US20240271310A1 - Reaction chamber component, preparation method, and reaction chamber - Google Patents

Reaction chamber component, preparation method, and reaction chamber Download PDF

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US20240271310A1
US20240271310A1 US18/626,331 US202418626331A US2024271310A1 US 20240271310 A1 US20240271310 A1 US 20240271310A1 US 202418626331 A US202418626331 A US 202418626331A US 2024271310 A1 US2024271310 A1 US 2024271310A1
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oxide film
film layer
reaction chamber
layer
substrate
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Yicheng Li
Yulin Peng
Yongyou CAO
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Beijing Naura Microelectronics Equipment Co Ltd
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Beijing Naura Microelectronics Equipment Co Ltd
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Priority claimed from CN201820317132.0U external-priority patent/CN208580713U/en
Priority claimed from CN201810190001.5A external-priority patent/CN110246738A/en
Priority claimed from PCT/CN2018/118897 external-priority patent/WO2019169912A1/en
Application filed by Beijing Naura Microelectronics Equipment Co Ltd filed Critical Beijing Naura Microelectronics Equipment Co Ltd
Priority to US18/626,331 priority Critical patent/US20240271310A1/en
Assigned to BEIJING NAURA MICROELECTRONICS EQUIPMENT CO., LTD. reassignment BEIJING NAURA MICROELECTRONICS EQUIPMENT CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CAO, Yongyou, LI, YICHENG, PENG, YULIN
Publication of US20240271310A1 publication Critical patent/US20240271310A1/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C24/00Coating starting from inorganic powder
    • C23C24/02Coating starting from inorganic powder by application of pressure only
    • C23C24/04Impact or kinetic deposition of particles
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/12Anodising more than once, e.g. in different baths
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/16Pretreatment, e.g. desmutting
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/18After-treatment, e.g. pore-sealing
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/18After-treatment, e.g. pore-sealing
    • C25D11/24Chemical after-treatment
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/18After-treatment, e.g. pore-sealing
    • C25D11/24Chemical after-treatment
    • C25D11/246Chemical after-treatment for sealing layers
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated
    • C25D5/42Pretreatment of metallic surfaces to be electroplated of light metals
    • C25D5/44Aluminium

Definitions

  • the disclosure belongs to the technical field of microelectronics processing, and in particular relates to a reaction chamber component, a preparation method, and a reaction chamber.
  • aluminum alloy is widely used to manufacture the reaction chamber component for the production of plasma. This is because not only the aluminum alloy has high strength and good weldability, but also the anode oxide film of aluminum alloy has good corrosion resistance. However, the aluminum alloy contains a large number of alloy elements, such as Mg, Cu, Zn, Mn, Fe, Si, etc.
  • the reacting gases used in the reaction chamber include CF 4 /O 2 , NF 3 , Cl 2 , CH 4 /Ar, etc., and these reacting gases can generate a large number of active free radicals such as Cl and F and react with the alloy elements of the aluminum alloy to produce metal compound particles, which may easily cause metal contamination on the surface of the reaction chamber and severely affect the electrical performance of the device.
  • the metal compound particles in the reaction chamber are difficult to clean, and long-term accumulation may cause the entire reaction chamber to fail.
  • the base material of the reaction chamber component is usually made of 6000-series aluminum alloy such as A6061, and a layer of aluminum oxide film is formed on the surface of the component by the sulfuric acid anodic method, to prevent the reaction chamber component from being corroded by plasma.
  • the reaction chamber components can still be easily corroded in the environment of plasma bombardment, which not only reduces the lifespan of the reaction chamber, but also causes metal contamination to the chamber.
  • the present disclosure aims to solve at least one of the technical problems existing in the existing technology, and proposes a reaction chamber component, a preparation method, and a reaction chamber, which can improve the corrosion resistance of the reaction chamber component, thereby improving the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber component.
  • a reaction chamber component including: a body, and an oxide film layer disposed on a surface-to-be-covered of the body.
  • the body is made of a 5000-series aluminum alloy material.
  • the reaction chamber component further includes a ceramic layer covering a surface of the oxide film layer away from the surface-to-be-covered of the body.
  • the surface of the oxide film layer away from the surface-to-be-covered of the body has a predetermined roughness for improving adhesion between the ceramic layer and the oxide film layer.
  • the predetermined roughness has a value range of 3.2 ⁇ m to 6.3 ⁇ m.
  • the ceramic layer includes yttrium oxide or zirconium oxide.
  • a thickness of the ceramic layer ranges from 50 ⁇ m to 200 ⁇ m.
  • the oxide film layer is made by oxidizing the surface-to-be-covered of the body.
  • a thickness of the oxide film layer ranges from 50 ⁇ m to 60 ⁇ m.
  • the present disclosure also provides a reaction chamber including the above-mentioned reaction chamber components provided by the present disclosure.
  • the present disclosure also provides a method for preparing a reaction chamber component, including: producing the body with 5000-series aluminum alloy material; and covering the surface-to-be-covered of the body with an oxide film layer.
  • an oxidation treatment may be performed on the surface-to-be-covered of the body of the to form the oxide film layer.
  • performing oxidation treatment on the surface-to-be-covered of the body to form the oxide film layer includes: preheating the body; and placing the body in an electroplating tank containing nitric acid and oxalic acid for anodizing treatment to form the oxide film layer.
  • a ratio of a mass percentage of nitric acid to a mass percentage of oxalic acid ranges from 0.8 to 1.2.
  • the ratio can be 1.
  • the method further includes: performing a sealing process to the oxide film layer.
  • the method further includes: covering the surface of the oxide film layer away from the surface-to-be-covered of the body with a ceramic layer.
  • the method further includes: performing a roughening process to the surface of the oxide film layer away from the surface-to-be-covered of the body to cause the surface to have the predetermined roughness that can improve the adhesion between the ceramic layer and the oxide film layer.
  • performing a roughening process to the surface of the oxide film layer away from the surface-to-be-covered of the body to cause the surface to have the predetermined roughness that can improve the adhesion between the ceramic layer and the oxide film layer includes: sandblasting the surface of the oxide film layer away from the surface-to-be-covered of the body; and cleaning the surface of the oxide film layer away from the surface-to-be-covered of the body.
  • covering the ceramic layer on the surface of the oxide film layer away from the surface-to-be-covered of the body includes: preheating the oxide film layer; selecting ceramic powder with a preset purity and a preset particle size, and spraying the ceramic powder on the surface of the oxide film layer away from the surface-to-be-covered of the body to form the ceramic layer; and annealing the ceramic layer.
