JP2009287058A - Film-forming method by direct-current reactive facing target type sputtering, pure yttria corrosion-resistant film formed with the film-forming method, and corrosion-resistant quartz assembly - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a film-forming method by direct-current reactive facing target type sputtering, which can form a pure yttria corrosion-resistant film on a substrate at a high film-forming rate, and has superior mass productivity. <P>SOLUTION: This film-forming method includes: arranging a pair of targets 5 and 5 made from yttrium metal so as to face to each other in a target arrangement region 2 in a vacuum chamber 1; arranging a substrate 7 in a film-forming region 3; applying direct-current voltage to the targets 5 and 5; constraining plasma P which has been generated in between the targets 5 and 5 within a space between the targets 5 and 5 by a magnetic field and also supplying an inert gas such as argon gas into the space of the magnetic field; on the other hand, setting a pressure of the inert gas in the vacuum chamber 1 to 0.01 to 1.0 Pa while supplying a reactive gas such as oxygen gas toward the substrate 7; and coupling an yttrium metal atom with a reactive gas on the surface of the substrate 7 without substantially introducing the reactive gas into the plasma P to form the pure yttria corrosion-resistant film on the substrate 7. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a DC reactive counter target sputtering film forming method for forming a pure yttria corrosion-resistant film on the surface of a component in a semiconductor processing apparatus and an electronic component manufacturing apparatus, and pure yttria formed by the film forming method. The present invention relates to a corrosion-resistant film and a corrosion-resistant quartz structure.

  For example, in a semiconductor process, a film forming or etching gas is supplied into a vacuum chamber, and the gas is turned into plasma at high frequency to be activated, and a thin film is formed on the substrate by etching or chemical vapor deposition (CVD). Etc. are performed. The inductively coupled plasma reactor, the electron cyclotron resonance reactor, and their components existing in such a process are exposed to a fluorine-based plasma chamber gas, so that excellent corrosion resistance is required. In addition, quality degradation of semiconductor products due to particle and heavy metal contamination must be prevented. Therefore, it is an important requirement that the surfaces of the component parts and the like are covered with a dense and uniform coating having excellent corrosion resistance. In addition, semiconductor processes such as silicon wafers and processes related to flat panel displays require a high-purity environment in which foreign substances such as particles are more severely removed. Therefore, components with higher corrosion resistance are required. Yes.

  For example, a conductive sputtering target for forming a thin film containing amorphous yttria on a substrate by a DC magnetron sputtering method and a method for manufacturing the same have been proposed (see, for example, Patent Document 1). The conductive sputtering target is said to contain amorphous carbon and at least 35% by volume yttria based on the total volume of the target. A thin film formed by such a target is said to have good electrical and optical properties and can be used as a protective coating and a chemical resistant coating.

  In addition, a component of a semiconductor processing apparatus in which a film containing boron nitride or a yttria composite material is formed on the surface and a manufacturing method thereof have been proposed (for example, see Patent Document 2). The coating is supposed to be formed by any well-known coating technique such as thermal spraying, plasma spraying, chemical vapor deposition (CVD), sublimation, laser deposition, sputtering (hereinafter abbreviated).

Alternatively, a plasma processing apparatus and a plasma processing method have been proposed in which yttria (Y ₂ O ₃ ) is coated on a component exposed to plasma in the apparatus (see, for example, Patent Document 3). By applying such yttria coating to the constituent members in the plasma processing apparatus, it is said that contamination can be prevented from occurring in the film formed by the plasma processing apparatus by directly sputtering those members. . The coating is preferably formed by plasma spraying, CVD, sputtering, ion grating method or the like.

Japanese Patent Laid-Open No. 7-180045 Special Table 2004-523649 JP 2005-268763 A

  As described above, there is a description about the point of forming an yttria film or an yttria-containing film in a plurality of documents, but a long period of use in a severe environment such as being exposed to a fluorine-based plasma chamber gas in a semiconductor process or the like. An yttria film-forming member suitable for the purpose of use capable of maintaining good corrosion resistance has not been put into practical use yet.

