JP2007046091A - Temperature control device in vacuum vessel, and thin film deposition method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a temperature control device in a vacuum vessel where a member can be controlled to the vicinity of a set temperature or below the set temperature in a vacuum vessel, and to provide a thin film deposition method. <P>SOLUTION: The temperature control device in a vacuum vessel performing prescribed treatment in a vacuum atmosphere has a structure where the inside of a member 8 composing the vacuum vessel involves a phase change material 11 having a melting point in the vicinity of the treatment temperature. At this time, the phase change material is composed of a low melting point alloy essentially consisting of any element selected from In, Sb, Bi and Pb, and having a melting point of about 10 to 327°C. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a temperature control device in a vacuum vessel and a thin film forming method. In particular, the present invention relates to a temperature control device in a vacuum vessel used when a target is sputtered to form a film on a substrate.

  In recent years, various high-functional devices such as electronic devices and optical devices have been developed, and thin film formation technology is indispensable for these high-functional devices. Such thin film formation techniques can be generally classified into dry thin film formation techniques and wet thin film formation techniques. Among them, the dry thin film formation technology is a technology for forming a thin film on a substrate mainly in a vacuum vessel. By a method of forming a thin film material on the substrate, (physical) vapor deposition technology, sputtering technology, CVD technology, etc. are categorized.

When a highly functional device is formed by the dry thin film formation technique, a common factor that greatly affects the quality of the thin film is the substrate temperature during the formation of the thin film. For example, when an antireflection film or a high reflection film is formed on an optical component such as a lens by using a vapor deposition technique, if the substrate temperature is too low, the film density is lowered and the refractive index of the film is lowered. As a result, desired optical characteristics cannot be obtained, and environmental resistance is also deteriorated.
Conversely, if the substrate temperature is too high, it will not function as an optical component due to film cracking due to stress strain, cloudiness, deformation of the substrate, and the like. In addition, in the reactive sputtering technique and the CVD technique in which a thin film is formed using a chemical reaction, the reaction rate greatly varies depending on the temperature. As a result, the characteristics of the film are greatly changed, or the formation speed of the thin film is greatly changed. From the above, it is indispensable to stably maintain a desired substrate temperature during the thin film formation process in order to form a thin film having desired characteristics on the substrate.

On the other hand, in the case of forming a high-functional device by the dry thin film forming technique, a substrate rotation mechanism is generally employed in order to ensure uniformity of film characteristics on the substrate. As such a substrate rotating mechanism, there is known a mechanism that uses two rotating mechanisms, ie, rotation and revolution of a substrate, when a thin film is simultaneously formed on a plurality of substrates.
In addition to the above rotating mechanism, there is also known one having a driving mechanism that forms a thin film while the substrate itself moves. For such a drive mechanism, a bearing or a gear is used. However, these members deteriorate at a high temperature due to oxidation or the like. In addition, the grease for vacuum may be deteriorated, the slidability may be deteriorated due to evaporation, or galling or seizing may occur, resulting in failure to drive. In such a case, in order to perform the thin film formation process stably, it is necessary to control the temperature so that the drive mechanism does not become high temperature.

  In order to control the temperature of such a thin film formation process, for example, Patent Document 1 proposes a sputtering apparatus that controls a substrate heating apparatus using a dummy substrate. The sputtering apparatus here is a sputtering apparatus that deposits a film on a substrate by sputtering a plurality of targets while moving the substrate. In such a sputtering apparatus substrate, a substrate heating / moving mechanism capable of moving the substrate relative to the target while heating is provided. In addition, a dummy substrate is attached to the substrate heating and moving mechanism separately from the substrate, and the dummy substrate is arranged so that the positional relationship between the substrate and the target and the positional relationship between the dummy substrate and the target are geometrically equivalent. Is done. Based on the temperature of the dummy substrate, the substrate heating device of the substrate heating and moving mechanism is controlled. Further, the substrate heating / moving mechanism is composed of a substrate holder portion, a substrate heating portion, and a substrate holder rotating portion, and a plurality of sealing devices separated in the axial direction are provided on the rotation introduction shaft of the substrate holder rotating portion. Yes. The space between the plurality of sealing devices is evacuated or non-oxidizing gas atmosphere. Further, a connection member is interposed in the connection portion between the substrate holder part and the substrate holder rotating part, and the connection member is formed of a material having high melting point and low thermal conductivity or ceramics.