  • the preset purity may be greater than 99.99%, and the value range of the preset particle size may be 5-10 ⁇ m.
  • the present disclosure overcomes the technical prejudice in the existing technology that only considers the need for higher strength of the reaction chamber component and uses the 6000-series aluminum alloys.
  • the 5000-series aluminum alloy is used to produce the body of the reaction chamber component. Since the 5000-series aluminum alloy is work-hardening Al—Mg aluminum alloy such as A5052, which contains very little Si element, it is not prone to grain boundary corrosion. Accordingly, the corrosion resistance of the reaction chamber component can be improved, thereby increasing the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber.
  • FIG. 1 is a schematic structural diagram of an exemplary reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 2 is a flow chart of an exemplary method for preparing a reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 3 is another flow chart of an exemplary method for preparing a reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 4 illustrates another exemplary method for preparing a reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 5 illustrates another exemplary reaction chamber component according to an embodiment of the present disclosure.
  • the reaction chamber component may include, but is not limited to: an inner wall of the reaction chamber, a lining disposed on the inner wall, an adjustment bracket, and an electrostatic chuck.
  • FIG. 1 is a schematic structural diagram of a reaction chamber component.
  • an embodiment of the present disclosure provides a reaction chamber component, including: a body 1 , and an oxide film layer 11 of a surface of body 1 .
  • the surface-to-be-covered of the body can be an entire outer surface-to-be-covered of the body 1 , or it can also selectively cover a part of the outer surface-to-be-covered of the body 1 .
  • the surface-to-be-covered of the body can be the surface-to-be-covered of the body 1 exposed in the reaction chamber.
  • the body 1 can be made of 5000 series aluminum alloy material.
  • the 6000-series aluminum alloy is used to manufacture the body.
  • the 6000-series aluminum alloy is a heat-treatable and strengthened Al—Mg—Si aluminum alloy (e.g., A6061).
  • the aluminum alloy adds more Si elements to form a Mg 2 Si reinforcing phase, thereby increasing the strength of the substrate.
  • the excessive Si element can cause grain boundary corrosion, which affects the corrosion resistance of the reaction chamber components.
  • the technical bias in the existing technology that only considers the need for higher strength of the reaction chamber components and uses the 6000-series aluminum alloys can be overcome.
  • the 5000-series aluminum alloys are used to produce the body 1 . Because the 5000-series aluminum alloys are work-hardened Al—Mg aluminum alloy (e.g., A5052, A5054, A5083, etc.) and contain very little Si element, they are not prone to grain boundary corrosion. Accordingly, the corrosion resistance of the reaction chamber component can be improved, thereby improving the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber component.
  • the oxide film layer 11 is made by oxidizing the surface-to-be-covered of the body 1 .
  • the oxide film layer 11 has high roughness, and good corrosion resistance and wear resistance.
  • a thickness of the oxide film layer 11 ranges from 50 ⁇ m to 60 ⁇ m.
  • the reaction chamber component further includes a ceramic layer 12 covering a surface of the oxide film layer 11 away from the surface-to-be-covered of the body.
  • the ceramic layer 12 can be used as a barrier layer to prevent corrosion by plasma, so that the corrosion resistance of the reaction chamber components can be further improved.
  • the surface of the oxide film layer 11 away from the surface-to-be-covered of the body has a predetermined roughness for improving adhesion between the ceramic layer 12 and the oxide film layer 11 .
  • the predetermined roughness ranges from 3.2 ⁇ m to 6.3 ⁇ m, and within this range, the oxide film layer 11 and the ceramic layer 12 have strong adhesion.
  • predetermined roughness can be obtained by, but not limited to, plasma sandblasting.
  • the above-mentioned ceramic layer 12 can be obtained by the following method: first, preheating the body 1 until the temperature of the body 1 reaches 100° C. ⁇ 120° C.; then, selecting ceramic powder with a purity greater than 99.99% and a particle size range of 5 ⁇ m ⁇ 10 ⁇ m, and spraying the ceramic powder on the surface of the oxide film layer 11 away from the surface-to-be-covered of the body to form the above-mentioned ceramic layer 12 ; after that, annealing the ceramic layer 12 , preferably, but not limited to, annealing at a temperature of 100° C. to 120° C. for 2 to 5 hours.
  • the ceramic layer 12 formed by this method can not only have higher purity and density, but also have a smaller porosity, which can better prevent the corrosion by plasma.
  • the ceramic layer 12 includes but is not limited to: yttrium oxide or zirconium oxide. Since both yttrium oxide and zirconium oxide have better plasma corrosion resistance and longer lifespan than aluminum oxide, Compared with the barrier layer in the existing technology where only aluminum oxide is used as the barrier layer, the use of two barrier layers of the oxide film layer 11 and the ceramic layer 12 can greatly improve the corrosion resistance and lifespan of the reaction chamber component.
  • the thickness of the ceramic layer 12 ranges from 50 ⁇ m to 200 ⁇ m, which can well meet the requirements of corrosion resistance.
  • reaction chamber which includes the reaction chamber component provided in the foregoing embodiment of the present disclosure.
  • the reaction chamber includes, but is not limited to: a physical vapor deposition chamber, a chemical vapor deposition chamber, an etching chamber.
  • the reaction chamber provided by the embodiment of the present disclosure can improve the corrosion resistance of the reaction chamber by using the reaction chamber component provided in the above embodiment, thereby increasing the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber component.
  • a method for preparing the reaction chamber component includes the following:
  • reaction chamber component can improve the corrosion resistance of the reaction chamber component, thereby increasing the lifespan of the reaction chamber and reducing metal contamination on the surface of the reaction chamber component.
  • the surface-to-be-covered of the body 1 may be oxidized to form an oxide film layer 11 .
  • the oxide film layer 11 may have high strength, and good corrosion resistance and wear resistance.
  • the thickness of the oxide film layer ranges from 50 ⁇ m to 60 ⁇ m.
  • the foregoing S 2 includes:
  • the component body 1 can be placed in warm water of 30° C. to 40° C. for preheating.
  • a stirring method can be used to keep the solution in the electroplating tank at a uniform temperature, and the temperature can be set according to the actual processing temperature.
  • the oxide film layer 11 can be formed by applying the mixed acid anodic oxidation method.
  • the 6000-series aluminum alloy contains more Si material.