  Since the sputtering target described in Patent Document 1 contains amorphous carbon in yttria in order to impart conductivity, the thin film formed by such a target is not pure yttria, such as a carbon compound. Impurities are mixed. When such a thin film is applied to, for example, a surface coating of a component in a semiconductor processing apparatus or an electronic component manufacturing apparatus that is exposed to plasma, there is a concern that corrosion may proceed from that portion due to the presence of the impurities. .

  In addition, as described in Patent Documents 2 and 3, when a film containing an yttria composite material or an yttria film is formed by plasma spraying, the film has a weak adhesion to the substrate and easily peels off, and has many pinholes. It will be a thing. A plasma chamber gas enters the pinholes and corrosion easily proceeds. Therefore, it is not possible to bring out the original characteristic of yttria that is excellent in corrosion resistance against the plasma chamber gas. Moreover, the film thickness becomes comparatively thick, for example, there also exists a difficulty that it cannot form in the film thickness of 1 micrometer or less.

  The present invention has been made in view of such circumstances, and one of its purposes is to provide a dense and homogeneous pure yttria on various substrates in order to improve the corrosion resistance of the semiconductor processing apparatus and its components. It is an object to provide a direct-current reactive target sputtering deposition method capable of forming a corrosion-resistant film, a pure yttria corrosion-resistant film formed by the film-forming method, and a corrosion-resistant quartz structure.

  Another object of the present invention is to provide a direct-current reactive target sputtering method for forming a pure yttria anticorrosive film on various substrates at a high film formation rate, and a pure yttria anticorrosive film formed by the film forming method. And providing a corrosion resistant quartz construction.

  As a result of various studies on the yttria film forming method, the present inventor has found that a practical yttria film forming is possible according to the direct current reactive mirrortron type sputtering film forming method using metal yttrium as a target. Obtaining knowledge, the present invention has been completed.

  The direct-current reactive counter-target type sputtering film forming method of the present invention relates to a direct-current reactive counter-target type sputtering film forming method for forming a pure yttria corrosion-resistant film on a substrate. In this direct current reactive target sputtering method, a target placement region and a film formation region are provided in a vacuum chamber. In the target arrangement region, a pair of targets made of yttrium metal are arranged to face each other, and the base material is arranged in the film formation region. A DC voltage is applied to the target to generate plasma between the targets, the plasma is restrained between the targets by a magnetic field, and an inert gas such as argon gas is supplied to the magnetic field space. Meanwhile, while supplying a reactive gas such as oxygen gas toward the substrate, the pressure of the inert gas in the vacuum chamber is set to 0.01 to 1.0 Pa, and the reactive gas is substantially contained in the plasma. Without intruding, a yttrium metal atom and a reactive gas are bonded on the surface of the base material to form a pure yttria corrosion-resistant film on the base material.

  In such a method, since plasma is generated between a pair of targets arranged opposite to each other, the plasma peripheral magnetic field is strong and the density near the plasma boundary is high. Therefore, a state in which a reactive gas such as oxygen gas does not easily enter into the plasma is formed, and the film formation region is partitioned from the target placement region, so that it is not directly affected by the plasma, A pure yttria corrosion-resistant film having high purity can be formed at a high film formation rate by substantially bonding only yttrium metal atoms and reactive gas on the substrate surface. The film formation rate (film formation rate) can be set, for example, from 20 nm to 200 nm / min (input power Pw = 1 kW to 5 kW), as will be apparent from Examples described later. When Pw = 2 kW, 120 nm / Min can be secured. In contrast, the RF bipolar reactive sputtering method can ensure only 8 nm / min, and the DC magnetron reactive sputtering method can only ensure 12 nm / min.

  And by setting the pressure of the inert gas in the vacuum chamber to a low gas pressure of 0.01 to 1.0 Pa, free movement of yttrium metal atoms is allowed on the surface of the base material. In this way, a fine grain-sized dense-packed and uniform mirror-like film can be formed. Note that when the pressure of the inert gas in the vacuum chamber becomes lower than 0.01 Pa, the discharge voltage becomes too high. Further, when the pressure of the inert gas is higher than 1.0 Pa, the sputtered particles (yttrium metal atoms) are clustered (powdered), so that the denseness of the film is lowered and the corrosion resistance is also lowered. Furthermore, since the target arrangement region and the film formation region are partitioned, the target arrangement region and the film formation region are independently formed into film formation conditions (in the target arrangement region, the DC applied voltage and the flow rate of the inert gas, the film formation region Can control the flow rate of the reactive gas, etc., so that the film forming process can be simplified and simplified, the film composition can be easily controlled, and desired film characteristics can be easily imparted. Become. In addition, according to the direct current reactive counter target type sputtering film forming method, a thin film can be formed. In particular, a thin film having a thickness of 1 μm or less can be formed without roughening the surface. This is presumably because the sputtering pressure can be set low.

