JPH07102366A - Thin film forming device - Google Patents

Abstract

PURPOSE:To prevent the peeling and scattering of stuck deposits and to enable the reprocessing use by constituting apparatus or constituting parts in a thin film forming device of a contamination preventing material obtd. by coating the surface of Ti or a Ti alloy with an Al or Al alloy layer. CONSTITUTION:The surface of a substrate holder 5 arranged in a sputtering chamber 1 is mounted with a substrate 4, a target 6 is oppositely arranged on a cathode 7 across a shutter plate 9, and the circumference is provided with a shield plate 8. A reaction gas is introduced into the sputtering chamber 1 from a gas introducing port 2, the target is sputtered, and sputtering grains are deposited on the substrate 4 to form a thin film. In the thin film forming device, apparatus or constituting parts therein such as a shield plate 8, a shutter plate 9 and a substrate holder 5 are constituted of a contamination preventing material obtd. by coating the surface of Ti or a Ti alloy with an Al layer or an Al alloy layer. Thus, the peeling and scattering of stuck deposits from the apparatus and parts is prevented in the process of the formation of a thin film, and the deformation and gaseous release caused by the heat and stress in the apparatus or the like are prevented.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thin film forming apparatus,
More specifically, contaminants adhere to the equipment or components in the equipment used to physically or physically form a thin film on a substrate in a vacuum, and this reattaches to the thin film formed on the substrate. The present invention relates to a thin film forming apparatus for preventing this.

[0002]

2. Description of the Related Art As a thin film forming method for physically or physicochemically forming a thin film on a substrate in vacuum, there are vapor phase growth methods such as vacuum deposition, sputtering and plasma CVD. Widely used. As a factor that significantly impairs the quality of the thin film formed on the substrate by the above method, there is a problem that fine particles, which are said to be particles having a diameter of about submicron or more, are taken into the thin film.

The particle generation source may be related to the purity or density of the thin film forming material, or may be related to contaminants caused by peeling and scattering of deposited deposits adhered to equipment or components in the thin film forming apparatus. There is. As a solution to the latter pollutants that have been industrially studied in various ways, the empirical rule is to adhere to the equipment or components inside the equipment physically or mechanically at each batch process during production. Removes adhered deposits and cleans them. Covers equipment or components inside the equipment with foils of aluminum (Al), copper (Cu), etc., and removes and removes them for each batch processing. Shield plate, shutter plate, substrate Making holders and the like processed products of aluminum or stainless steel Spray coating aluminum or molybdenum on the surface of processed products of titanium or stainless steel. It is known to perform spot welding to cover equipment or components with processed copper foil.

[0004]

A specific problem of a conventional technique for preventing contamination in a thin film forming apparatus on a substrate, which has been conventionally practiced, will be described by taking a sputtering apparatus as an example. The particle contaminants generated in the sputtering apparatus are the deposits deposited on the equipment, components and the like in the apparatus by sputtering, and are separated and scattered by physical and mechanical actions such as adhesion and thermal expansion stress.

As a preventive measure against these problems, a physical treatment may be performed for each batch treatment or depending on the amount of deposited deposits.
Remove deposits chemically or mechanically. In this case, a) the surface condition (cleanliness, roughness, residual stress) of the equipment and component materials changes with each cleaning process (removal of adhered deposits), resulting in an increase in particle generation. The cleaning process requires 20% or more of the actual thin film formation time, and there are problems such as low productivity and workability.

Equipment and components in the apparatus are covered with aluminum or copper foil, and removed by each batch process or by the amount of deposited deposits. In this case, a) Deposition of the foil that occurs during removal work inside the equipment causes the deposited deposits to separate from the foil surface and scatter to become a particle generation source. B) Attached as the amount of deposited deposits increases. Deformation of the foil occurs due to the internal stress of the deposits, peeling and scattering causes particles to be generated. C) There is a problem that the coating foil is removed and then discarded, which is not economical. .