In such a sputtering apparatus, it is important to stabilize the temperature of the sputtering target in order to perform sputtering stably. Therefore, for example, as in Patent Document 2, a backing plate for a sputtering apparatus having a cooling performance that can stably perform sputtering for a long time has been proposed. This has a substantially constant cross-sectional area along the entire length, and the cooling medium passage is provided in the backing plate body so that the cooling medium first goes around the outer periphery of the backing plate and gradually moves to the center. Have.
Patent Document 3 proposes a sputtering apparatus that stabilizes the substrate temperature during sputtering. The sputtering apparatus here has a vacuum processing chamber, a stage electrode for placing a substrate disposed in the chamber, and a target electrode disposed to form a plasma discharge with respect to the stage electrode. ing. Also provided is a substrate temperature measuring block disposed on the stage electrode and causing a temperature change substantially the same as the substrate, and a temperature control unit. The temperature control unit has temperature control means for controlling the temperature of the chamber and the stage electrode independently of each other. When controlling the temperature, the temperature control means is configured to instruct the temperature of the chamber and the stage electrode to be complementarily controlled based on the temperature of the block, and to keep the temperature of the substrate constant. ing.
Japanese Patent No. 344002 JP 2000-219963 A JP 2003-7644 A

However, since the conventional example of Patent Document 1 uses a dummy substrate and measures its temperature to control the temperature, it has the following problems.
In other words, since the thermocouple is bonded on the dummy substrate, the replacement frequency must be extremely low. For this reason, a film several times thicker is formed on the dummy substrate while the substrate is replaced with a load lock and sputtering is performed a plurality of times. Since heat transfer in vacuum has a large ratio of radiant heat transfer, heat transfer by radiant heat transfer greatly depends on the film thickness when the substrate and the film have different emissivities. For example, when the emissivity of the film is larger than that of the substrate, the radiant heat transfer increases as the film thickness increases until the film thickness reaches several μm to several tens of μm, which is about the wavelength of infrared rays that contributes to radiant heat transfer. . For this reason, the heat escape due to radiant heat transfer from the dummy substrate is greater than the heat escape from the substrate having a smaller film thickness than the dummy substrate. On the contrary, when the emissivity of the film is smaller than that of the substrate, the heat escape due to the radiant heat transfer from the dummy substrate is smaller than the heat escape from the substrate. For this reason, as the number of times the same dummy substrate is used increases, the difference between the actual substrate temperature and the dummy substrate temperature increases, thereby causing a problem that the substrate temperature cannot be controlled correctly.
In the conventional example of Patent Document 1, a plurality of sealing devices separated in the axial direction are provided on the rotation introduction shaft of the substrate holder rotating portion, and the space between the plurality of sealing devices is evacuated. Or the structure made into non-oxidizing gas atmosphere is taken. Further, a connection member is interposed in a connection portion between the substrate holder part and the substrate holder rotating part, and the connection member is formed of a material having a high melting point and low thermal conductivity. With these, it is possible to protect the rotation introduction shaft from high temperature and oxidation, but when rotating the substrate to make the in-plane characteristics of the film on the substrate uniform, the rotation driving mechanism is closer to the substrate. It is configured. For this reason, it is difficult to protect the rotation driving mechanism from high temperatures with the above configuration.
Furthermore, when plasma is used for forming a thin film such as a sputtering apparatus or a plasma CVD apparatus, the temperature may increase. That is, even when the substrate does not have a heating mechanism, the temperature may increase while the thin film is being formed by heating with charged particles flowing from the plasma or by radiation from the plasma. In these cases, it is difficult to keep the temperature of the substrate driving mechanism below the operating limit temperature in the configuration of the conventional example.
Further, in the conventional example of Patent Document 2 described above, the inlet temperature of the cooling medium flowing through the cooling medium passage inside the backing plate can be controlled from the outside, but there are cases where the actual target temperature cannot be controlled. For example, when excessive power is supplied to the target in a short time, a sufficient cooling capacity may not be obtained.
Further, in the conventional example of Patent Document 3, a dummy substrate is used, and its temperature is measured and temperature control is performed, so the same problem as in Patent Document 1 occurs. In addition, since it is necessary to control the chamber temperature and the substrate temperature independently of each other, there is a problem that the apparatus configuration and the control system become complicated. In addition, when using a deposition plate to prevent the film from adhering to the chamber, it is necessary to control the temperature of the deposition plate as employed in Patent Document 3 above. A similar problem arises in that the configuration and control system are complicated.