  • silicon remains in the film as elemental particles, and may not be oxidized or dissolved.
  • the mixed acid-based anodic oxidation requires high voltage.
  • the silicon remained in the film can easily cause larger porosity of the oxide film, and when the film is thick, cracks are likely to form.
  • the body 1 is made of the 5000-series aluminum alloy material, and the oxide film layer 11 is formed by the mixed acid anodic oxidation method, it can not only meet the requirements of strength, but also meet the requirements for the density of the oxide film layer 11 .
  • the above step S 22 is to use the mixed acid anodic oxidation method to form the oxide film layer 11 , which can not only reduce the porosity of the oxide film layer 11 , but also obtain the oxide film layer 11 with better temperature resistance to avoid the occurrence of cracks at high temperatures (e.g., 80° C. ⁇ 120° C.), to be more suitable to meet the requirements of etching equipment above 14 nm.
  • high temperatures e.g. 80° C. ⁇ 120° C.
  • other oxidation methods can also be used to form the oxide film layer 11 .
  • a ratio of mass percentage of nitric acid to mass percentage of oxalic acid ranges from 0.8 to 1.2. More preferably, the ratio can be 1, which can further reduce the porosity of the oxide film layer 11 .
  • the method further includes the following: performing a sealing process to the oxide film layer 11 .
  • the sealing process can adopt methods such as pressurized (for example, 110 kPa) steam sealing or boiling water sealing.
  • mixed acids for example, nitric acid and chromic acid, nitric acid and phosphoric acid, etc.
  • the method further includes:
  • the ceramic layer 12 can be used as a barrier layer to prevent the corrosion by plasma, so that the corrosion resistance of the reaction chamber component can be further improved.
  • a thickness of the ceramic layer 12 ranges from 50 ⁇ m to 200 ⁇ m, and this range can well meet the corrosion resistance requirements.
  • step S 2 and before step S 3 the method further includes:
  • step S 23 the surface of the oxide film layer 11 away from the surface-to-be-covered of the body may be roughened, so that the surface can have a predetermined roughness for improving adhesion between the ceramic layer 12 and the oxide film layer 11 .
  • the value range of the aforementioned predetermined roughness may be 3.2 ⁇ m to 6.3 ⁇ m, and within this range, the adhesion between the oxide film layer 11 and the ceramic layer 12 can be strong.
  • step S 23 includes:
  • the method of sandblasting can be, but not limited to, the method of plasma sandblasting.
  • step S 3 includes:
  • the body 1 may be preheated until the temperature of the body 1 reaches 100° C. to 120° C.
  • the preset purity can be greater than 99.99%, and the value range of the preset particle size can be 5 ⁇ m-10 ⁇ m.
  • step S 33 it is preferable but not limited to annealing at a temperature of 100° C. to 120° C. for 2 to 5 hours.
  • the ceramic layer 12 formed by this method can not only have a higher purity and density, but also have a smaller porosity, which can better prevent the corrosion by plasma.
  • the ceramic layer 12 includes yttrium oxide or zirconium oxide. Since both yttrium oxide and zirconium oxide have better plasma corrosion resistance and longer lifespan than aluminum oxide, compared with the existing technology where only aluminum oxide is used as the barrier layer, the use of the two barrier layers of oxide film layer 11 and ceramic layer 12 can largely improve the corrosion resistance and lifespan of the reaction chamber component.
  • FIG. 4 illustrates an exemplary method of preparing the reaction chamber component
  • FIG. 5 illustrate a structure of the reaction chamber component correspondingly.
  • an aluminum alloy material is selected and is used for a substrate, e.g., substrate 502 of FIG. 5 , for preparing a reaction chamber component.
  • the substrate 502 may be the same as or similar to the body 1 as illustrated in FIG. 1 .
  • the substrate 502 may be aluminum alloy with minimum amount of silicon (Si), e.g., less than 0.25% by weight, or with zero amount of silicon.
  • the aluminum alloy may be an AlMg alloy with minimum amount of silicon (Si), e.g., less than 0.25% by weight, or with zero amount of silicon.
  • the silicon may not be oxidized or dissolved during a subsequent anodic oxidation process.
  • the silicon remained in the substrate can easily cause larger porosity of the formed oxide film, forming cracks as the film gets thick.
  • the oxide film layer 504 may be formed with reduced porosity, high strength, high density, and desirable corrosion resistance and wear resistance.
  • the prepared reaction chamber component can thus have improved properties, thereby increasing the lifespan of the reaction chamber and reducing metal contamination on the surface of the reaction chamber component.
  • the substrate 502 may be pre-treated, preparing the surface for forming an oxide film layer thereon.
  • the substrate 502 may be preheated, for example, by being placed in warm water, e.g., of 30° C. to 40° C. for preheating.
  • an oxide film layer 504 may be formed on the substrate 502 .
  • the surface of the substrate 502 may undergo an anodizing treatment, for example, using mixed-acids. At least two acids may be selected, with respect to the selected aluminum material of the substrate 502 for forming the oxide file layer 504 .
  • the mixed-acids may at least include nitric acid.
  • the mixed-acids include nitric acid and oxalic acid.
  • the mixed-acids may be mixed in an electroplating solution.
  • the substrate 502 may be placed in the electroplating solution containing the mixed-acids for an anodic oxidation reaction to form the oxide film layer 504 from the surface portion of the substrate 502 .
  • the thickness of the disclosed oxide film layer may range from 50 ⁇ m to 60 ⁇ m.
  • a ratio of mass percentage of nitric acid to mass percentage of oxalic acid may range from 0.8 to 1.2.
  • the mass ratio between the nitric acid and the oxalic acid can be, for example, about 1, providing reduced porosity of the formed oxide film layer 504 .
  • the growth process of the oxide film layer includes chemical dissolution process and electrochemical formation process of the oxide film. As the formation speed of the oxide film layer is greater than the dissolution speed, a certain degree of oxidation can be obtained.
  • Table 1 lists features of various oxide film layers made from different mixed-acids on an AlMg alloy based substrate.
  • the formed oxide film layers provide significantly different features.
  • the use of mixed nitric acid and oxalic acid provides the formed oxide film layer (e.g., layer 504 ) with unexpected results as shown in Table 1.
  • the disclosed oxide film layer 504 formed by use of mixed nitric acid and oxalic acid, had a temperature resistance to avoid the occurrence of cracks at high temperatures of 150° C. to 200° C., more suitable to meet the requirements of etching equipment above 14 nm, while under the same condition, the oxide film layer, formed by use of mixed sulfuric acid with different other acids in Table 1, had a temperature resistance of 100° C. to 150° C.