Equipment and components such as shield plates, shutter plates, and substrate holders where the amount of adhered deposits is particularly remarkable are processed products of aluminum and copper. In this case, a) the thermal deformation due to the heat generated during sputtering and the internal stress of the deposited deposits cause abnormal sputtering conditions, especially abnormal discharge, resulting in variations in thin film quality and deposits. Particles are generated due to peeling and scattering. (2) Similar to the above-mentioned coating foil, since it is discarded and discarded, it is economically disadvantageous.

A spray coating layer of aluminum or molybdenum is formed on the surface of equipment such as a shield plate, a shutter plate, a substrate holder, and processed products of components (titanium, stainless steel). In this case, a) the adhesion of the thermal spray coating layer to titanium and stainless steel is about 20 to 30% of the strength of the thermal spray base material, so the internal stress due to the increase of deposits causes delamination and scattering to generate particles. B) The density of the thermal spray coating layer is 80% of the density of the thermal spray base metal.
%, So there are a lot of occluded impure gases, which causes variations in thin film quality due to gas release during sputtering and the generation of particles due to abnormal discharge. C) Cohesive force between sprayed particles at irregularities or holes in components Is weak and is a source of particles.

Spot welding is performed so that the surface of the device or component is covered with a bellows- or embossed copper foil. In this case, a) foreign matter is mixed in each process such as a) bellows of copper foil or forming into embossed shape, spot welding of uneven copper foil on the surface of equipment or component parts, especially from spot welding part (2) Unevenness (bellows, embossed pattern) of copper foil, holes, etc., which are sources of thin film quality variations and particles due to abnormal discharge due to gas release from the product, become uncoverable parts during spot welding. (3) Particles are generated, and c) Formed copper foil is removed and then discarded, which is not economical.

The present invention solves the above-mentioned problems, prevents adhered deposits from being separated from the equipment or components during film formation of a thin film on a substrate, and does not scatter. It is an object of the present invention to provide a thin film forming apparatus which does not undergo deformation and gas release due to stress and which can be reprocessed and used and which is internally equipped with components and components.

[0011]

Means for Solving the Problems As a result of intensive studies to achieve the above-mentioned object, the present inventors formed equipments and components with titanium or its alloy, and aluminum or its alloy in a molten state on its surface. It has been found that it is optimal to install and use a processed product which is coated to form an aluminum layer or an aluminum alloy layer as a device or a component in a thin film forming apparatus.

The present invention has been made on the basis of the above findings. A thin film forming apparatus is a thin film forming apparatus for forming a thin film on a substrate in a vacuum, and a device or a component in the thin film forming apparatus is made of titanium or It is characterized in that it is composed of a pollution control material in which a surface of a titanium alloy is coated with an aluminum layer or an aluminum alloy layer. The device or component in the thin film forming apparatus is a target shield plate, shutter plate, or substrate holder.

[0013]

The thin film formed on the substrate of the device or component during film formation because the device or component is composed of a pollution-preventing material in which the surface of titanium or a titanium alloy is coated with an aluminum layer or an aluminum alloy layer. When the fine particles of the material adhere, they are surely adhered and accumulated and do not peel off easily, so that no particles are generated from the device or the component during film formation or inspection, and no occluded gas is released.

[0014]

Embodiments of the present invention will be described below with reference to the accompanying drawings.

First, equipment or components (hereinafter referred to as equipment) such as a target shield plate, a shutter plate, and a substrate holder, which are provided in the thin film forming apparatus, will be described.

For example, a titanium plate having a thickness of 1 mm is subjected to a vacuum annealing treatment, and then a finishing process is performed to a predetermined size of the equipment, and the surface is washed with acetone or the like. At the time of the dimensional finishing process, the roughness of the finished surface of the equipment does not cause any particular problem, but the surface roughness of about # 400 has a good coating formability of the subsequent aluminum layer or aluminum alloy layer.