In view of the above-described problems, an object of the present invention is to provide a temperature control device in a vacuum vessel that can control a member in the vacuum vessel to be close to or below a set temperature.
Another object of the present invention is to provide a thin film forming method capable of forming a thin film while maintaining the substrate temperature at a predetermined temperature stably.

In order to solve the above problems, the present invention provides a temperature control device and a thin film forming method in a vacuum vessel configured as follows.
That is, the temperature control device of the present invention is a temperature control device in a vacuum vessel that performs a predetermined treatment in a vacuum atmosphere, and a phase having a melting point in the vicinity of the treatment temperature is formed inside a member constituting the vacuum vessel. It is characterized by the inclusion of change material.
In the present invention, the phase change material may be composed of a low melting point alloy having a melting point of about 10 ° C. or more and 327 ° C. or less, with any of In, Sb, Bi, and Pb as a main component.
The thin film forming method of the present invention is the thin film forming method in which the temperature in the vacuum vessel is controlled by the temperature control means, and the thin film is formed on the substrate using a sputtering method, a CVD method, a vacuum deposition method or the like. A phase change material having a melting point in the vicinity of the processing temperature is included in a member constituting the container, and the temperature of the member in which the phase change material is included is maintained in the vicinity of the melting point of the phase change material. Thereafter, a thin film is formed on the substrate.

  ADVANTAGE OF THE INVENTION According to this invention, the temperature control apparatus in a vacuum vessel which becomes possible to control a member to set temperature vicinity or below setting temperature in a vacuum vessel is realizable. Further, it is possible to realize a thin film forming method capable of forming a thin film while keeping the temperature of the substrate stably at a predetermined temperature.

Next, an embodiment of the present invention will be described. In the present invention, in order to control the member in the vacuum vessel near the set temperature or below the set temperature, the member in which the phase change material is included can be configured as follows.
That is, a substrate holder that holds a substrate used for film formation can be configured with a member in which the phase change material is included. Further, the member in the vicinity of the drive mechanism that rotates and / or advances the substrate holder can be constituted by a member in which the phase change material is included. Further, the wall surface constituting member of the vacuum vessel can be constituted by a member in which the phase change material is included. In addition, the adhering matter preventing member adhering to the wall surface of the vacuum vessel can be configured by a member in which the phase change material is included. Moreover, the backing plate holding the sputtering target by bonding can be configured by a member in which the phase change material is included.

With the above configuration, the amount of heat flowing into or out of the member can be absorbed or released by the latent heat of fusion of the phase change material contained in the member. This makes it possible to keep these members at a substantially constant temperature or below a certain temperature. Especially in a vacuum vessel, as described in the above problem, the technical difficulty of accurate temperature measurement of members is high, and even if the temperature can be measured relatively accurately, the state of heat transfer is in the atmosphere. Difficulty arises in control responsiveness.
On the other hand, according to the above configuration of the present invention, it is possible to easily keep the temperature of the member stably in the vicinity of the predetermined temperature or below the predetermined temperature without requiring special temperature measurement and temperature control. .
Further, in the above configuration, the substrate holder has a driving mechanism that rotates and / or goes straight, so that it can greatly contribute to the uniformity of the film thickness distribution and characteristic distribution of the thin film to be formed in the substrate. . In this case, temperature measurement and temperature control become more difficult compared with the case where the substrate holder is fixed. However, in the temperature control based on the latent heat of fusion of the phase change material contained in the substrate holder, temperature measurement and temperature Wiring for control becomes unnecessary. Therefore, the apparatus configuration is simplified, and there is no error due to fluctuation of the measurement control system due to driving of the substrate holder, and the thin film can be formed stably and accurately at a predetermined temperature.
In the above configuration, the temperature of the sputtering target can be stably kept below the melting point temperature of the bonding material by incorporating the phase change material having the melting point below the set temperature in the backing plate. Become. Thereby, a thin film can be stably formed by sputtering.
In addition, as in the present invention, the phase change material is made of an alloy having any of In, Sb, Bi, and Pb as a main component and a melting point of 30 ° C. or higher and 327 ° C. or lower, so that the melting point temperature can be set by the component ratio. It can be changed freely. Thereby, it becomes possible to cope with various processes and film materials.

