WO2009133841A1 - 水反応性Al膜の製造方法及び成膜室用構成部材 - Google Patents
水反応性Al膜の製造方法及び成膜室用構成部材 Download PDFInfo
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- WO2009133841A1 WO2009133841A1 PCT/JP2009/058260 JP2009058260W WO2009133841A1 WO 2009133841 A1 WO2009133841 A1 WO 2009133841A1 JP 2009058260 W JP2009058260 W JP 2009058260W WO 2009133841 A1 WO2009133841 A1 WO 2009133841A1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4404—Coatings or surface treatment on the inside of the reaction chamber or on parts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/067—Metallic material containing free particles of non-metal elements, e.g. carbon, silicon, boron, phosphorus or arsenic
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/08—Metallic material containing only metal elements
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/123—Spraying molten metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/129—Flame spraying
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/131—Wire arc spraying
Definitions
- the present invention relates to a method for producing a water-reactive Al film and a constituent member for a film forming chamber, and more particularly to a method for producing a water-reactive Al film by arc spraying and a constituent member for a film forming chamber covered with this Al film.
- a film forming material is provided during the film forming process in the film forming chamber constituent member provided in the apparatus.
- the film forming chamber component for example, a deposition plate for preventing the film from adhering to the inside of the vacuum vessel other than the substrate, a shutter, or a film used only for a predetermined place on the substrate.
- a mask, a tray for transporting a substrate, and the like can be given.
- a film having the same composition as the target thin film (thin film to be formed on the substrate) adheres to these members. These members are usually used repeatedly after removing the adhered film.
- the film that inevitably adheres to these film forming chamber components becomes thicker according to the working time of the film forming process.
- Such an attached film peels off as particles from the film forming chamber component due to the internal stress or stress due to repeated thermal history, adheres to the substrate, and causes film defects. Therefore, the film forming chamber component is removed from the film forming apparatus at a stage where the attached film does not peel off, washed to remove the attached film, and then surface-finished and reused. It is done regularly.
- the deposit on the film is peeled off. It is currently being reused.
- a sandblasting method, a wet etching method using acid or alkali, a peeling method using hydrogen embrittlement such as hydrogen peroxide, and a peeling method using electrolysis are generally performed. It has been broken. In this case, when the deposit is peeled off, the deposition preventing plate is not a little dissolved and damaged, so the number of reuses is limited. Therefore, it is desired to develop a film peeling method that minimizes damage to the deposition preventing plate.
- the concentration of the peeled film in the waste liquid generated in the chemical treatment such as acid or alkali treatment is low, the recovery cost of valuable metals becomes high and it is not profitable. In such a case, the present situation is that it is treated as waste.
- An object of the present invention is to solve the above-mentioned problems of the prior art, a method for producing an Al film capable of reacting and dissolving in an atmosphere containing moisture, and a film formation chamber covered with the Al film. It is in providing the structural member.
- a material obtained by adding 2 to 5 wt% In to 4NAl or 5NAl so as to have a uniform composition is melted, and this molten material is arc sprayed.
- Thermal spraying is performed on the surface of the substrate by the method, and rapid solidification is performed to form an Al film in which In is uniformly dispersed in Al crystal grains.
- the reactivity with water decreases, and if it exceeds 5 wt%, the reactivity with water becomes very high, and may react with moisture in the atmosphere.
- the Al sprayed film thus obtained is a film in which In crystal grains are uniformly dispersed in Al crystal grains and reacts easily in an atmosphere containing moisture to generate hydrogen. Dissolve.
- the method for producing a water-reactive Al film of the present invention is also based on 4NAl or 5NAl, taking into account 2-5 wt% In and the amount of impurity Si in Al, and 0% in total with the amount of impurity Si. 0.04 to 0.6 wt%, preferably 0.04 to 0.2 wt% of Si-added material was melted so that the composition was uniform, and this molten material was then applied to the substrate surface by arc spraying. By spraying and rapidly solidifying, an Al film in which In is uniformly dispersed in Al crystal grains is formed.