Next, the equipment is placed in a melting crucible of aluminum which is heated and melted to 700 to 800 ° C. by induction or the like in an argon gas having a degree of vacuum of about 5 × 10 ⁻⁵ Torr, for example, a purity of 99.999%. 0.5 to
After soaking for 1.0 minute, the aluminum crucible is immediately pulled up from the melting crucible and naturally cooled in the furnace to form an aluminum layer on the surface of a titanium device. The aluminum melting crucible is preferably made of high-purity high-density graphite, and the
Any material that has been subjected to a heat degassing treatment at ˜1500 ° C. may be used, and if a vacuum melting aluminum material is used as a melting material for forming a coating on the surface of the equipment, the adhesion strength of the aluminum coating forming film to the equipment surface, Significant improvements in quality such as purity and pinhole-free.

In the case of a device having a surface coated with an aluminum layer, in the case of a target shield plate, shutter plate, etc. on which the amount of deposited deposits is remarkably increased, the thickness of the aluminum layer is set to about 200 to 500 μm. It is preferable that the aluminum layer on which the columnar recessed groove processing has been formed is subjected to molding processing, and then subjected to heat treatment at a temperature of 550 to 600 ° C. for a time of 20 to 30 minutes. In addition, depending on the structure of the device, work molding may be performed before forming the aluminum layer on the surface of the titanium material by coating.

When deposits adhere to the surfaces of these devices and the devices are used up, the concentration of the devices is 15%.
After immersing in the hydrochloric acid solution of No. 1 and performing a reaction treatment until a black titanium surface appears to remove the deposited deposits and the aluminum layer, it is pulled up from the hydrochloric acid solution and washed with water. Then HF, H
Pickling is performed with a mixed acid solution of NO ₃ and H ₂ SO ₄ at room temperature. And after the metallic surface of titanium appears, wash it with water,
Properly dry and store. By this treatment, the titanium material of the equipment itself causes a thickness loss of about 5 to 6 μm / cycle, but with a titanium thickness of 0.5 mm, it can be reused about 10 times in terms of strength, which is an economic advantage. Is big.

The equipment subjected to the regeneration treatment can be reused because the aluminum layer is coated on the surface of the regeneration equipment by subjecting the equipment to the immersion treatment (dip) in the vacuum-melted aluminum under the above conditions.

As described above, the antifouling material of the present invention directly coats aluminum on the surface of titanium using a high-purity high-density graphite crucible and vacuum-melted aluminum in a vacuum degree of about 5 × 10 ⁻⁵ Torr. Therefore, it is possible to provide a high-quality aluminum-coated pollution control material.

Next, a titanium member (for example, a thickness of 1 mm)
The quality of equipment made of a pollution control material having an aluminum layer coated on its surface will be described.

FIG. 1 shows the relationship between the melting temperature of aluminum with which the surface of the titanium member is coated, the thickness of the aluminum coating, and the thickness of the aluminum compound layer (the compound layers of both compounds formed at the interface between titanium and aluminum). The titanium member was immersed in the molten aluminum for 1 minute.

When it is desired to increase the thickness of the aluminum layer coating the surface of the titanium member as shown in FIG. 1, the melting temperature of aluminum is set to 700 to 750 ° C., and the titanium member is immersed in the molten aluminum. The pulling may be repeated several times, and the immersion time per one time at that time may be set to about 5 seconds so that the aluminum member is well covered with the aluminum layer. Further, when the melting temperature of aluminum is high, the thickness of the aluminum layer coated on the surface of the titanium member becomes thin, but the thickness of the compound layer of titanium and aluminum near the interface becomes thick. Therefore, by adjusting the dipping time and the number of dipping of the titanium member in molten aluminum and the melting temperature of aluminum according to the structure of the equipment installed in the thin film forming apparatus and the type of thin film material for forming the thin film, The thickness of the aluminum layer formed and coated on the surface of the member can be set arbitrarily.