Further, when configuring the film forming apparatus, it is possible to adopt a configuration having a transfer means for transferring the substrate holder together with the substrate to the vacuum vessel. In that case, the said conveyance means can be comprised by the conveyance chamber connected to the said vacuum vessel, and can be set as the structure which has a heating mechanism which heats a substrate holder and a board | substrate in this conveyance chamber.
Further, a member in the vicinity of the drive mechanism in which the phase change material is included may be configured to include a phase change material having a melting point equal to or lower than an upper limit temperature at which the drive mechanism can operate. At that time, the drive mechanism may include at least a bearing or a gear, and the operable upper limit temperature may be 150 ° C. or less.
Further, it is possible to adopt a configuration in which the substrate is a substrate used for forming an optical thin film, and the optical thin film is formed on the substrate.
With the above configuration, it is possible to easily form a thin film while stably maintaining the temperature of the member near or below a predetermined temperature without requiring special temperature measurement and temperature control.
Further, in the above configuration, by adopting a configuration in which a thin film is formed after the substrate holder and the substrate are transported together, the substrate can be attached to the substrate holder outside the vacuum container, so that the degree of freedom of the shape of the substrate is increased. can do.
Further, in the above configuration, by adopting a configuration in which a phase change material having a melting point equal to or lower than the upper limit temperature at which the drive mechanism can operate is included in the substrate holder in the vicinity of the drive mechanism, the drive mechanism is made stable and has a long life. Is possible. At that time, the maximum temperature at which a standard bearing or gear can operate in a vacuum is often 150 ° C. or lower. However, according to the above configuration, a thin film can be stably formed by controlling the temperature below this temperature. be able to.

Further, the step of forming the thin film includes a process of forming a thin film on the substrate after maintaining the temperature of the substrate holder in which the phase change material is contained in the vicinity of the melting point of the phase change material. Can be taken.
Moreover, the structure including the process of forming a thin film on a board | substrate, rotating the said substrate holder and / or moving straight can be taken.
Further, it is possible to adopt a configuration including a process in which the substrate is attached to the substrate holder outside the vacuum vessel, put into a transfer chamber connected to the vacuum vessel and heated, and then transferred to the vacuum vessel to form a thin film.
Further, a member in the vicinity of the drive mechanism includes a phase change material having a melting point not higher than the upper limit temperature at which the drive mechanism can operate, and after maintaining the phase change material at a temperature not higher than the melting point, the substrate holder is rotated. A configuration including a process of forming a thin film by going straight and / or straight can be adopted.
Moreover, the process of forming the said thin film can be made into the process of forming an optical thin film.
With the above configuration, it is possible to easily keep the temperature of the member stable near the predetermined temperature or below the predetermined temperature and form a thin film without requiring special temperature measurement and temperature control. Further, in the above configuration, by adopting a configuration in which the substrate is attached to the substrate holder outside the vacuum vessel, charged into a transfer chamber connected to the vacuum vessel, heated, and then transferred to the vacuum vessel to form a thin film. It is possible to attach the substrate to the substrate holder externally. For this reason, it is possible to easily cope with various substrate shapes as well as plate shapes. When the substrate holder can be transported together with the substrate in this way, it is almost impossible to use a contact type such as a thermocouple for measuring the temperature of the substrate, and normal temperature control becomes impossible.
On the other hand, according to the above configuration, if temperature control based on the latent heat of fusion of the phase change material contained in the substrate holder is used, a thin film can be formed with high accuracy and stability and the substrate temperature at a predetermined temperature. .