  In such a DC reactive facing target type sputtering film forming method, the periphery of the target is covered with a shield cover having an opening formed of a conductive material that is not melted by the heat of the plasma, and the target is opened from the opening. It is preferable that the shield cover is connected to the ground potential. By providing such a shield cover, the DC power supply circuit can be held in a closed state via the shield cover without spattering members other than the target, thereby increasing the discharge voltage in the container. Therefore, the occurrence of abnormal discharge (arc) can be effectively prevented. Therefore, the film forming operation can be continued for a long time.

  In this direct current reactive facing target type sputtering film forming method, the base material is either quartz, metal or ceramics, and the temperature of the base material is maintained at 600 ° C. or less, particularly 400 to 600 ° C. A corrosion-resistant film can also be formed. Quartz has a heat-resistant temperature of 1,000 ° C or higher, and metals and ceramics have a high heat-resistant temperature. Therefore, when these are used as base materials, the base temperature can be maintained at 400 to 600 ° C., and a pure yttria corrosion-resistant film can be efficiently formed.

For example, when forming a pure yttria corrosion-resistant film on the surface of various quartz parts used in semiconductor processes, input power 2.0-5.0 kW, current 5-10 A, sputtering pressure 0.05-0.1 Pa, Ar flow rate 30-80 sccm, 0 ₂ A uniform pure yttria corrosion-resistant film can be formed at a flow rate of 15 to 50 sccm while maintaining the temperature of the substrate surface at about 400 to 600 ° C.

In the direct current reactive target sputtering method, the base material is a resin material such as plastic, and the temperature of the base material is maintained at room temperature to 150 ° C. to form a pure yttria corrosion-resistant film. . For example, when the acrylic or polyethylene terephthalate base material, input power 2 kW, a sputtering pressure 0.05 Pa, even one hour deposition in Ar flow rate 50 sccm, 0 ₂ flow rate 50 sccm, temperature of the substrate surface to 100 ° C. or less be able to. Therefore, a homogeneous pure yttria corrosion-resistant film can be formed even on a resin material having a low heat-resistant temperature. For example, it is considered that a plastic having a softening point of about 150 ° C. or lower can be used as the base material.

  The pure yttria corrosion-resistant film of the present invention is a pure yttria corrosion-resistant film formed by any one of the above-described direct-current reactive counter target sputtering film forming methods, and has a film thickness of 1 μm or less. In the direct current reactive facing target type sputtering film forming method, as described above, the film thickness can be easily controlled, and a homogeneous pure yttria corrosion resistant film having a thickness of 1 μm or less can be formed. Such a pure yttria anti-corrosion film is not only a coating on the surface of semiconductor processing equipment exposed to plasma and components in an electronic component manufacturing apparatus, but also various parts in the field of semiconductor microfabrication processes where a thin coating is desired, If it is applied to coatings such as products, it is possible to significantly improve durability, downsize and reduce costs, and thus contribute to resource saving.

  Still another pure yttria corrosion-resistant film of the present invention is a pure yttria corrosion-resistant film formed by any one of the above-described direct-current reactive counter target type sputtering film forming methods, and has a light transmittance of 90% or more for visible light. It is characterized by being. Pure yttria anti-corrosion film has a uniform surface and high corrosion resistance even though it is thin, so it is also suitable for covering observation windows made of quartz in semiconductor processing equipment and various quartz parts used in semiconductor processes. is there. Moreover, since the optical properties are good and the film thickness is thin and the surface can be formed into a mirror surface, it can be suitably used as a protective coating for optical components. This light transmittance is particularly preferably 95% or more.