- the constituent member for the film forming chamber of the film forming apparatus of the present invention is characterized in that the water-reactive Al film is provided on the surface.
- the above-mentioned constituent member is a deposition plate, a shutter or a mask.
- the Al sprayed film obtained by the arc spraying method of the present invention can be easily manufactured at a low cost by a simple process.
- a thermal history from a film forming process of about 300 to 350 ° C. there is an effect that it has a property of reacting and dissolving in an atmosphere in which moisture exists.
- the Al film reacts in the presence of moisture and efficiently dissolves while generating hydrogen. Therefore, the film forming chamber components (for example, a deposition plate, a shutter, and the like) covered with the water-reactive Al film are used. If a film is formed using a film forming apparatus equipped with a mask, etc., an inevitable adhesion film made of a film deposition material that adheres to the surface of an adhesion-preventing plate or the like during the film formation process is reacted and dissolved in this Al film. Thus, it is possible to peel and separate from the constituent members for the film forming chamber, and it is possible to easily recover the valuable metal of the film forming material from the peeled attached film, and to increase the number of reuse of the constituent members.
- the film forming chamber components for example, a deposition plate, a shutter, and the like
- FIG. 6 is a graph showing the relationship between the heat treatment temperature (° C.) and the dissolution current density (mA / cm 2 ) for the Al film obtained in Example 1.
- the graph which shows the relationship between the heat processing temperature (degreeC) with respect to Al film
- the photograph which shows the peeling state of the adhesion film adhering to the base material of Al sprayed film obtained in Example 3.
- FIG. The graph which shows the relationship between the heat processing temperature (degreeC) with respect to Al sprayed film obtained in Example 4, and melt
- the film forming chamber undergoes a repeated thermal history.
- the surface of the constituent member provided in the deposition chamber such as an adhesion-preventing plate coated with the Al film of the present invention also undergoes a repeated thermal history. Therefore, the Al film at the time of thermal spray film formation before receiving the thermal history is stable and easy to handle, and the Al film with the inevitable attached film after the thermal history in the film forming process is the base material of the constituent member It is necessary to have a solubility (activity) that can be easily peeled off from the attached film and be stable.
- the water-reactive Al film obtained according to the present invention sufficiently satisfies such solubility.
- the upper limit temperature of the thermal history in the film forming chamber is, for example, about 300 to 350 ° C. in the case of film formation by sputtering, vacuum deposition, ion plating, CVD, etc. It is practically sufficient if the Al film having undergone the thermal history is water-reactive, and it is even better if the Al film having undergone the thermal history up to 350 ° C. is water-reactive. As will be described below, the water-reactive Al film in the present invention sufficiently satisfies such solubility.
- the dissolution current Evaluation is performed by density (mA / cm 2 ).
- This measurement method is a method of measuring the mass decrease before and after immersion of the sample in the treatment liquid and converting it to the value of current density from the surface area, immersion treatment time, and the like. If the dissolution current density measured by this method is 50 mA / cm 2 or more, the Al film with the unavoidable adhered film after the thermal history in the film forming process can be easily peeled from the substrate together with the adhered film. It can be said that it has solubility (activity).
- Al used in the present invention has a purity of 4N (99.99%) and 5N (99.999%).
- 2N (99%) Al and 3N (99.9%) Al obtained by electrolysis are further added to the solid phase during solidification by three-layer electrolysis or partial solidification (segregation). It can be obtained by a method using a temperature difference from the liquid phase.
- the main impurities in 4NAl and 5NAl are Fe and Si, and Cu, Ni, C, etc. are included in addition to them.
- the electrochemical potential difference between Al and In is very large, but if an Al natural oxide film exists, the ionization of Al does not proceed. However, once the natural oxide film is broken and directly bonded to In, the potential difference rapidly promotes the ionization of Al. At that time, In is present in a highly dispersed state in the Al crystal grains as it is without being chemically changed. Since In has a low melting point (157 ° C.) and does not form a solid solution with Al, a material obtained by melting Al and In so as to have a uniform composition while paying attention to the difference in density between Al and In is used. When thermal spraying is performed on the substrate according to the arc spraying method, a desired film is obtained by rapid solidification and its compression effect.
