporation source 2 was adjusted to 8 kV and 300 mA so that the evaporation rate was 0.5 μm per minute. The deposition rate of the gadolinium is 0.3 ~ 0.5㎛ / min, this evaporation rate has become an important parameter in controlling the growth mode of the gadolinium film. During the gadolinium deposition, the thickness of the film was monitored by using a thickness gauge 10 using quartz single crystal, and the substrate was rotated five times per minute by using the substrate rotating apparatus 9 to evenly distribute the thickness.

Next, the substrate on which the buffer layer 22 and the metal film layer 23 were deposited was taken out in the air, and the film was peeled off. In order to keep the substrate exposed to the atmosphere as low as possible, the substrate 21 was cooled by spraying water on the back of the film or by blowing extruded air. When this is maintained for several minutes, the film is peeled off from the edge of the substrate 21. The peeled film is peeled off slowly to obtain a metal film with the buffer layer 22 attached thereto. The reason for keeping the substrate at a low temperature during peeling of the film was that when the substrate 21 became low temperature, the stress of the film became larger, and thus peeling easily occurred.

As another embodiment of the present invention, a metal film layer 23 'having a buffer layer 22' separated by the method of FIG. 2B was prepared, and a gadolinium film having a thickness of 15 μm was prepared. The embodiment of FIG. 2B was carried out in the same manner as the embodiment of FIG. 2A, except that the substrate 21 'used was an iron plate having a thickness of 1 mm and a width of 200 mm in length and width, respectively, and the buffer layer 22' was made of chromium (Cr). Evaporated).

The reason why the substrate 21 'and the buffer layer 22' were used as the iron plate and chromium was because the adhesion between iron and chromium was very large and the adhesion between chromium and gadolinium was small. That is, when the iron substrate 21 'to which the chromium buffer layer 22' and the gadolinium metal film layer 23 'are attached is exposed to the air, and kept at a low temperature, the buffer layer 22' is the substrate 21 '. ) And separated from the metal film layer 23 '.

Accordingly, the metal film may be manufactured in the form of FIG. 2A or 2B by appropriately selecting materials of the substrates 21 and 21 ', the buffer layers 22 and 22', and the metal film layers 23 and 23 '. That is, in the case of FIG. 2A, a buffer layer 22 having excellent adhesion with the film 23 to be manufactured but having a minimum adhesion with the substrate 21 is formed to form a metal film having the buffer layer 22 attached thereto. It can manufacture. In addition, in the case of FIG. 2B, a buffer layer 22 'having an excellent adhesion with the substrate 21' but a minimum adhesion with the film 23 'to be manufactured is constructed, and thus the metal film layer 23' is formed. It is possible to produce a single metal film.

When manufacturing a film using the method of the present invention, it is possible to produce a small amount of metal films of various thicknesses, it is possible to manufacture the film in an economical and environmentally friendly way because a large rolling facility is unnecessary.

1 is a cross-sectional view of a film production apparatus for explaining the present invention.

Figure 2a is a cross-sectional view showing the separation of the buffer layer and the metal film layer from the substrate in accordance with an embodiment of the present invention.

2B is a cross-sectional view schematically showing that the metal film layer is separated from the buffer layer and the substrate according to another embodiment of the present invention.

Figure 3 is a photograph of a gadolinium film prepared according to an embodiment of the present invention.

<Description of the symbols for the main parts of the drawings>

1: vacuum chamber 2: electron beam evaporation source

3: coating material 4: evaporation source shutter

5: substrate shutter 6, 21, 21 ': substrate

7: substrate holder 8: substrate heating heater

9 substrate rotating apparatus 10 thickness gauge

22, 22 ': buffer layer 23, 23': metal film layer

Claims (3)

In manufacturing the metal film using vacuum deposition, while maintaining the substrate (6, 21, 21 ') at room temperature, Vacuum depositing a buffer layer (22, 22 ') having a thickness of 500-1500 에 on the substrate (6, 21, 21'); Depositing a metal film layer (23, 23 ') on an upper surface of the buffer layer (22, 22'), wherein the evaporation rate of the metal is 0.3 to 0.5 µm / min; Exposing the substrate on which the buffer layers (22, 22 ') and the metal film layers (23, 23') are formed in the air, and then keeping the substrate at a low temperature; And separating the buffer layer 22 and the metal film layer 23 from the substrate 21, or separating the metal film layer 23 ′ from the buffer layer 22 ′ and the substrate 21 ′. Method for producing a metal film comprising a. According to claim 1, wherein the substrate (6, 21) is an aluminum plate having an aluminum oxide film formed on the surface, the metal film layer 23 is deposited using a gadolinium (Gd) or dysprosium (Dy) as a source, the buffer layer (22) is a method for producing a metal film, characterized in that deposited by using aluminum as a source. The method of claim 1, wherein the substrate (6, 21 ') is an iron plate, the metal film layer 23' is deposited using a gadolinium (Gd) or dysprosium (Dy) as a source, the buffer layer 22 ' Method for producing a metal film, characterized in that deposited by chromium (Cr) as a source.