In FIG. 2, the titanium member was immersed in molten aluminum at a temperature of 800 ° C. for 10 minutes and then pulled up.
Stored in the same vacuum furnace, the temperature of molten aluminum is 70
The relationship between hardness (titanium (base material) and aluminum (coating material)) and hardness when immersion is further performed for 2 minutes at 0 ° C. is shown. The pressure during immersion of titanium in the molten aluminum was 5 × 10 ⁻⁵ Torr, and the atmosphere was argon gas with a purity of 99.999%. Moreover, the load in hardness measurement was 50 g. Further, the hardness measurement positions of titanium (base material) and aluminum (coating material) (measurement points are indicated by white circles in spots) are shown on the right side of FIG. The aluminum compound layer at the measurement point was a compound of titanium and aluminum formed at the interface between titanium (base material) and aluminum (coating material), and the thickness of the layer was about 50 μm.

As shown in FIG. 2, it can be seen that titanium and aluminum are strongly bonded at the interface. Further, this sample was subjected to a 90 ° deformation bending test at 2R, but no peeling occurred near the interface. Therefore, it can be sufficiently seen that no peeling occurs at the interface between the titanium and the aluminum coating during use.

FIG. 3 is a sectional view of a sample in which the surface of the titanium member is coated with an aluminum layer by immersion treatment at a temperature of 750 ° C. for 10 minutes by a scanning electron microscope (SEM), and FIG. Distribution state of aluminum by analyzer (EPMA), FIG. 5 shows distribution state of titanium by electron beam microanalyzer (EPMA) in aluminum portion, FIG. 6 shows oxygen (O ₂ ) by electron beam microanalyzer (EPMA) in titanium and aluminum portion. Shows the distribution state of. As shown in FIG. 3 (magnification × 250), FIG. 4 (magnification × 250), FIG. 5 (magnification × 250), and FIG. 6 (magnification × 250), titanium is molten in the aluminum layer at the interface between titanium and aluminum. In addition, it was found that the titanium layer and the aluminum layer had no pinholes or slag, and that the titanium material was surely covered with the aluminum layer. It can be seen that no occluded gas is generated.

FIG. 7, FIG. 8, FIG. 9, and FIG. 10 show the surface condition (scanning electron microscope photograph) of the aluminum layer coated on the surface of the titanium material. FIG. 7 (magnification x50), FIG. 8 (magnification x2)
50), FIG. 9 (magnification × 1000), FIG. 10 (magnification × 30)
(00), grains are generated on the surface of the aluminum layer, there are no foreign matters, etc., and the surface of the aluminum layer is in a very healthy state like the cross sections shown in FIGS. 3, 4, 5 and 6. It turns out that As a result, minute foreign matter that occurs in the apparatus during film formation and causes deterioration of the quality of the thin film formed on the substrate is reliably adhered to the aluminum layer, and the adhesion of the adhered deposit becomes extremely good, It can be seen that the internal stress due to the increase of the deposited deposit is absorbed by the "Yawasawa" of the aluminum layer, and it is difficult to generate particles due to the deformation of the device and the peeling and scattering of the deposit.

FIG. 11 shows an embodiment (thin film forming apparatus by sputtering method) of the thin film forming apparatus of the present invention. In the figure, reference numeral 1 denotes a sputtering chamber, and a sputtering gas inlet 2 for introducing the sputtering gas into the sputtering chamber 1 is provided in the sputtering chamber 1.
Then, an exhaust port 3 for providing a predetermined degree of vacuum in the sputtering chamber 1 was provided.

The substrate 4 for forming a thin film in the upper portion of the sputtering chamber 1 is held downward by the substrate holder 5. Further, a cathode 7 on which a target 6 made of a thin film material is placed is arranged at a position facing the substrate 4 below in the sputtering chamber 1. Further, a wall-shaped shield plate 8 was surrounded around the target 6 and the cathode 7, and a shutter plate 9 was arranged between the substrate 4 and the target 6. In the embodiment of FIG. 11, the substrate holder 5, the shield plate 8 of the target, and the shutter plate 9 are made of a pollution preventing material in which the surface of titanium is covered with an aluminum layer. 1 in the figure
0 is a power source for applying a predetermined voltage to the cathode 7, 1
Reference numeral 1 indicates an insulating plate.

Next, specific examples of the present invention will be described together with comparative examples.