  The corrosion-resistant quartz structure of the present invention is characterized in that the pure yttria corrosion-resistant film described above is coated on the surface of quartz. In the semiconductor process, various quartz parts (containers, pipes, etc.) are used for each process. Conventionally, these parts are often exposed to plasma gas and corroded and deformed. In many cases, it was used for reuse. However, by applying a pure yttria anti-corrosion film to these quartz parts, the durability against plasma gas can be drastically improved, so that it can be used for a long time without being subjected to reprocessing. Therefore, the running cost of the semiconductor process can be greatly reduced.

  In the direct-current reactive target sputtering method of the present invention, the pressure of the inert gas in the vacuum chamber is set to a low gas pressure of 0.01 to 1.0 Pa, so that the yttrium metal atoms on the surface of the substrate are free. It is possible to form a dense and uniform film while allowing a smooth movement and maintaining the substrate temperature at a low temperature.

  The pure yttria corrosion-resistant film of the present invention is not only a coating on the surface of a semiconductor processing apparatus exposed to plasma or a component part in an electronic component manufacturing apparatus, but also various parts in the field of semiconductor microfabrication process where a thin coating is desired, If it is used for a product, etc., it is possible to significantly improve durability, downsize and reduce costs, and to contribute to resource saving.

  Hereinafter, embodiments of the direct-current reactive counter target (mirrortron) type sputtering film forming method of the present invention will be described. FIG. 1 is an explanatory view showing a basic configuration of a direct-current reactive target sputtering system (hereinafter referred to as a sputtering apparatus). This sputtering apparatus is partitioned by a partition wall 2 in a vacuum chamber 1. The target arrangement region 3 and the film formation region 4 are provided, and a pair of targets 5 and 5 made of yttrium metal are arranged in the target arrangement region 3 so as to face each other, and a ring-shaped magnet is provided on the back side of the targets 5 and 5. 6,6 are arranged. On the other hand, a base material 7 is disposed in the film formation region 4.

Then, a DC voltage is applied to the targets 5 and 5 to generate plasma P between the targets 5 and 5, and the plasma P is restrained by a magnetic field between the targets 5 and 5, and argon gas or the like is placed in the magnetic field space. While supplying an inert gas, while supplying a reactive gas such as oxygen gas toward the base material 7, the pressure of the inert gas in the vacuum chamber 1 is set to 0.01 to 1.0 Pa to react in the plasma P. A pure yttria corrosion-resistant film is formed on the base material 7 by bonding the yttrium metal atom and the reactive gas (O ₂ ) on the surface of the base material 7 without substantially invading the reactive gas. The surroundings of the targets 5 and 5 are respectively covered with shield covers 10 and 10 formed of a conductive material that is not melted by the heat of the plasma P, and the targets 5 and 5 are made into the constraining region of the plasma P from the openings 11 and 11. The shield covers 10 and 10 are connected to the ground potential.

  In the sputtering apparatus configured in this manner, the plasma P generated between a pair of targets 5 and 5 arranged facing each other is constrained by a magnetic field around the plasma that is stronger than the central part. The density is high. Therefore, a state in which oxygen gas is difficult to enter into the plasma P is formed. Since the film formation chamber 4 is partitioned from the target chamber 3 by the partition wall 2, substantially only yttrium metal atoms and reactive gas are not affected by the plasma P directly on the surface of the base material 7. Thus, a pure yttria corrosion-resistant film with high purity can be formed at a high film formation rate. Moreover, since the targets 5 and 5 are consumed evenly without being reduced, the target utilization efficiency is high.

  Since the inert gas pressure in the vacuum chamber 1 is set to a low gas pressure of about 0.01 to 1.0 Pa, free movement of yttrium metal atoms on the surface of the substrate 7 is allowed. A fine grain-sized dense-packed and uniform film can be formed while maintaining the material temperature at a low temperature. Further, since the target chamber 3 and the film forming chamber 4 are partitioned, the target chamber 3 and the film forming chamber 4 are controlled independently (in the target arrangement region, a DC applied voltage, an inert gas flow rate, a film forming region). In this case, the flow rate of the reactive gas etc. can be simplified, so that the film forming process can be simplified and simplified, the film composition can be easily controlled, and the desired film characteristics can be imparted. .