Next, the specific configuration of the present invention will be described in more detail with reference to the drawings.
FIG. 1 shows a cross-sectional view of a DC magnetron sputtering apparatus in the present embodiment. In FIG. 1, 1 is a vacuum vessel, 2 is a cathode electrode, 3 is a backing plate, 4 is a target, and 5 is an anode electrode. 6 is an insulating material, 7 is a substrate, 8 is a substrate holder, 9 is a gate valve, and 10 is a load lock chamber. Further, 11 is a low melting point alloy, 12 is an exhaust system, and 13 is a sputtering gas introduction port. 14 is a DC power source, and 15 is a magnet.

  The sputtering apparatus of the present embodiment is provided with a vacuum vessel 1 that maintains the inside in a substantially vacuum state, and in the center of the bottom of the vacuum vessel 1 is provided a cathode 15 that houses a magnet 15 and can be cooled with water. It has been. A backing plate 3 is disposed on the upper surface of the cathode electrode 2, and a high-purity Al metal target 4 is fixed on the upper surface of the backing plate 3. Of course, the target material may be a target made of various metals, oxygen-added metal, fluorine-added metal or the like as long as it has a low electric resistance and allows direct current to pass. An anode electrode 5 disposed outside the target 4 with a predetermined gap is fixed to the vacuum vessel 1. An insulating material 6 is disposed between the anode electrode 5 and the backing plate 3.

Further, on the upper surface of the vacuum vessel 1, the substrate 7 is provided so as to be movable between the substrate holder 8 and the load lock chamber 10 via a gate valve 9 by a moving mechanism (not shown). Although not particularly illustrated, a seal member is provided at an appropriate location in order to prevent leakage in the vacuum vessel 1.
Further, Ar gas can be introduced from the gas introduction port 13 as a sputtering gas by a gas supply system including a mass flow controller. When the thin film formed on the substrate by reactive sputtering is an oxide or fluoride of Al, oxygen (O ₂ ) gas or fluorine (F ₂ ) gas can be introduced from the gas introduction port 13 together with Ar gas. good. Alternatively, another gas introduction port (not shown) may be provided for introduction. Here, the flow rate, purity, and pressure of the introduced gas are limited to high precision and can be held at a constant value.
A low melting point alloy 11 is sealed inside the substrate holder 8. The low melting point alloy can be adjusted to various melting points depending on the alloy composition. As a specific example, an alloy of In, Sn, Bi, Ga, Pb, and Cd can be used, and the melting point can be arbitrarily changed between about 10 ° C. and about 327 ° C. depending on the composition. In recent years, Pb-free solder has been actively developed due to environmental problems, and it is possible to use a low melting point alloy that does not contain harmful substances such as Pb and Cd, and it is desirable to use such a material.
What is sealed in the substrate holder 8 may be a substance other than a low melting point alloy, for example, a pure metal such as In or various organic substances, as long as it has a melting point at the temperature at which the substrate holder is desired to be held. The low melting point alloy 11 is preheated to a temperature near the melting point. Here, when the heat balance of the substrate holder 8 and the substrate 7 becomes negative during the formation of the thin film, that is, when the outflow is larger than the inflow of heat, more than half of the low melting point alloy is in a liquid state. Therefore, the substrate holder 8 and the low melting point alloy 11 are preheated to the melting point of the low melting point alloy 11 or a slightly higher temperature before forming a thin film, and more than half of the low melting point alloy is brought into a liquid state. As a result, heat flow proceeds during the thin film formation process, but the low melting point alloy 11 is changed from a liquid to a solid to release latent heat of fusion, and the substrate holder 8 and the substrate 7 can be kept at a constant temperature. It becomes.
Conversely, when the heating from the plasma is significant, the heat balance of the substrate holder 8 and the substrate 7 becomes positive during the formation of the thin film, that is, when the inflow is more than the outflow of heat, the low melting point alloy is more than half. Try to be in a solid state. Therefore, before the thin film formation of the substrate holder 8 and the low melting point alloy 11, the melting point of the low melting point alloy 11 or a slightly lower temperature is set in advance, and more than half of the low melting point alloy is in a solid state. Thereby, inflow of heat proceeds during the thin film forming process, but the low melting point alloy 11 is changed from solid to liquid to absorb the latent heat of fusion, and the substrate holder 8 and the substrate 7 can be kept at a constant temperature. It becomes.