  • the formed oxide film layer 504 may include various pore structures including, such as columnar pore structures or honeycomb columnar pores.
  • a sealing process may be performed to the oxide film layer 504 to seal the pore structures formed in the oxide film layer 504 with hydrated alumina 507 .
  • the sealing process can adopt methods, such as pressurized (for example, at a pressure of about 110 kPa) steam sealing or boiling water sealing.
  • a sandblasting process may be performed on the oxide film layer 504 .
  • the sandblasting process may be a plasma sandblasting process.
  • a cleaning process can be performed on the sealed oxide film layer 504 .
  • the surface of the oxide film layer 504 may be roughened, so that the surface can have a predetermined roughness for receiving additional layers (e.g., a ceramic layer) with improved adhesion there-between.
  • additional layers e.g., a ceramic layer
  • the sealing process can allow hydrated alumina 507 to fill the columnar pores, which improves at least the corrosion resistance of the resultant oxide film layer 504 and also avoid adsorption of impurities or oil stains into the columnar pores.
  • the sandblasting process can allow the sealed oxide film layer to have desirable surface roughness to significantly smooth the large, uneven roughness of the oxide film generated due to anodization.
  • the formed oxide film layer 504 may have a predetermined roughness controlled to be between 3.2 ⁇ m to 6.3 ⁇ m, providing strong adhesion between the oxide film layer 504 and the ceramic layer to be formed thereon.
  • the ceramic layer (not shown in FIG. 5 ) is formed to cover the surface of the oxide film layer 504 .
  • the ceramic layer may be same as or similar to the ceramic layer 12 as disclosed herein.
  • the oxide film layer 504 before forming the ceramic layer, can be preheated, e.g., until a temperature of 100° C. to 120° C. is reached.
  • the ceramic layer can be formed by selecting ceramic powder with a preset purity (e.g., greater than 99.99%) and a preset particle size (e.g., about 5 ⁇ m-10 ⁇ m), spraying the ceramic powder to the surface of the oxide film layer 504 , and annealing the spray-coated ceramic powder (e.g., at a temperature of 100° C. to 120° C. for 2 to 5 hours) to form the ceramic layer.
  • a preset purity e.g., greater than 99.99%
  • a preset particle size e.g., about 5 ⁇ m-10 ⁇ m
  • the ceramic layer can be used as a barrier layer to prevent corrosion by plasma, so that the corrosion resistance of the reaction chamber component can be further improved.
  • a thickness of the ceramic layer ranges from 50 ⁇ m to 200 ⁇ m, and this range can well meet the corrosion resistance requirements.
  • the ceramic layer formed by this method can not only have a higher purity and density, but also have a smaller porosity, which can better prevent the corrosion by plasma.
  • the ceramic layer includes yttrium oxide or zirconium oxide. Since both yttrium oxide and zirconium oxide have better plasma corrosion resistance and longer lifespan than aluminum oxide, compared with the existing technology where only aluminum oxide is used as the barrier layer, the use of the two barrier layers of oxide film layer 504 and ceramic layer can largely improve the corrosion resistance and lifespan of the reaction chamber component.

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Abstract

A method for preparing reaction chamber component includes providing a substrate; forming an oxide film layer from a surface of the substrate by performing an anodizing treatment with mixed-acids; performing a sealing process to the oxide film layer to seal pores formed in the oxide film layer; performing a sandblasting process to the oxide film layer to provide the oxide film layer with a predetermined roughness for receiving a ceramic layer; and forming the ceramic layer on the oxide film layer.

Description

    CROSS-REFERENCE TO RELATED APPLICATIONS
  • This application is a continuation-in-part application of Ser. No. 16/976,703, filed on Aug. 28, 2020, which is National Stage entry under 35 U.S.C. § 371 of International Application No. PCT/CN2018/118897, filed on Dec. 3, 2018, which claims priority to the Chinese Applications No. 201810190001.5 and No. 201820317132.0, both filed on Mar. 8, 2018, the entire contents of all of which are incorporated herein by reference.
  • TECHNICAL FIELD
  • The disclosure belongs to the technical field of microelectronics processing, and in particular relates to a reaction chamber component, a preparation method, and a reaction chamber.
  • BACKGROUND TECHNOLOGY
  • In the semiconductor manufacturing process, aluminum alloy is widely used to manufacture the reaction chamber component for the production of plasma. This is because not only the aluminum alloy has high strength and good weldability, but also the anode oxide film of aluminum alloy has good corrosion resistance. However, the aluminum alloy contains a large number of alloy elements, such as Mg, Cu, Zn, Mn, Fe, Si, etc. In the plasma etching process, the reacting gases used in the reaction chamber include CF4/O2, NF3, Cl2, CH4/Ar, etc., and these reacting gases can generate a large number of active free radicals such as Cl and F and react with the alloy elements of the aluminum alloy to produce metal compound particles, which may easily cause metal contamination on the surface of the reaction chamber and severely affect the electrical performance of the device. In addition, the metal compound particles in the reaction chamber are difficult to clean, and long-term accumulation may cause the entire reaction chamber to fail.
  • At present, the base material of the reaction chamber component is usually made of 6000-series aluminum alloy such as A6061, and a layer of aluminum oxide film is formed on the surface of the component by the sulfuric acid anodic method, to prevent the reaction chamber component from being corroded by plasma. However, in practical applications, the reaction chamber components can still be easily corroded in the environment of plasma bombardment, which not only reduces the lifespan of the reaction chamber, but also causes metal contamination to the chamber.
  • SUMMARY OF THE DISCLOSURE
  • The present disclosure aims to solve at least one of the technical problems existing in the existing technology, and proposes a reaction chamber component, a preparation method, and a reaction chamber, which can improve the corrosion resistance of the reaction chamber component, thereby improving the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber component.
  • In order to solve one of the above problems, the present disclosure provides a reaction chamber component, including: a body, and an oxide film layer disposed on a surface-to-be-covered of the body. The body is made of a 5000-series aluminum alloy material.
  • In some embodiments, the reaction chamber component further includes a ceramic layer covering a surface of the oxide film layer away from the surface-to-be-covered of the body.
  • In some embodiments, the surface of the oxide film layer away from the surface-to-be-covered of the body has a predetermined roughness for improving adhesion between the ceramic layer and the oxide film layer.