  Further, the surroundings of the targets 5 and 5 are covered with shield covers 10 and 10 formed of a conductive material such as stainless steel that is not melted by the heat of the plasma P, and the targets 5 and 5 are plasma from the openings 11 and 11. The shield covers 10 and 10 are connected to the ground potential while facing the restricted region of P. The shield covers 10 and 10 are preferably formed with thin portions that are heated to a red hot state by the plasma P. By providing such shield covers 10, 10, no insulating film is formed on the red-hot portions, and members other than the targets 5, 5 are not sputtered, and the shield covers 10, 10 10, the DC power supply circuit can always be kept closed. Therefore, the occurrence of abnormal discharge (arc) can be effectively prevented without increasing the discharge voltage in the vacuum chamber 1. Thereby, sputtering operation (film formation operation) can be continued for a long time, and excellent mass productivity can be ensured.

  Using the above apparatus, a pure yttria film was formed on a quartz substrate under the conditions shown in Table 1 by the direct current reactive target sputtering deposition method (reactive mirrortron sputtering) of the present invention. Here, the sputtering pressure in the vacuum chamber 1 was changed in the range of 0.01 to 1.0 Pa to obtain Sample 1 to Sample 5.

Further, as a sample 6, a pure yttria film was formed on a quartz substrate 7 by a DC magnetron sputtering apparatus as shown in FIG. In this magnetron sputtering apparatus, a target 5 made of yttrium metal is placed in a vacuum chamber 1, a base material 7 made of quartz is placed facing the target 5, and the plasma P is restrained on the back side of the target 5. The magnet 6 is arranged. The base material 7 is covered with a shield cover 10, and the target 5 faces the constraining region of the plasma P from the opening 11. The vacuum chamber 1 is evacuated by a vacuum pump 8, and argon gas (Ar) and oxygen gas (O ₂ ) are supplied to the magnetic field space.

  Further, as a sample 7, a pure yttria film was formed on a quartz substrate with an RF sputtering apparatus (using an RF bipolar reactive sputtering method). This apparatus is different from the apparatus of FIG. 2 in that the power source applied to the target is a high frequency power source and that no magnet is used.

  Regarding the film forming conditions for producing each sample, the film forming speed and film forming continuity were evaluated, and the yttria film obtained under each condition was evaluated for the corrosion resistance of the film, the degree of droplets, and the transmittance. And about some samples, the sample cross section was observed with the optical microscope, and the film | membrane structure was considered. The evaluation results of the film are shown in Table 2.

  The film formation rate was evaluated based on the film formation thickness per minute. The film formation rate is less than 10 nm / min, x, 10 nm / min or more and less than 20 nm / min is Δ, 20 nm / min or more and less than 40 nm / min is ◯, and 40 nm / min or more is ◎.

  Deposition continuity is ◎ when the film can be formed continuously for 5 days or more under the same conditions as in Table 1, and when it can be formed continuously for 2 days or more but less than 5 days, ○, 2 days The case of less than was made x.

  Corrosion resistance was evaluated by exposing the obtained sample to a fluorine plasma gas used in a chamber of a semiconductor processing apparatus and conducting a corrosion resistance test, and comparing the time during which peeling occurs on the yttria film. “X” indicates that the time from the start of the corrosion resistance test to peeling is less than 1 day, “◯” indicates that the time is from 1 day to less than 6 days, and “◎” indicates that the time is 6 days or more.

  The droplets were evaluated by magnifying and observing the yttria film with an optical microscope and counting the number of droplets per predetermined area. Here, it is examined whether droplets are observed in the observation area of 3 mm square per place in two places of the center part and the outer peripheral part of the yttria film having a diameter of 4 inches. Then, the total number of droplets in the two observation areas is measured and evaluated. The number of droplets is 0, ◎, the number of 1 to 3 is ◯, and the number of 4 or more is △.

  The light transmittance was determined by measuring the light transmittance of each sample with a commercially available visible light transmittance meter. The wavelength of visible light used for measurement is 550 nm. A light transmittance of 95% or more is marked with ◎, and a light transmittance of 90% or more is marked with ○.