  An exhaust system 12 including a valve and a vacuum pump is connected to the vacuum container 1 in order to exhaust the gas in the vacuum container. Further, in the thin film forming apparatus of the present embodiment, an adhesion preventing member 16 may be attached to the vacuum vessel 1 in order to prevent the film from adhering to the vacuum vessel as shown in FIG. It is also possible to control the temperature by sealing a low melting point alloy (not shown) inside the vacuum vessel 1 or the deposition preventing member 16. It is also possible to control the temperature by sealing a low melting point alloy (not shown) inside the backing plate 3.

  In the thin film forming apparatus of the present embodiment, a drive mechanism that can rotate a single substrate may be configured. FIG. 3 shows the configuration. In FIG. 3, 1 is a vacuum vessel, 7 is a substrate, 8 is a substrate holder, 11a and 11b are low melting point alloys, and 17 is a substrate driving mechanism. As shown in FIG. 3, the substrate 7 and the substrate holder 8 are configured to be rotated with respect to the vacuum vessel 1 by the substrate driving mechanism 17, and the low melting point alloy 11a is placed in the substrate holder 8 so that the temperature of the substrate is stabilized. Encapsulate. Further, the low melting point alloy 11b is also sealed in the vicinity of the substrate driving mechanism so that the temperature of the substrate driving mechanism does not rise above the melting point of the low melting point alloy 11b.

Further, the thin film forming apparatus of the present invention may constitute a drive mechanism that can revolve and revolve a plurality of substrates. FIG. 4 shows the configuration. In FIG. 4, 1 is a vacuum vessel, 7 is a substrate, 8a and 8b are substrate holders, 11c and 11d are low melting point alloys, and 17a and 17b are substrate drive mechanisms. As shown in FIG. 4, the substrates 7 are respectively installed on the substrate holder 8a, and the substrate holders 8a can be rotated on the substrate holder 8b by the substrate driving mechanism 17a so that the substrate can rotate. Further, a low melting point alloy 11c is sealed inside the substrate holder 8a so that the substrate temperature is stabilized at a predetermined temperature. The low melting point alloy 11d is also sealed inside the substrate holder 8b in the vicinity of the substrate driving mechanism 17a so that the substrate driving mechanism 17a does not rise above the operation upper limit temperature.
The substrate 7 may be configured so that it can be transported into the vacuum container 1 by being put together with the substrate holder 8 a into the transport chamber connected to the vacuum container 1. Further, a heating mechanism for heating the substrate holder and the substrate may be configured in the transfer chamber.

Next, a method for forming an alumina (Al ₂ O ₃ ) thin film on the quartz substrate 7 using the apparatus of FIG. 1 will be described.
First, the vacuum vessel 1 is evacuated to a vacuum by an exhaust system 12 including a valve and a vacuum pump. Next, the substrate holder 8 is heated in advance to the vicinity of the melting point of the low melting point metal 11 by an external heater (not shown). When the exhaust is completed to 1 × 10 ⁻⁴ Pa, 200 sccm of Ar gas is introduced from the sputtering gas introduction port 13.
Next, O ₂ gas is introduced into the vicinity of the 50 sccm substrate 7 from a reactive gas introduction port (not shown). When a DC voltage of 500 W is applied to the backing plate 3 from the DC power source 14, the discharge discharges and the Ar gas is ionized, and the magnetic field generated by the magnet 15 is formed above the target 4. Magnetron plasma is generated. A sheath is formed on the surface of the target by the discharge, positive ions in the plasma are accelerated by the sheath and collide with the target 4, and Al particles sputtered from the target 4 are released.

The gas pressure, flow rate, applied power, and the like are selected so that abnormal discharge does not occur, and a shutter (not shown) disposed between the substrate and the target is closed until the discharge is stabilized. When it is stable, the shutter is opened and a thin film is formed on the substrate 7.
When a film is formed under conditions that cause abnormal discharge, foreign matter is mixed into the film, resulting in a highly scattering film. The sputtered particles react with active oxygen atoms, oxygen molecules, and oxygen ions in the plasma and on the substrate surface, and an alumina thin film is deposited on the substrate 7. After the film formation is completed, the shutter is closed and the discharge is stopped. Here, the substrate is carried out to the atmosphere via the load lock chamber 10. The spectral characteristics of the alumina film on the substrate 7 are measured with a spectrophotometer, and the thickness, absorption, and the like are calculated by an optical interference method or the like.