Example 1 A square sample plate having a total thickness of 1 mm and a size of 50 mm was prepared by coating the inner wall of the ion plating apparatus with an aluminum layer having a purity of 99.999% of 120 μm at right angles to the evaporation direction of the thin film forming material. It was placed and the distance between the sample plate and the evaporation source was maintained at 400 mm. In addition, titanium was prepared as a thin film material to be formed on the sample plate. Subsequently, after the pressure inside the ion plating apparatus was set to 5 × 10 ⁻⁵ Torr, argon / nitrogen gas (mixing ratio 1: 4) was introduced as a film forming atmosphere gas, and the inside of the apparatus was adjusted to 5 × 10 ⁻² Torr. After maintaining, while heating the sample plate to a temperature of 150 ° C., a vapor deposition rate of 0.2 μm / on the sample plate by the ion plating method.
In a minute, a titanium nitride thin film having a thickness of 180 μm was formed.

Then, the peelability (according to JIS-H-8504) of the deposited deposit on the sample plate by the Scotch tape was examined, and the degree of deformation of the sample plate (the maximum deformation height in a plane) was measured. Table 1 shows the peelability of the deposited deposits examined and the results of the measured degree of deformation.

Comparative Example 1 As a sample plate, a SU having a thickness of 1 mm and a size of 50 mm was rectangular.
A thin film of titanium nitride having a film thickness of 180 μm was formed on the sample plate in the same manner as in Example 1 except that the S 304 (stainless steel) plate was used. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits by the Scotch tape on the sample plate was examined, and the degree of deformation of the sample plate was measured. Table 1 shows the peelability of the deposited deposits examined and the results of the measured degree of deformation.

Comparative Example 2 A thin film of titanium nitride having a film thickness of 180 μm was formed on a sample plate in the same manner as in Example 1 except that a rectangular titanium plate having a thickness of 1 mm and a size of 50 mm was used as the sample plate. Was formed. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits by the Scotch tape on the sample plate was examined, and the degree of deformation of the sample plate was measured. Table 1 shows the peelability of the deposited deposits examined and the results of the measured degree of deformation.

Comparative Example 3 A titanium nitride film having a thickness of 180 μm was formed on a sample plate in the same manner as in Example 1 except that a rectangular oxygen-free copper plate having a thickness of 1 mm and a size of 50 mm was used as the sample plate. A thin film was formed. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits on the sample plate with the Scotch tape was examined, and
The degree of deformation of the sample plate was measured. Table 1 shows the peelability of the deposited deposits examined and the results of the measured degree of deformation.

Comparative Example 4 A titanium nitride film having a thickness of 180 μm was formed on a sample plate in the same manner as in Example 1 except that a rectangular plate made of high-purity aluminum having a thickness of 1 mm and a size of 50 mm was used as the sample plate. Thin film was formed. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits by the Scotch tape on the sample plate was examined, and the degree of deformation of the sample plate was measured. Table 1 shows the peelability of the deposited deposits examined and the results of the measured degree of deformation.

[0038]

[Table 1] The partial peeling in Table 1 means that an adhered deposit is observed on the adhesive surface of the peeled tape.

As is clear from Table 1, in Example 1, the adhered deposits were not peeled and the degree of deformation was extremely small, whereas in Comparative Examples 1 and 2, the degree of deformation was extremely small, but the adhered deposits were very small. Peeling was observed in a part of. In addition, Comparative Example 3,
In No. 4, the deposited deposit was not peeled off, but the degree of deformation was large. Therefore, it was confirmed that the pollution control material of the present invention does not generate particles that cause deterioration of the quality of the thin film during use, and there is no risk of deformation of the equipment members during use.

Example 2 Each of the substrate holder 5, the shield plate 8 and the shutter plate 9 in the sputtering chamber 1 shown in FIG. 11 was formed on a surface of a titanium base material having a thickness of 0.8 mm and a purity of 99. 99
It was composed of a pollution control material coated with a 9% aluminum layer.