  • In some embodiments, the predetermined roughness has a value range of 3.2 μm to 6.3 μm.
  • In some embodiments, the ceramic layer includes yttrium oxide or zirconium oxide.
  • In some embodiments, a thickness of the ceramic layer ranges from 50 μm to 200 μm.
  • In some embodiments, the oxide film layer is made by oxidizing the surface-to-be-covered of the body.
  • In some embodiments, a thickness of the oxide film layer ranges from 50 μm to 60 μm.
  • As another technical solution, the present disclosure also provides a reaction chamber including the above-mentioned reaction chamber components provided by the present disclosure.
  • As another technical solution, the present disclosure also provides a method for preparing a reaction chamber component, including: producing the body with 5000-series aluminum alloy material; and covering the surface-to-be-covered of the body with an oxide film layer.
  • In some embodiments, during the process of covering the surface-to-be-covered of the body with the oxide film layer, an oxidation treatment may be performed on the surface-to-be-covered of the body of the to form the oxide film layer.
  • In some embodiments, performing oxidation treatment on the surface-to-be-covered of the body to form the oxide film layer includes: preheating the body; and placing the body in an electroplating tank containing nitric acid and oxalic acid for anodizing treatment to form the oxide film layer.
  • In some embodiments, a ratio of a mass percentage of nitric acid to a mass percentage of oxalic acid ranges from 0.8 to 1.2.
  • In some embodiments, the ratio can be 1.
  • In some embodiments, after the step of covering the surface-to-be-covered of the body with the oxide film layer, the method further includes: performing a sealing process to the oxide film layer.
  • In some embodiments, after forming the oxide film layer on the surface-to-be-covered of the body, the method further includes: covering the surface of the oxide film layer away from the surface-to-be-covered of the body with a ceramic layer.
  • In some embodiments, after forming the oxide film layer on the surface-to-be-covered of the body but before covering the surface of the oxide film layer away from the surface-to-be-covered of the body with the ceramic layer, the method further includes: performing a roughening process to the surface of the oxide film layer away from the surface-to-be-covered of the body to cause the surface to have the predetermined roughness that can improve the adhesion between the ceramic layer and the oxide film layer.
  • In some embodiments, performing a roughening process to the surface of the oxide film layer away from the surface-to-be-covered of the body to cause the surface to have the predetermined roughness that can improve the adhesion between the ceramic layer and the oxide film layer includes: sandblasting the surface of the oxide film layer away from the surface-to-be-covered of the body; and cleaning the surface of the oxide film layer away from the surface-to-be-covered of the body.
  • In some embodiments, covering the ceramic layer on the surface of the oxide film layer away from the surface-to-be-covered of the body includes: preheating the oxide film layer; selecting ceramic powder with a preset purity and a preset particle size, and spraying the ceramic powder on the surface of the oxide film layer away from the surface-to-be-covered of the body to form the ceramic layer; and annealing the ceramic layer.
  • In some embodiments, the preset purity may be greater than 99.99%, and the value range of the preset particle size may be 5-10 μm.
  • The present disclosure has the following beneficial effects:
  • The present disclosure overcomes the technical prejudice in the existing technology that only considers the need for higher strength of the reaction chamber component and uses the 6000-series aluminum alloys. In the present disclosure, the 5000-series aluminum alloy is used to produce the body of the reaction chamber component. Since the 5000-series aluminum alloy is work-hardening Al—Mg aluminum alloy such as A5052, which contains very little Si element, it is not prone to grain boundary corrosion. Accordingly, the corrosion resistance of the reaction chamber component can be improved, thereby increasing the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber.
  • BRIEF DESCRIPTION OF THE DRAWINGS
  • FIG. 1 is a schematic structural diagram of an exemplary reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 2 is a flow chart of an exemplary method for preparing a reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 3 is another flow chart of an exemplary method for preparing a reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 4 illustrates another exemplary method for preparing a reaction chamber component according to an embodiment of the present disclosure.
  • FIG. 5 illustrates another exemplary reaction chamber component according to an embodiment of the present disclosure.
  • DETAILED DESCRIPTION OF THE EMBODIMENTS
  • In order to enable those skilled in the art to better understand the technical solutions of the present disclosure, the reaction chamber component, the preparation method, and the reaction chamber provided by the present disclosure will be described in detail below with reference to the accompanying drawings.
  • In this specification, the reaction chamber component may include, but is not limited to: an inner wall of the reaction chamber, a lining disposed on the inner wall, an adjustment bracket, and an electrostatic chuck.
  • FIG. 1 is a schematic structural diagram of a reaction chamber component. As shown in FIG. 1 , an embodiment of the present disclosure provides a reaction chamber component, including: a body 1, and an oxide film layer 11 of a surface of body 1. The surface-to-be-covered of the body can be an entire outer surface-to-be-covered of the body 1, or it can also selectively cover a part of the outer surface-to-be-covered of the body 1. For example, the surface-to-be-covered of the body can be the surface-to-be-covered of the body 1 exposed in the reaction chamber.
  • The body 1 can be made of 5000 series aluminum alloy material.
  • Often, the 6000-series aluminum alloy is used to manufacture the body. The 6000-series aluminum alloy is a heat-treatable and strengthened Al—Mg—Si aluminum alloy (e.g., A6061). The aluminum alloy adds more Si elements to form a Mg2Si reinforcing phase, thereby increasing the strength of the substrate. However, the excessive Si element can cause grain boundary corrosion, which affects the corrosion resistance of the reaction chamber components.
  • In this embodiment, the technical bias in the existing technology that only considers the need for higher strength of the reaction chamber components and uses the 6000-series aluminum alloys can be overcome. The 5000-series aluminum alloys are used to produce the body 1. Because the 5000-series aluminum alloys are work-hardened Al—Mg aluminum alloy (e.g., A5052, A5054, A5083, etc.) and contain very little Si element, they are not prone to grain boundary corrosion. Accordingly, the corrosion resistance of the reaction chamber component can be improved, thereby improving the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber component.
  • In this embodiment, the oxide film layer 11 is made by oxidizing the surface-to-be-covered of the body 1. The oxide film layer 11 has high roughness, and good corrosion resistance and wear resistance. In some embodiments, a thickness of the oxide film layer 11 ranges from 50 μm to 60 μm.