Examples of the present invention will be described below.
[Example 1]
In Example 1, an alumina film was formed by the above-described method using the DC magnetron sputtering apparatus shown in FIG.
The substrate holder shown in FIG. 3 was used. In FIG. 3, an alloy of Sn / Bi = 65.5 / 31.5 (%) was used as the low melting point alloy 11a in order to keep the temperature in the vicinity of the substrate at 170.degree. Similarly, as the low melting point alloy 11b, one having Sn / Bi = 33.0 / 67.0 (%) was used so that the substrate driving mechanism 17 was at a temperature of 109 ° C. or lower. During film formation by sputtering, the substrate driving mechanism 17 stably operated at a temperature of 109 ° C. or lower and the substrate temperature was stable at around 170 ° C., so that an alumina film having desired optical characteristics was stabilized. I was able to get it.

[Example 2]
In Example 2, an alumina film was formed by the above-described method using the DC magnetron sputtering apparatus shown in FIG. The substrate holder shown in FIG. 4 was used. In FIG. 4, an alloy of Sn / Bi = 65.5 / 31.5 (%) was used as the low melting point alloy 11c in order to keep the temperature in the vicinity of the substrate at 170.degree.
Similarly, the low melting point alloy 11d is Sn / Bi = 33.0 / 67.0 (%) so that the substrate driving mechanism 17a has a temperature of 109 ° C. or lower.
During film formation by sputtering, the substrate driving mechanism 17a stably operated at a temperature of 109 ° C. or lower, and the substrate temperature was stable at around 170 ° C. Therefore, an alumina film having desired optical characteristics was stabilized. I was able to get it.

[Example 3]
In Example 3, an alumina film was formed by the above-described method using the DC magnetron sputtering apparatus shown in FIG. The substrate holder shown in FIG. 3 was used. In FIG. 1, a low melting point alloy (not shown) is sealed inside the backing plate 3.
The low melting point alloy is an alloy of In / Sn = 52/48 (%) having a melting point lower than the melting point 157 ° C. of indium (In) bonding the target 4 and the backing plate 3, and a temperature of 118 ° C. or less. I tried to become. During film formation by sputtering, the temperature of the target 4 was kept lower than the melting point of indium (In) 157 ° C., and an alumina film could be obtained stably.

[Example 4]
In Example 4, an alumina film was formed by the above-described method using the DC magnetron sputtering apparatus shown in FIG. The substrate holder shown in FIG. 3 was used. In FIG. 2, the adhesion preventing member 16 was removed using a vacuum vessel 1 in which a low melting point metal was sealed. Since the vacuum vessel 1 uses a rubber O-ring for vacuum-sealing, use a low melting point alloy of In / Bi = 66.3 / 33.7 (%) so as to keep the temperature at 72 ° C. or lower. I made it.
The substrate temperature is stabilized by stabilizing the heat transfer from the vacuum vessel 1 to the substrate 7, and the film is prevented from being peeled off due to thermal stress from the vacuum vessel 1. A small amount of alumina film could be obtained stably.

[Example 5]
In Example 5, an alumina film was formed by the above-described method using the DC magnetron sputtering apparatus shown in FIG. The substrate holder shown in FIG. 3 was used. In FIG. 2, the anti-adhesion member 16 in which a low melting point metal is sealed is used. Since the vacuum vessel 1 uses a rubber O-ring for vacuum-sealing, use a low melting point alloy of In / Bi = 66.3 / 33.7 (%) so as to keep the temperature at 72 ° C. or lower. I made it. The substrate temperature is stabilized by stabilizing the heat transfer by the heat radiation from the deposition preventing member 16 to the substrate 7, and the film has desired optical characteristics due to the effect of preventing film peeling due to thermal stress from the deposition preventing member 16. An alumina film with few defects could be stably obtained.