- the added In is highly dispersed in the Al crystal grains by the arc spraying process and is kept in direct contact with Al. Since In does not form a stable layer with Al, the Al / In interface retains high energy and reacts violently at the contact surface with moisture in an atmosphere where moisture exists.
- the reaction product mainly composed of AlOOH is pulverized without filming on the surface due to the mechanical action caused by the expansion of the generated H 2 bubbles. Dispersed into the liquid, the dissolution reaction proceeds continuously and explosively at the reaction interface that is renewed one after another.
- the Al—In system behavior as described above is more remarkable when the Al purity is higher, that is, when 4N and 5N than when 2N and 3N.
- the Al sprayed film is manufactured by forming a film on the surface of the substrate to be processed in a predetermined atmosphere using a composite material made of Al—In according to an arc spraying method. That is, 4NAl and In are prepared, 2-5 wt% In is mixed with this Al, In is uniformly dissolved in Al, processed into a rod or wire shape, and this is used as a thermal spray material.
- the desired water reaction is achieved by spraying and rapidly solidifying and coating the surface of the base material, which is a constituent member for a film forming chamber such as a deposition plate of a film forming apparatus, using Ar as a spraying gas by an arc spraying method.
- the base material provided with the property Al sprayed film can be manufactured.
- the sprayed film thus obtained is a film in which In crystal grains (grain size of 10 nm or less) are uniformly and highly dispersed in Al crystal grains.
- the conditions for performing the arc spraying process are air, N 2 or Ar atmosphere.
- the Al sprayed film made of the above 4NAl-In composite material has high activity in the state formed through the arc spraying process, and is too difficult to handle because it is too soluble in an atmosphere containing moisture.
- a predetermined amount of Si is added to this material, the resulting Al sprayed film is less active and easy to handle, and the film after thermal history becomes very active and has an atmosphere where moisture exists.
- High solubility (activity) is expressed. Therefore, depending on the composition ratio of In and Si, there is a case where the powder is pulverized at normal temperature in the atmosphere. In that case, in a dry atmosphere (even in a vacuum atmosphere) to prevent reaction with moisture in the atmosphere. It is preferable to store.
- 4NAl, In, and Si are prepared, and 2 to 5 wt% In and the amount of impurity Si in 4NAl are taken into account with respect to this Al, and the total amount of impurities is 0.04 to 0.6 wt%. %, Preferably 0.04 to 0.2 wt% of Si is blended, In and Si are uniformly dissolved in Al, and processed into a rod or wire shape as a thermal spray material.
- the desired water-reactive Al is obtained by spraying, using Ar as a spraying gas, spraying rapidly on the surface of the base material to be a constituent member for a film forming chamber such as a deposition plate of a film forming apparatus, and solidifying by coating.
- a base material provided with a sprayed film can be manufactured. As described above, the sprayed film thus obtained is a film in which In is uniformly and highly dispersed in Al crystal grains.
- the activity that is, the solubility
- the activity can be controlled while being formed by spraying. It becomes possible to prevent dissolution of the Al sprayed film due to reaction with moisture, and it becomes easy to handle.
- the upper limit of the temperature due to the thermal history in the film formation chamber is about 300 ° C.
- an Al composite material to which 0.04 to 0.6 wt%, preferably 0.05 to 0.5 wt% of Si is added is used.
- the reaction starts immediately after immersion, and hydrogen gas
- water becomes black due to the deposited In or the like and finally the sprayed film is completely dissolved, and Al, In and the like remain as precipitates in the hot water. This reaction proceeds more vigorously as the water temperature is higher.
- a deposition chamber constituent member such as a deposition plate or a shutter provided in the deposition chamber of the deposition apparatus
- the deposited film can be easily peeled off from the film forming chamber constituent member to which the film forming material has inevitably adhered, and valuable metals can be easily recovered.