  • In this embodiment, the reaction chamber component further includes a ceramic layer 12 covering a surface of the oxide film layer 11 away from the surface-to-be-covered of the body. The ceramic layer 12 can be used as a barrier layer to prevent corrosion by plasma, so that the corrosion resistance of the reaction chamber components can be further improved.
  • In some embodiments, the surface of the oxide film layer 11 away from the surface-to-be-covered of the body has a predetermined roughness for improving adhesion between the ceramic layer 12 and the oxide film layer 11. Preferably, the predetermined roughness ranges from 3.2 μm to 6.3 μm, and within this range, the oxide film layer 11 and the ceramic layer 12 have strong adhesion.
  • It should be noted here that the above-mentioned predetermined roughness can be obtained by, but not limited to, plasma sandblasting.
  • In some embodiment, the above-mentioned ceramic layer 12 can be obtained by the following method: first, preheating the body 1 until the temperature of the body 1 reaches 100° C.˜120° C.; then, selecting ceramic powder with a purity greater than 99.99% and a particle size range of 5 μm˜10 μm, and spraying the ceramic powder on the surface of the oxide film layer 11 away from the surface-to-be-covered of the body to form the above-mentioned ceramic layer 12; after that, annealing the ceramic layer 12, preferably, but not limited to, annealing at a temperature of 100° C. to 120° C. for 2 to 5 hours. The ceramic layer 12 formed by this method can not only have higher purity and density, but also have a smaller porosity, which can better prevent the corrosion by plasma.
  • In some embodiments, the ceramic layer 12 includes but is not limited to: yttrium oxide or zirconium oxide. Since both yttrium oxide and zirconium oxide have better plasma corrosion resistance and longer lifespan than aluminum oxide, Compared with the barrier layer in the existing technology where only aluminum oxide is used as the barrier layer, the use of two barrier layers of the oxide film layer 11 and the ceramic layer 12 can greatly improve the corrosion resistance and lifespan of the reaction chamber component.
  • In addition, the thickness of the ceramic layer 12 ranges from 50 μm to 200 μm, which can well meet the requirements of corrosion resistance.
  • According to an embodiment of the present disclosure, there is further provided a reaction chamber, which includes the reaction chamber component provided in the foregoing embodiment of the present disclosure.
  • Specifically, the reaction chamber includes, but is not limited to: a physical vapor deposition chamber, a chemical vapor deposition chamber, an etching chamber.
  • The reaction chamber provided by the embodiment of the present disclosure can improve the corrosion resistance of the reaction chamber by using the reaction chamber component provided in the above embodiment, thereby increasing the lifespan of the reaction chamber and reducing the metal contamination on the surface of the reaction chamber component.
  • Referring to FIGS. 1 and 2 , a method for preparing the reaction chamber component provided by the embodiment of the present disclosure includes the following:
      • S1: Producing a body 1 by using a 5000-series aluminum alloy material; and
      • S2: Covering a surface-to-be-covered of the body 1 with an oxide film layer 11.
  • Using the above preparation method provided in the embodiments of the present disclosure to prepare the reaction chamber component can improve the corrosion resistance of the reaction chamber component, thereby increasing the lifespan of the reaction chamber and reducing metal contamination on the surface of the reaction chamber component.
  • In the above step S2, the surface-to-be-covered of the body 1 may be oxidized to form an oxide film layer 11. The oxide film layer 11 may have high strength, and good corrosion resistance and wear resistance. In some embodiments, the thickness of the oxide film layer ranges from 50 μm to 60 μm.
  • In some embodiments, the foregoing S2, includes:
      • S21: Preheating the body 1; and
      • S22: Placing the body 1 in an electroplating tank containing nitric acid and oxalic acid to perform anodizing treatment to form the oxide film layer 11.
  • In the above step S21, preferably, the component body 1 can be placed in warm water of 30° C. to 40° C. for preheating. Specifically, a stirring method can be used to keep the solution in the electroplating tank at a uniform temperature, and the temperature can be set according to the actual processing temperature.
  • In the above step S22, the oxide film layer 11 can be formed by applying the mixed acid anodic oxidation method. Often, the 6000-series aluminum alloy contains more Si material. During the anodic oxidation process, silicon remains in the film as elemental particles, and may not be oxidized or dissolved. The mixed acid-based anodic oxidation requires high voltage. The silicon remained in the film can easily cause larger porosity of the oxide film, and when the film is thick, cracks are likely to form. In this embodiment, since the body 1 is made of the 5000-series aluminum alloy material, and the oxide film layer 11 is formed by the mixed acid anodic oxidation method, it can not only meet the requirements of strength, but also meet the requirements for the density of the oxide film layer 11.
  • Therefore, based on the method to produce the body 1 by using the 5000-series aluminum alloy material, the above step S22 is to use the mixed acid anodic oxidation method to form the oxide film layer 11, which can not only reduce the porosity of the oxide film layer 11, but also obtain the oxide film layer 11 with better temperature resistance to avoid the occurrence of cracks at high temperatures (e.g., 80° C.˜120° C.), to be more suitable to meet the requirements of etching equipment above 14 nm. Of course, in practical applications, other oxidation methods can also be used to form the oxide film layer 11.
  • Preferably, a ratio of mass percentage of nitric acid to mass percentage of oxalic acid ranges from 0.8 to 1.2. More preferably, the ratio can be 1, which can further reduce the porosity of the oxide film layer 11.
  • In some embodiments, after the above step S2, the method further includes the following: performing a sealing process to the oxide film layer 11. Specifically, the sealing process can adopt methods such as pressurized (for example, 110 kPa) steam sealing or boiling water sealing.
  • In practical applications, other mixed acids can also be used, for example, nitric acid and chromic acid, nitric acid and phosphoric acid, etc.
  • Referring to FIG. 3 , preferably, after the above step S2, the method further includes:
      • S3: covering a surface of the oxide film layer 11 away from the surface-to-be-covered of the body with a ceramic layer 12.
  • The ceramic layer 12 can be used as a barrier layer to prevent the corrosion by plasma, so that the corrosion resistance of the reaction chamber component can be further improved.
  • In some embodiments, a thickness of the ceramic layer 12 ranges from 50 μm to 200 μm, and this range can well meet the corrosion resistance requirements.
  • In some embodiments, after step S2 and before step S3, the method further includes:
  • In step S23, the surface of the oxide film layer 11 away from the surface-to-be-covered of the body may be roughened, so that the surface can have a predetermined roughness for improving adhesion between the ceramic layer 12 and the oxide film layer 11.