It is sectional drawing of the DC magnetron sputtering apparatus in embodiment of this invention. It is sectional drawing of the DC magnetron sputtering device which attached the adhesion prevention member in embodiment of this invention. It is sectional drawing of the board | substrate holder which has a board | substrate drive mechanism which can rotate the single board | substrate in the sputtering apparatus of embodiment of this invention. It is sectional drawing of the board | substrate holder which has a board | substrate drive mechanism in which the several board | substrate can revolve automatically in the sputtering apparatus of embodiment of this invention.

Explanation of symbols

1: Vacuum container 2: Cathode electrode 3: Backing plate 4: Target 5: Anode electrode 6: Insulating material 7: Substrate 8, 8a, 8b: Substrate holder 9: Gate valve 10: Load lock chamber 11, 11a, 11b, 11c 11d: Low melting point alloy 12: Exhaust system 13: Sputter gas introduction port 14: DC power supply 15: Magnet 16: Deposition member 17, 17a, 17b: Substrate drive mechanism

Claims (14)

  A temperature control device in a vacuum vessel for performing a predetermined treatment in a vacuum atmosphere, characterized in that a phase change material having a melting point in the vicinity of the treatment temperature is included in a member constituting the vacuum vessel. A temperature control device in a vacuum vessel.   2. The inside of the vacuum vessel according to claim 1, wherein the phase change material is a low melting point alloy having a melting point of 10 ° C. or higher and 327 ° C. or lower mainly containing any of In, Sb, Bi, and Pb. Temperature control device.   The said process is a vacuum film-forming which forms a thin film in a board | substrate, The member in which the said phase-change material is included is a board | substrate holder holding the said board | substrate, The Claim 1 or Claim 2 characterized by the above-mentioned. Temperature control device in the vacuum vessel.   The temperature control in the vacuum vessel according to claim 1 or 2, wherein the member in which the phase change material is included is a member in the vicinity of a driving mechanism that rotates and / or advances the substrate holder. apparatus.   The temperature control device in a vacuum vessel according to claim 1 or 2, wherein the member containing the phase change material is a wall surface constituting member of the vacuum vessel.   The temperature control device in a vacuum vessel according to claim 1 or 2, wherein the member in which the phase change material is contained is a member for preventing an adhering matter adhering to a wall surface of the vacuum vessel. .   The temperature control device in a vacuum vessel according to claim 1 or 2, wherein the member containing the phase change material is a backing plate that holds a sputtering target by bonding.   The temperature control device in a vacuum vessel according to claim 3, wherein the substrate is a substrate used for forming an optical thin film.   5. The phase change material having a melting point equal to or lower than an upper limit temperature at which the drive mechanism can operate is included in a member in the vicinity of the drive mechanism in which the phase change material is included. Temperature control device in a vacuum vessel.   The temperature control device in a vacuum vessel according to claim 9, wherein the drive mechanism includes at least a bearing or a gear, and the operable upper limit temperature is 150 ° C or lower. In the thin film formation method of controlling the temperature in the vacuum vessel by the temperature control means and forming a thin film on the substrate using a sputtering method, a CVD method or a vacuum deposition method,
A phase change material having a melting point in the vicinity of the processing temperature is included in a member constituting the vacuum vessel, and the temperature of the member in which the phase change material is included is set in the vicinity of the melting point of the phase change material. A thin film forming method comprising forming a thin film on the substrate after holding.   12. The method of forming a thin film according to claim 11, wherein the step of forming the thin film includes a process of forming a thin film on a substrate while rotating and / or straightly moving the substrate holder.   The step of forming the thin film includes a process of attaching the substrate to the substrate holder outside the vacuum vessel, placing the substrate in a transfer chamber connected to the vacuum vessel and heating, and then transferring the substrate to the vacuum vessel to form the thin film. The method for forming a thin film according to claim 11, wherein:   A member in the vicinity of the drive mechanism includes a phase change material having a melting point equal to or lower than the upper limit temperature at which the drive mechanism can be operated. After the phase change material is maintained at a temperature equal to or lower than the melting point, the substrate holder is moved by a drive function. The method of forming a thin film according to claim 11, comprising a process of forming a thin film by rotating and / or moving straight.

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