Then, a rectangular plate having a total thickness of 1 mm and a size of 50 mm made of titanium having a surface coated with an aluminum layer having a purity of 99.999% of 100 μm is attached to the substrate holder 5 and formed on the substrate 4. Aluminum having a purity of 99.999% was prepared as the target 6 of the thin film material, and the distance between the substrate holder 5 and the target 6 was maintained at 50 mm. Then, sputter chamber 1
After setting the pressure to 5 × 10 ⁻⁷ Torr, argon gas is introduced as a sputtering gas to maintain the pressure in the sputtering chamber 1 at 5 × 10 ⁻³ Torr, and the substrate 4 is heated to 150 ° C.
While maintaining the above, an output of 6 KW was applied to the target 6 to form an aluminum thin film having a film thickness of 500 μm on the substrate 4 by the sputtering method at a film forming rate of 60 μm / hour.

Then, according to the above-mentioned Example 1, the peelability of the deposited deposit on the substrate by the Scotch tape was examined, and the degree of deformation of the substrate was measured. The peelability of the deposited deposits examined,
The results of the measured deformation degree are shown in Table 2.

Comparative Example 5 As a substrate, a square SUS having a thickness of 1 mm and a size of 50 mm
An aluminum thin film having a thickness of 500 μm was formed on the substrate by the same method as in Example 2 except that the 304 plate was used. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits on the substrate by the Scotch tape was examined, and the degree of deformation of the substrate was measured. Table 2 shows the results of the peelability of the deposited deposits examined and the measured deformation degree.

Comparative Example 6 An aluminum thin film having a film thickness of 500 μm was formed on a substrate by the same method as in Example 2 except that a rectangular titanium plate having a thickness of 1 mm and a size of 50 mm was used as the substrate.
Then, according to the above-mentioned Example 1, the peelability of the adhered deposits on the substrate by the Scotch tape was examined, and the degree of deformation of the substrate was measured. Table 2 shows the results of the peelability of the deposited deposits examined and the measured deformation degree.

Comparative Example 7 An aluminum thin film having a thickness of 500 μm was formed on a substrate in the same manner as in Example 2 except that a rectangular oxygen-free copper plate having a thickness of 1 mm and a size of 50 mm was used as the substrate. . Then, according to the above-mentioned Example 1, the peelability of the adhered deposits on the substrate by the Scotch tape was examined, and the degree of deformation of the substrate was measured. Table 2 shows the results of the peelability of the deposited deposits examined and the measured deformation degree.

[0046]

[Table 2] As is clear from Table 2, in Example 2, the adhered deposits did not peel, and the degree of deformation was extremely small, whereas in Comparative Examples 5, 6 and 7, the adhered deposits did not peel, but the degree of deformation did not occur. Was great. Therefore, the pollution control material of the present invention does not generate particles that cause deterioration of the quality of the thin film during use,
It was also confirmed that there is no risk of deformation of the equipment members during use.

Example 3 Each of the substrate holder 5, the shield plate 8 and the shutter plate 9 in the sputtering chamber 1 shown in FIG. 11 was formed on a surface of a titanium base material having a thickness of 0.6 mm and a purity of 99. 99
It was composed of a pollution control material coated with a 9% aluminum layer.

Then, a rectangular plate having a total thickness of 1 mm and a size of 50 mm made of titanium having a surface coated with an aluminum layer of 220 μm and a purity of 99.999% is attached to the substrate holder 5 and is formed on the substrate 4. Prepare Mo-37wt% Si as the target 6 of the thin film material,
In addition, the distance between the substrate holder 5 and the target 6 is set to 5
It was maintained at 0 mm. Then, the pressure in the sputtering chamber 1 is set to 5 ×.
After the pressure is set to 10 ⁻⁷ Torr, argon is introduced as a sputtering gas to adjust the pressure in the sputtering chamber 1 to 5 × 10 ⁻³ To.
While maintaining the temperature at rr and the substrate 4 at a temperature of 150 ° C.,
An output of 2 kW is applied to the target 6 to form an M film having a film thickness of 500 μm on the substrate 4 by a sputtering method at a film forming rate of 13 μm / hour.
A thin film of o-Si alloy was formed on the substrate 4.