  • Further, the value range of the aforementioned predetermined roughness may be 3.2 μm to 6.3 μm, and within this range, the adhesion between the oxide film layer 11 and the ceramic layer 12 can be strong.
  • In addition, preferably, the above step S23 includes:
      • S231: Sandblasting the surface of the oxide film layer 11 away from the surface-to-be-covered of the body; and
      • S232: Cleaning the surface of the oxide film layer 11 away from the surface-to-be-covered of the body.
  • In the above step S231, the method of sandblasting can be, but not limited to, the method of plasma sandblasting.
  • In this embodiment, the above step S3 includes:
      • S31: Preheating the oxide film layer 11;
      • S32: Selecting ceramic powder with a preset purity and a preset particle size, and spraying the ceramic powder to the surface of the oxide film layer 11 away from the surface-to-be-covered of the body to form the ceramic layer 12; and
      • S33: Annealing the ceramic layer.
  • In the above step S31, the body 1 may be preheated until the temperature of the body 1 reaches 100° C. to 120° C.
  • In the above step S32, in some embodiments, the preset purity can be greater than 99.99%, and the value range of the preset particle size can be 5 μm-10 μm.
  • In the above step S33, it is preferable but not limited to annealing at a temperature of 100° C. to 120° C. for 2 to 5 hours.
  • The ceramic layer 12 formed by this method can not only have a higher purity and density, but also have a smaller porosity, which can better prevent the corrosion by plasma.
  • In some embodiments, the ceramic layer 12 includes yttrium oxide or zirconium oxide. Since both yttrium oxide and zirconium oxide have better plasma corrosion resistance and longer lifespan than aluminum oxide, compared with the existing technology where only aluminum oxide is used as the barrier layer, the use of the two barrier layers of oxide film layer 11 and ceramic layer 12 can largely improve the corrosion resistance and lifespan of the reaction chamber component.
  • Various embodiments further provide additional exemplary reaction chamber component and exemplary method of preparing a reaction chamber component. For example, FIG. 4 illustrates an exemplary method of preparing the reaction chamber component, and FIG. 5 illustrate a structure of the reaction chamber component correspondingly.
  • Referring to FIG. 4 , at 410, an aluminum alloy material is selected and is used for a substrate, e.g., substrate 502 of FIG. 5 , for preparing a reaction chamber component. In one embodiment, the substrate 502 may be the same as or similar to the body 1 as illustrated in FIG. 1 . In another embodiment, the substrate 502 may be aluminum alloy with minimum amount of silicon (Si), e.g., less than 0.25% by weight, or with zero amount of silicon. In another embodiment, the aluminum alloy may be an AlMg alloy with minimum amount of silicon (Si), e.g., less than 0.25% by weight, or with zero amount of silicon.
  • When the surface of the substrate includes silicon elemental particles, the silicon may not be oxidized or dissolved during a subsequent anodic oxidation process. The silicon remained in the substrate can easily cause larger porosity of the formed oxide film, forming cracks as the film gets thick. As such, by using the substrate with minimum amount of silicon, the oxide film layer 504 may be formed with reduced porosity, high strength, high density, and desirable corrosion resistance and wear resistance. The prepared reaction chamber component can thus have improved properties, thereby increasing the lifespan of the reaction chamber and reducing metal contamination on the surface of the reaction chamber component.
  • At 420 of FIG. 4 , the substrate 502 may be pre-treated, preparing the surface for forming an oxide film layer thereon. In one embodiment, the substrate 502 may be preheated, for example, by being placed in warm water, e.g., of 30° C. to 40° C. for preheating.
  • At 430 of FIG. 4 , an oxide film layer 504 may be formed on the substrate 502.
  • In one embodiment, the surface of the substrate 502 may undergo an anodizing treatment, for example, using mixed-acids. At least two acids may be selected, with respect to the selected aluminum material of the substrate 502 for forming the oxide file layer 504.
  • As disclosed herein, the mixed-acids may at least include nitric acid. In one embodiment, the mixed-acids include nitric acid and oxalic acid. The mixed-acids may be mixed in an electroplating solution. The substrate 502 may be placed in the electroplating solution containing the mixed-acids for an anodic oxidation reaction to form the oxide film layer 504 from the surface portion of the substrate 502. The thickness of the disclosed oxide film layer may range from 50 μm to 60 μm. A ratio of mass percentage of nitric acid to mass percentage of oxalic acid may range from 0.8 to 1.2. In one embodiment, the mass ratio between the nitric acid and the oxalic acid can be, for example, about 1, providing reduced porosity of the formed oxide film layer 504. The growth process of the oxide film layer includes chemical dissolution process and electrochemical formation process of the oxide film. As the formation speed of the oxide film layer is greater than the dissolution speed, a certain degree of oxidation can be obtained.
  • The disclosed combination of the mixed-acids, together with the selected substrate material, are critical for forming the disclosed oxide film layer. For example, Table 1 lists features of various oxide film layers made from different mixed-acids on an AlMg alloy based substrate.
  • TABLE 1
    Mixed-acids
    Sulfuric acid + Sulfuric acid + Sulfuric acid + Nitric acid +
    Features Oxalic acid Phosphoric acid Chromic acid Oxalic acid
    Corrosion Resistance high modest modest high
    (5% HCl foaming test
    at room temperature)
    Temperature Resistance high modest high very high
    Pore size low modest low low
    Film thickness high modest low high
  • As shown in Table 1, under same process condition, when an AlMg alloy substrate with minimum amount of silicon is placed in an electroplating solution containing the listed mixed-acids for an anodic oxidation reaction, the formed oxide film layers provide significantly different features. The use of mixed nitric acid and oxalic acid provides the formed oxide film layer (e.g., layer 504) with unexpected results as shown in Table 1.
  • For example, the disclosed oxide film layer 504, formed by use of mixed nitric acid and oxalic acid, had a temperature resistance to avoid the occurrence of cracks at high temperatures of 150° C. to 200° C., more suitable to meet the requirements of etching equipment above 14 nm, while under the same condition, the oxide film layer, formed by use of mixed sulfuric acid with different other acids in Table 1, had a temperature resistance of 100° C. to 150° C.
  • As shown in FIG. 5 , the formed oxide film layer 504 may include various pore structures including, such as columnar pore structures or honeycomb columnar pores.
  • At 440 of FIG. 4 , a sealing process may be performed to the oxide film layer 504 to seal the pore structures formed in the oxide film layer 504 with hydrated alumina 507. The sealing process can adopt methods, such as pressurized (for example, at a pressure of about 110 kPa) steam sealing or boiling water sealing.