  Then, the practicality of the film forming method and the characteristics of the yttria film was comprehensively evaluated. This evaluation is carried out in four stages, and 及 び and 〇 indicate those that can be used practically, and Δ indicates those that cannot be used practically.

  As is apparent from Table 1, Samples 1 to 5 in which the sputtering pressure in the vacuum chamber 1 is set to a relatively low value within the range of 0.01 to 1.0 Pa have a high film formation speed and a short film formation time. A dense and high-quality yttria coating that can be put to practical use could be formed on a quartz substrate. When this film formation rate was converted into a film formation rate, it was 40 nm / min or more. Moreover, as a result of observing the cross section of the yttria film of Sample 1 with a high-sensitivity electron microscope, a large number of thin short fibers are arranged along the thickness direction of the film, and the large number of short fibers are perpendicular to the thickness direction of the film. A dense parallel membrane structure was observed.

  On the other hand, when the sputtering pressure is less than 0.01 Pa, the discharge voltage becomes high, and it is considered that a dense and high-quality yttria coating cannot be formed on the quartz substrate. In addition, when the sputtering pressure is higher than 1.0 Pa, the sputtered particles (yttrium metal atoms) are likely to be clustered (powdered), and the denseness of the film is lowered and the corrosion resistance is also lowered.

  On the other hand, in the sample 6 formed by the DC magnetron sputtering method, as a result of observation with an electron microscope, the yttria coating had a columnar rough film structure. Moreover, in this sample 6, the sputtering pressure was high, and it became easy to generate | occur | produce an arc, and many droplets were seen compared with the samples 1-5. In order to reduce the occurrence of such droplets, the input power may be reduced to, for example, about 100 W. However, if such a measure is taken, the film formation speed will be further reduced, so that mass productivity can be expected at all. Disappear. And also in the result of the corrosion resistance test, the sample 6 was significantly inferior to the samples 1 to 5.

  This is considered to be due to the following reasons. When a pure yttria corrosion-resistant film is formed by a magnetron sputtering apparatus, the base material 5 is impacted by high-energy particles because the base material 5 exists in the plasma P due to the structure of the apparatus. That is, the base material 5 has a kinetic energy equivalent to the target applied voltage, and the gamma electrons of the secondary electrons colliding along the magnetic field lines, so that the kinetic energy is heated and the base material temperature becomes 200 ° C. or higher. Become. Further, since negative charges are charged up by the impact of gamma electrons, the self-bias of the base material 5 becomes negative, and this time, positive argon ions collide with the base material 5. Since the mass of the argon ions is the same as that of the film atoms, defects are generated in the film or lattice defects are generated by resputtering. Therefore, when the film surface is roughened and such a film is exposed to a fluorine plasma gas, corrosion tends to proceed. In addition, when reactive sputtering is applied, in particular, oxygen tends to be negative ions, and, like electrons, impinges on the base material 5 to cause a large film damage. An yttria corrosion-resistant film could not be formed. The film structure is in the form of forested columnar grains, and the surface is not smooth. Therefore, it is estimated that the plasma gas easily enters the gaps between the columnar grains and is easily corroded.

  Furthermore, Sample 7 was the same as Sample 1 to Sample 5 in terms of film continuity, film structure, and some of the droplets, but the film formation rate was significantly slow. When this film formation rate was converted into a film formation rate, it was less than 10 nm / min. Therefore, the film forming method of Sample 7 is hardly a practical film forming method.

  Next, a case where a pure yttria corrosion-resistant film is formed on the surface of polyethylene terephthalate (PET) by the direct-current reactive facing target type sputtering film forming method of the present invention will be described using the apparatus shown in FIG. As shown in Table 3, the sputtering pressure in the vacuum chamber 1 was changed in the range of 0.01 to 1.0 Pa to obtain Sample 11 to Sample 14.

  Table 4 shows the evaluation of each sample. The evaluation criteria for film formation speed and film formation continuity were the same as those in Example 1. Further, comprehensive evaluation of practicality is also performed in four stages according to the case of Example 1, ◯ indicates that it can be used practically, and ◎ indicates that it is particularly excellent in evaluation.