- the stripping solution simply using water such as pure water, water vapor, or an aqueous solution without using chemicals, it is possible to avoid damage due to dissolution of the constituent members for the film forming chamber such as a deposition plate, The number of times of reuse increases dramatically compared to the case where chemicals are used. In addition, since no chemicals are used, processing costs are greatly reduced and environmental conservation is achieved. Furthermore, since many film-forming materials adhering to the film-forming chamber components such as a deposition plate do not dissolve in water, there is an advantage that the same composition as the film-forming material can be recovered as a solid in the same form. . Furthermore, not only does the recovery cost drop dramatically, but the recovery process is simplified, which has the advantage of expanding the range of recoverable materials.
- the sprayed film made of the water-reactive Al composite material of the present invention is applied to a film forming chamber constituent member such as a deposition plate.
- the deposited film made of the film forming material can be peeled off by immersing the film forming chamber constituent member having the film inevitably adhered during the film formation in water or by spraying water vapor.
- rare metals can be recovered. The recovery cost is low, and the film forming material can be recovered with high quality.
- 3NAl, 4NAl, and 5NAl were used as Al, and the relationship between Al purity and In concentration in the following Al-In composition and the solubility of the obtained sprayed film was compared.
- the addition amount of In is based on Al weight.
- the base material with the thermal spray film before being subjected to the heat treatment (0 ° C.) and the base material with the thermal spray film after the heat treatment are immersed in 300 ml of pure water at 80 ° C., and the solubility of each thermal spray film is determined by the current of the immersion liquid. The density was measured and examined. The obtained results are shown in FIG. In FIG. 1, the horizontal axis is the heat treatment temperature (° C.), and the vertical axis is the dissolution current density (mA / cm 2 ).
- 3NAl and 4NAl were used as Al, and the relationship between the sprayed gas species by the arc spraying method and the solubility of the obtained sprayed film was compared in the following Al—In composition.
- the addition amount of In is based on Al weight.
- the base material with the thermal spray film without heat treatment (0 ° C.) and the base material with the thermal spray film after the heat treatment were immersed in 300 ml of pure water at 60 ° C. and 80 ° C. was measured and examined.
- the obtained results are shown in FIG.
- the horizontal axis represents the heat treatment temperature (° C.)
- the vertical axis represents the dissolution current density (mA / cm 2 ).
- Air is used as the blowing gas, it is not shown in FIG. 2 because it hardly dissolved.
- a platinum (Pt) film was formed by using a sputtering apparatus provided with an adhesion-preventing plate whose surface was coated with 4NAl-3 wt% In (spraying gas: Ar) sprayed film (film thickness: 200 ⁇ m) obtained in Example 2.
- the Pt-attached adhesion plate was removed and treated with hot water at 80 ° C., and the sprayed film dissolved in 30 minutes.
- the Pt adhesion film was removed from the adhesion plate. It peeled. For this reason, Pt which is a film forming material could be easily recovered.
- AlOOH was precipitated in addition to In in the warm water.
- This example shows an example in which Si is added to control the activity (solubility) of the obtained Al sprayed film.
- a rod-type arc thermal spray (heat source: electrical energy, about 6000 ° C.) was sprayed onto the surface of the base material made of aluminum using Ar gas (spraying gas pressure: 50 psi) to form a sprayed film.
- Ar gas spraying gas pressure: 50 psi
- the substrate with the thermal spray film in a state before being subjected to the heat treatment (0 ° C.) and the substrate with the thermal spray film after the heat treatment (after the thermal history) were immersed in 300 ml of pure water at 80 ° C.
- the solubility was examined by measuring the current density of the immersion liquid. The obtained results are shown in FIG. In FIG. 4, the horizontal axis represents the heat treatment temperature (° C.), and the vertical axis represents the dissolution current density (mA / cm 2 ).
- Example 4 a sprayed film was formed in the same manner as in Example 1 (spraying gas: Ar).
- Each sprayed coating thus obtained was subjected to heat treatment (in the atmosphere, for 1 hour, furnace cooling) in the same manner as in Example 4.
- the substrate with the thermal spray film in a state before being subjected to the heat treatment (0 ° C.) and the substrate with the thermal spray film after the heat treatment (after the thermal history) were immersed in 300 ml of pure water at 80 ° C. The solubility was examined by measuring the current density of the immersion liquid.