Then, according to the first embodiment, the peelability of the adhered deposit on the substrate by the Scotch tape was examined, and the degree of deformation of the substrate 4 was measured. Table 3 shows the results of the peelability of the deposited deposits examined and the measured degree of deformation.

Comparative Example 8 A SUS substrate having a thickness of 1 mm and a size of 50 mm
A Mo—Si alloy thin film having a film thickness of 500 μm was formed on the substrate in the same manner as in Example 3 except that the 304 plate was used. Then, according to the above-mentioned Example 1, the peelability of the deposited deposit on the substrate with the Scott tape was examined, and the degree of deformation of the substrate was measured. Table 3 shows the results of the peelability of the deposited deposits examined and the measured degree of deformation.

Comparative Example 9 A Mo-Si alloy thin film having a thickness of 500 μm was formed on a substrate in the same manner as in Example 3 except that a rectangular titanium plate having a thickness of 1 mm and a size of 50 mm was used as the substrate. Formed. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits on the substrate by the Scotch tape was examined, and the degree of deformation of the substrate was measured. Table 3 shows the results of the peelability of the deposited deposits examined and the measured degree of deformation.

Comparative Example 10 An Mo-Si alloy thin film having a thickness of 500 μm was formed on a substrate in the same manner as in Example 3 except that a rectangular oxygen-free copper plate having a thickness of 1 mm and a size of 50 mm was used as the substrate. Was formed. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits on the substrate by the Scotch tape was examined, and the degree of deformation of the substrate was measured. Table 3 shows the results of the peelability of the deposited deposits examined and the measured degree of deformation.

Comparative Example 11 A Mo—Si alloy having a film thickness of 500 μm was formed on a substrate in the same manner as in Example 3 except that a square high-purity aluminum plate having a thickness of 1 mm and a size of 50 mm was used as the substrate. A thin film was formed. Then, according to the above-mentioned Example 1, the peelability of the adhered deposits of the substrate by the Scotch tape was examined, and
The degree of deformation of the substrate was measured. Table 3 shows the results of the peelability of the deposited deposits examined and the measured degree of deformation.

[0054]

[Table 3] Partial peeling in Table 3 means that adhered deposits are found on the adhesive surface of the peeled tape, and partial peeling at the deformed part means cracking and peeling of adhered deposits at the deformed head. It is indicated that.

As is clear from Table 3, in Example 3, there was no peeling of the deposited deposit, and the degree of deformation was extremely small, whereas in Comparative Example 8, peeling was observed in a part of the deposited deposit and deformation occurred. The degree of deformation was large, and in Comparative Example 9, the degree of deformation was large, although the adhered deposits did not peel off. Further, in Comparative Examples 10 and 11, there was a large deformation in which deformation was observed with the naked eye, cracking of the adhered deposit was observed in the deformed portion, and peeling was observed in part of the deformed portion. Therefore, it was confirmed that the pollution control material of the present invention does not generate particles that cause deterioration of the quality of the thin film during use, and there is no risk of deformation of the equipment members during use.

Example 4 Ti-5 wt% Al-2.5w having a surface coated with an aluminum layer having a purity of 99.999% of 200 μm as a substrate
Made of t% Sn (titanium alloy), total thickness 1 mm, size 50 m
A Mo—Si alloy thin film having a film thickness of 500 μm was formed on the substrate in the same manner as in Example 3 except that the m-square plate was used. Then, according to the above-described Example 1, the peelability of the adhered deposit on the substrate by the Scotch tape was not examined. When the deformation degree of the substrate was measured, the maximum value was 0.
It was 1 mm.