In the DC magnetron sputtering method and the RF bipolar sputtering method, the substrate temperature becomes 200 ° C. or more in all conditions under the conditions of Ar: 60 sccm, O ₂ : 30 sccm, gas pressure: 1 Pa, input power: 2 to 3 kW, Since it has been found that this is not applicable when a resin material is used as a base material, no film is formed.

  In Samples 11 to 14, the sputtering pressure was set to a low value in the range of 0.01 to 1.0 Pa, so that a high-quality yttria coating that can be used practically with a high film formation speed and a short film formation time was formed on the resin substrate. Could be formed. On the other hand, when the sputtering pressure is higher than the above range, the sputtered particles (yttrium metal atoms) are clustered (powdered), and the denseness of the film is lowered and the corrosion resistance is also lowered. The samples 11 to 14 can be used as an optical thin film, for example. Further, acrylic, PET, or the like can be applied to the substrate. Moreover, it can use for a sealing member, a film, etc. as the use. When such a pure yttria corrosion-resistant film is formed on the surface of a resin material, a high-quality film with few film defects can be formed at the time of film formation, and there is little damage such as film peeling at the time of use, and it has excellent durability. It can be set as the covering member.

  It should be noted that the present invention is not limited to the embodiment, and can be freely improved, changed, etc. as necessary without departing from the gist of the invention.

  The direct current reactive target sputtering film forming method of the present invention can be suitably applied to surface film formation of components and the like in semiconductor processing apparatuses and electronic component manufacturing apparatuses.

  The pure yttria corrosion-resistant film and the corrosion-resistant quartz structure of the present invention can be suitably applied to various parts and products in the field of semiconductor microfabrication processes.

It is composition explanatory drawing of the sputtering device for enforcing the direct current | flow reactive counter type sputtering film-forming method of this invention. FIG. 3 is a configuration explanatory diagram of a magnetron sputtering apparatus applied to a sample 6.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Vacuum chamber 2 Partition wall 3 Target room 4 Film-forming room 5 Target 6 Magnet 7 Base material 8 Vacuum pump 9 Pure yttria corrosion-resistant film 10 Shield cover 11 Opening P Plasma

Claims (6)

A direct-current reactive counter-target sputtering method for forming a pure yttria corrosion-resistant film on a substrate,
In the vacuum chamber, a target arrangement region and a film formation region which are partitioned from each other are provided, and a target made of a pair of yttrium metals is arranged in the target arrangement region so as to face each other, and the substrate is arranged in the film formation region. A material is arranged, a DC voltage is applied to the target, plasma is generated between the targets, the plasma is constrained by a magnetic field between the targets, and an inert gas such as argon gas is supplied to the magnetic field space. Meanwhile, while supplying a reactive gas such as oxygen gas toward the substrate, the pressure of the inert gas in the vacuum chamber is set to 0.01 to 1.0 Pa, and the reactive gas is substantially contained in the plasma. A pure yttria corrosion-resistant film is formed on the substrate by bonding yttrium metal atoms and a reactive gas on the substrate surface without intrusion. Reactive facing target system sputtering deposition method. 2. The direct current according to claim 1, wherein the base material is any one of quartz, metal, and ceramics, and the temperature of the base material is maintained at room temperature to 600 ° C. to form a pure yttria corrosion-resistant film. Reactive facing target type sputtering film forming method. 2. The direct-current reactive counter target according to claim 1, wherein the base material is a resin material such as plastic and the temperature of the base material is maintained at room temperature to 150 ° C. to form a pure yttria corrosion-resistant film. Sputtering deposition method. A pure yttria corrosion-resistant film formed by the direct-current reactive facing target-type sputtering film-forming method according to any one of claims 1 to 3, wherein the film thickness is 10 µm or less. film. A pure yttria corrosion-resistant film formed by the direct-current reactive target-type sputtering film-forming method according to any one of claims 1 to 3, wherein the light transmittance for visible light is 90% or more, A pure yttria corrosion-resistant film characterized in that the material is made of a light-transmitting material. 6. A corrosion-resistant quartz structure comprising the quartz surface coated with the pure yttria corrosion-resistant film according to claim 4 or 5.

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