- Example 4 As a result, the same tendency as in Example 4 was obtained.
- a predetermined amount of Si it was possible to control the activity, that is, the solubility, of the sprayed film before being subjected to the heat treatment while it was formed by spraying.
- the upper limit of the heat treatment temperature is about 300 ° C.
- an Al film is formed using an Al composite material in which the amount of In added is 2 wt% or more and 0.04 to 0.6 wt% of Si is added
- the upper limit of the heat treatment temperature is as high as about 350 ° C.
- an Al film is formed using an Al composite material in which the amount of In added is 2 wt% or more and 0.04 to 0.2 wt% of Si is added. It has been found that practical solubility can be obtained by forming.
- Example 4 Using the sputtering apparatus provided with an adhesion-preventing plate whose surface was coated with the 4NAl-3 wt% In-0.1 wt% Si sprayed film (film thickness 200 ⁇ m) obtained in Example 4, the film was formed according to the description in Example 3. The process was carried out and a peel test of the adhered film was performed. In the same manner as in Example 3, the sprayed film was dissolved, and the Pt adhesion film was peeled off from the deposition preventing plate.
- the surface of the film forming chamber component in the vacuum film forming apparatus for forming a metal or metal compound thin film by sputtering, vacuum deposition, ion plating, CVD, or the like reacts with water. Therefore, the unavoidable adhesion film adhering to the surface of the film forming chamber constituent member during the film forming process can be peeled off and collected in an atmosphere containing moisture. Therefore, the present invention increases the number of times the constituent members for the film forming chamber are reused and includes valuable metals in the field where these film forming apparatuses are used, for example, in the technical field such as semiconductor elements and electronic equipment. It can be used to recover the membrane material.
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Abstract
Description
・3NAl-3wt%In
・3NAl-4wt%In
・4NAl-2wt%In
・4NAl-3wt%In
・4NAl-4wt%In
・5NAl-1.5wt%In
・5NAl-2.5wt%In
・5NAl-3.5wt%In
・3NAl-3wt%In(吹き付けガス:Air)
・4NAl-3wt%In(吹き付けガス:Ar)
・4NAl-3wt%In(吹き付けガス:N2)
・4NAl-3wt%In(吹き付けガス:Air)
・4NAl-3wt%In-0.05wt%Si(このうち、不純物Si:90ppm)
・4NAl-3wt%In-0.1wt%Si(このうち、不純物Si:100ppm)
・4NAl-3wt%In-0.2wt%Si(このうち、不純物Si:100ppm)
・4NAl-2.6wt%In-0.5wt%Si(このうち、不純物Si:100ppm)
・4NAl-3wt%In-0.1wt%Si(このうち、不純物Si:100ppm)
・4NAl-4wt%In-0.5wt%Si(このうち、不純物Si:100ppm)
・5NAl-1.5wt%In-0.05wt%Si(このうち、不純物Si:100ppm)
・5NAl-2.6wt%In-0.1wt%Si(このうち、不純物Si:100ppm)
・5NAl-3.5wt%In-0.5wt%Si(このうち、不純物Si:100ppm)
Claims (4)
- 4NAl又は5NAlに、Al基準で、2~5wt%のInを添加した材料を組成が均一になるように溶融し、この溶融材料を、アーク溶射法により基材表面に対して溶射し、急冷凝固させることにより、Al結晶粒中にInが均一に分散してなるAl膜を形成することを特徴とする水反応性Al膜の製造方法。