  • At 450 of FIG. 4 , a sandblasting process may be performed on the oxide film layer 504. The sandblasting process may be a plasma sandblasting process. In one embodiment, following the sandblasting process, a cleaning process can be performed on the sealed oxide film layer 504.
  • As such, by performing the sealing process and the sandblasting process, the surface of the oxide film layer 504 may be roughened, so that the surface can have a predetermined roughness for receiving additional layers (e.g., a ceramic layer) with improved adhesion there-between. For example, the sealing process can allow hydrated alumina 507 to fill the columnar pores, which improves at least the corrosion resistance of the resultant oxide film layer 504 and also avoid adsorption of impurities or oil stains into the columnar pores. In addition, the sandblasting process can allow the sealed oxide film layer to have desirable surface roughness to significantly smooth the large, uneven roughness of the oxide film generated due to anodization.
  • As disclosed, the formed oxide film layer 504 may have a predetermined roughness controlled to be between 3.2 μm to 6.3 μm, providing strong adhesion between the oxide film layer 504 and the ceramic layer to be formed thereon.
  • At 460 of FIG. 4 , the ceramic layer (not shown in FIG. 5 ) is formed to cover the surface of the oxide film layer 504. In one embodiment, the ceramic layer may be same as or similar to the ceramic layer 12 as disclosed herein.
  • In one embodiment, before forming the ceramic layer, the oxide film layer 504 can be preheated, e.g., until a temperature of 100° C. to 120° C. is reached.
  • The ceramic layer can be formed by selecting ceramic powder with a preset purity (e.g., greater than 99.99%) and a preset particle size (e.g., about 5 μm-10 μm), spraying the ceramic powder to the surface of the oxide film layer 504, and annealing the spray-coated ceramic powder (e.g., at a temperature of 100° C. to 120° C. for 2 to 5 hours) to form the ceramic layer.
  • The ceramic layer can be used as a barrier layer to prevent corrosion by plasma, so that the corrosion resistance of the reaction chamber component can be further improved.
  • In some embodiments, a thickness of the ceramic layer ranges from 50 μm to 200 μm, and this range can well meet the corrosion resistance requirements.
  • The ceramic layer formed by this method can not only have a higher purity and density, but also have a smaller porosity, which can better prevent the corrosion by plasma.
  • In some embodiments, the ceramic layer includes yttrium oxide or zirconium oxide. Since both yttrium oxide and zirconium oxide have better plasma corrosion resistance and longer lifespan than aluminum oxide, compared with the existing technology where only aluminum oxide is used as the barrier layer, the use of the two barrier layers of oxide film layer 504 and ceramic layer can largely improve the corrosion resistance and lifespan of the reaction chamber component.
  • It can be understood that the above implementations are merely exemplary implementations used to illustrate the principle of the present disclosure, but the present disclosure is not limited thereto. For those of ordinary skill in the art, various modifications and improvements can be made without departing from the spirit and essence of the present disclosure, and these modifications and improvements are also regarded as the scope of the disclosure.

Claims (20)

What is claimed is:
1. A method for preparing reaction chamber component, comprising:
providing a substrate;
forming an oxide film layer from a surface of the substrate by performing an anodizing treatment with mixed-acids;
performing a sealing process to the oxide film layer to seal pores formed in the oxide film layer;
performing a sandblasting process to the oxide film layer to provide the oxide film layer with a predetermined roughness for receiving a ceramic layer; and
forming the ceramic layer on the oxide film layer.
2. The method according to claim 1, wherein the substrate includes an aluminum alloy having a silicon content of less than 0.25% by weight.
3. The method according to claim 1, further comprising:
preheating the substrate at a temperature of 30° C. to 40° C. for preparing the surface of the substrate for forming the oxide film layer.
4. The method according to claim 1, wherein the mixed-acids at least include nitric acid.
5. The method according to claim 4, wherein the mixed-acids include nitric acid and oxalic acid, and a ratio of mass percentage of the nitric acid to mass percentage of the oxalic acid ranges from 0.8 to 1.2.
6. The method according to claim 5, wherein the ratio is about 1.
7. The method according to claim 5, wherein forming the oxide film layer comprises:
placing the substrate in an electroplating solution containing the nitric acid and the oxalic acid for the anodizing treatment to form the oxide film layer.
8. The method according to claim 1, wherein a thickness of the oxide film layer ranges from 50 μm to 60 μm.
9. The method according to claim 1, wherein the pores in the oxide film layer include columnar pore structures, wherein the columnar pore structures are filled with hydrated alumina to seal the oxide film layer.
10. The method according to claim 1, wherein the sandblasting process includes a plasma sandblasting process, followed by a cleaning process of the oxide film layer.
11. The method according to claim 1, wherein the predetermined roughness the oxide film layer for receiving the ceramic layer is controlled between 3.2 μm to 6.3 μm by the sandblasting process.
12. The method according to claim 1, wherein the ceramic layer is formed by:
selecting ceramic powder with a preset purity and a preset particle size,
spraying the ceramic powder to a surface of the oxide film layer; and
annealing the ceramic layer.
13. The method according to claim 12, wherein:
the preset purity is greater than 99.99%; and
a value range of the preset particle size is 5 μm-10 μm.
14. The method according to claim 1, wherein the ceramic layer comprises yttrium oxide or zirconium oxide.
15. The method according to claim 1, wherein a thickness of the ceramic layer ranges from 50 μm to 200 μm.
16. A reaction chamber component, comprising:
a substrate;
an oxide film layer on a surface of the substrate, wherein the oxide film layer includes pore structures;
hydrated alumina filled in the pore structures to seal the oxide film layer; and
a ceramic layer on the sealed oxide film layer.
17. The component according to claim 16, wherein the substrate includes an aluminum alloy having a silicon content of less than 0.25% by weight.
18. The component according to claim 16, wherein a thickness of the oxide film layer ranges from 50 μm to 60 μm.
19. The component according to claim 16, wherein the sealed oxide film layer has a predetermined roughness between 3.2 μm to 6.3 μm for receiving the ceramic layer.
20. The component according to claim 16, wherein the ceramic layer comprises yttrium oxide or zirconium oxide.
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PCT/CN2018/118897 WO2019169912A1 (en) 2018-03-08 2018-12-03 Reaction chamber component and preparation method therefor, and reaction chamber
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