Example 5 Example 3 was repeated except that a rectangular plate made of titanium with a total thickness of 1 mm and a size of 50 mm, the surface of which was coated with an aluminum alloy layer of Al-1 wt% Si of 200 μm, was used as the substrate.
A thin film of a Mo—Si alloy having a film thickness of 500 μm was formed on the substrate by the same method as described above. Then, according to the above-described Example 1, the peelability of the adhered deposit on the substrate by the Scotch tape was not examined. Further, when the degree of deformation of the substrate was measured, the maximum value was 0.1 mm.

Therefore, the fourth and fifth embodiments are the same as the first and second embodiments.
As in Nos. 2 and 3, it was confirmed that there was no generation of per-particles that would cause deterioration of the quality of the thin film during use, and there was no fear of deformation of the device during use.

Although Ti-Al-Sn was used as the titanium alloy as the base material for coating the aluminum layer or aluminum alloy layer on the surface in the above-mentioned embodiment, the present invention is not limited to this, and the Ti- In addition to Al-Sn,
An example is a titanium alloy containing V, Mo, and Mn in Ti in an amount of 1 to 8 wt%.

Although Al-Si is used as the aluminum alloy layer for coating the surface of the titanium or titanium alloy of the base material in the above-mentioned embodiment, the present invention is not limited to this and the above-mentioned Al-Si is used. In addition to Cu, T in Al
An aluminum alloy containing 0.5 to 10 wt% of i and Sn can be used.

[0061]

As described above, according to the thin film forming apparatus of the present invention, the equipment or the constituent parts in the apparatus are constituted by the pollution preventing material in which the surface of titanium or titanium alloy is coated with the aluminum layer or the aluminum alloy layer. Therefore, if the fine particles of the thin film forming material that are generated during the thin film formation on the substrate in a vacuum by the sputtering method, etc., adhere to these devices or components, they will surely adhere and accumulate. Since it does not peel off or scatter on the surface, it is possible to remarkably control the particles that cause the deterioration of quality, and since there is no release of stored gas, it is possible to easily form a high quality thin film on the substrate. There is an effect that a forming apparatus can be provided. Further, since the contamination preventing material after being installed in the thin film forming apparatus of the present invention and having formed the thin film on the substrate can be reprocessed and reused after use,
Extremely economical.

[Brief description of drawings]

FIG. 1 is a characteristic diagram showing a relationship between an aluminum melting temperature and an aluminum coating thickness and an aluminum compound layer thickness.

FIG. 2 is a characteristic diagram showing hardness measurement points of titanium and aluminum and a relationship between titanium and aluminum and hardness.

FIG. 3 is a drawing-substituting photograph showing a metallographic structure of a pollution control material in which an aluminum layer is coated on a surface of a titanium material.

FIG. 4 is a drawing-substituting photograph showing a metal structure of an aluminum state of a titanium portion of a pollution control material.

FIG. 5 is a drawing-substituting photograph showing the metal structure of titanium state of the aluminum portion of the pollution control material.

FIG. 6 is a drawing-substituting photograph showing a metallographic structure in a state where oxygen is contained in titanium and aluminum portions of a pollution control material.

FIG. 7 is a drawing-substituting photograph showing a grain structure of an aluminum surface of a pollution control material.

FIG. 8 is a drawing-substituting photograph showing a grain structure of an aluminum surface of a pollution control material.

FIG. 9 is a drawing-substituting photograph showing a grain structure of an aluminum surface of a pollution control material.

FIG. 10 is a photograph as a substitute for a drawing showing a grain structure of an aluminum surface of a pollution control material.

FIG. 11 is an explanatory diagram of one embodiment of the thin film forming apparatus of the invention.

[Explanation of symbols]

 4 substrate 5 substrate holder 8 shield plate 9 shutter plate

Claims (2)

[Claims] 1. A thin film forming apparatus for forming a thin film on a substrate in a vacuum, wherein equipment or components in the thin film forming apparatus are coated with an aluminum layer or an aluminum alloy layer on the surface of titanium or a titanium alloy to prevent contamination. A thin film forming apparatus characterized by being made of a material. 2. The thin film forming apparatus according to claim 1, wherein the device or component in the thin film forming apparatus is any one of a target shield plate, a shutter plate, and a substrate holder.