- 4NAl又は5NAlに、Al基準で、2~5wt%のIn、及びAl中の不純物Si量を勘案して、不純物Si量との合計で0.04~0.6wt%となる量のSiを添加した材料を組成が均一になるように溶融し、この溶融材料を、アーク溶射法により基材表面に対して溶射し、急冷凝固させることにより、Al結晶粒中にInが均一に分散してなるAl膜を形成することを特徴とする水反応性Al膜の製造方法。
- 請求項1又は2記載の方法により製造された水反応性Al膜を表面に備えたことを特徴とする成膜装置の成膜室用構成部材。
- 前記構成部材が、防着板、シャッター又はマスクであることを特徴とする請求項3記載の成膜室用構成部材。
Priority Applications (5)
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JP2010510111A JP5371966B2 (ja) | 2008-04-30 | 2009-04-27 | 水反応性Al膜の製造方法及び成膜室用構成部材 |
EP09738778A EP2280091B9 (en) | 2008-04-30 | 2009-04-27 | METHOD FOR PRODUCTION OF WATER-REACTIVE Al FILM, AND STRUCTURAL MEMBER FOR FILM-FORMING CHAMBER |
RU2010148780/02A RU2468119C2 (ru) | 2008-04-30 | 2009-04-27 | СПОСОБ ПОЛУЧЕНИЯ РЕАГИРУЮЩЕЙ С ВОДОЙ Al ПЛЕНКИ И СОСТАВЛЯЮЩИЙ ЭЛЕМЕНТ ПЛЕНКООБРАЗУЮЩЕЙ КАМЕРЫ |
CN2009801154076A CN102016099B (zh) | 2008-04-30 | 2009-04-27 | 水反应性Al膜的制造方法及成膜室用构成部件 |
US12/990,152 US8596216B2 (en) | 2008-04-30 | 2009-04-27 | Method for the production of water-reactive Al film and constituent member for film-forming chamber |
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PCT/JP2009/058260 WO2009133841A1 (ja) | 2008-04-30 | 2009-04-27 | 水反応性Al膜の製造方法及び成膜室用構成部材 |
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US (1) | US8596216B2 (ja) |
EP (1) | EP2280091B9 (ja) |
JP (1) | JP5371966B2 (ja) |
KR (1) | KR20100136560A (ja) |
CN (1) | CN102016099B (ja) |
MY (1) | MY150439A (ja) |
RU (1) | RU2468119C2 (ja) |
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CN103228814A (zh) * | 2010-08-27 | 2013-07-31 | 株式会社爱发科 | 水反应性Al复合材料、水反应性Al喷镀膜、该Al喷镀膜的制造方法及成膜室用构成构件 |
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RU2468116C2 (ru) * | 2008-04-30 | 2012-11-27 | Улвак, Инк. | СПОСОБ ПОЛУЧЕНИЯ РЕАГИРУЮЩЕЙ С ВОДОЙ Al ПЛЕНКИ И СОСТАВЛЯЮЩИЙ ЭЛЕМЕНТ ПЛЕНКООБРАЗУЮЩЕЙ КАМЕРЫ |
US20150060263A1 (en) * | 2012-03-29 | 2015-03-05 | Toray Industries, Inc. | Vacuum film deposition device and vacuum film deposition method |
ITBA20130034A1 (it) * | 2013-04-30 | 2014-10-31 | Mrs S R L | Metodo per la pulizia di superfici in apparati di deposizione di film sottili da fase vapore e per il recupero del materiale rimosso |
CN106222617A (zh) * | 2016-08-26 | 2016-12-14 | 武汉华星光电技术有限公司 | 用于镀膜设备的防着板结构及其制造方法、镀膜设备 |
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US20110041762A1 (en) | 2011-02-24 |
TW201009120A (en) | 2010-03-01 |
RU2468119C2 (ru) | 2012-11-27 |
EP2280091B1 (en) | 2012-08-08 |
SG189753A1 (en) | 2013-05-31 |
JPWO2009133841A1 (ja) | 2011-09-01 |
US8596216B2 (en) | 2013-12-03 |
CN102016099B (zh) | 2012-10-10 |
TWI464300B (zh) | 2014-12-11 |
MY150439A (en) | 2014-01-30 |
EP2280091A4 (en) | 2011-04-20 |
EP2280091B9 (en) | 2013-03-27 |
KR20100136560A (ko) | 2010-12-28 |
JP5371966B2 (ja) | 2013-12-18 |
EP2280091A1 (en) | 2011-02-02 |
CN102016099A (zh) | 2011-04-13 |
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