WO2015080135A1 - プラズマ装置用部品及びその製造方法 - Google Patents
プラズマ装置用部品及びその製造方法 Download PDFInfo
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- WO2015080135A1 WO2015080135A1 PCT/JP2014/081190 JP2014081190W WO2015080135A1 WO 2015080135 A1 WO2015080135 A1 WO 2015080135A1 JP 2014081190 W JP2014081190 W JP 2014081190W WO 2015080135 A1 WO2015080135 A1 WO 2015080135A1
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- aluminum nitride
- particles
- film
- plasma device
- plasma
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- 239000002245 particle Substances 0.000 claims abstract description 196
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 169
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 4
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
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Images
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- 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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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
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- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
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- H01L21/02312—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment treatment by exposure to a gas or vapour
- H01L21/02315—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment treatment by exposure to a gas or vapour treatment by exposure to a plasma
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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Definitions
- the present invention is excellent in corrosion resistance against halogen-based corrosive gas and plasma, and can be suitably used for a plasma processing apparatus used for semiconductor / liquid crystal production, etc., and a plasma apparatus component coated with an aluminum nitride film and its components It relates to a manufacturing method.
- ceramics such as aluminum oxide, aluminum nitride, yttrium oxide, and YAG are used as components for components exposed to halogen plasma in the above-described processes.
- aluminum nitride having high thermal conductivity and excellent corrosion resistance is preferable in consideration of the balance between performance and cost.
- a conventional ceramic plasma device component for example, there is an electrostatic chuck disclosed in Patent Document 1, in which a metal electrode is embedded in aluminum nitride, and between the wafer and the internal electrode.
- a so-called Johnson Rabeck force that increases the adsorption force of the wafer at a low temperature is generated to attract the wafer.
- sintering is performed by adding a sintering aid to the aluminum nitride raw material powder.
- the sintering mechanism is such that by adding a sintering aid, a reaction product having a low melting point is generated at the grain boundary to form a liquid phase, and mass transfer of aluminum nitride is performed through this liquid phase. Therefore, there are many grain boundary layers between the grains of the sintered body, and when stress is concentrated, destruction proceeds from the grain boundaries, and the particles fall off.
- Patent Document 1 proposes a plasma device component (electrostatic chuck) using aluminum nitride that suppresses the breakage of grain boundaries that are likely to be particles generation sources with controlled sintering aids.
- Patent Document 1 As in Patent Document 1, in a plasma device component (electrostatic chuck) using aluminum nitride as a material, particles caused by grain boundary breakdown are a serious problem. For this reason, the type and amount of the sintering aid have been adjusted, but if the amount of sintering aid is reduced, the sintering becomes incomplete and the volume resistivity, which is an important function of the electrostatic chuck, is increased. It becomes difficult to control.
- titanium nitride is added to suppress the generation of particles, but in recent years, the demand for particle reduction has become stricter, and it is not sufficient to add titanium nitride alone, and it is difficult to reduce the amount of particles generated. It has become.
- the wiring width is being reduced (for example, 24 nm to 19 nm).
- the wiring width is being reduced (for example, 24 nm to 19 nm).
- extremely fine particles (fine particles) having a diameter of about 40 nm are mixed, defects such as defective wiring (conducting failure) and defective devices (short circuit) are caused. Therefore, it is strongly desired to more strictly suppress the generation of fine particles due to the device components.
- the present invention was made to cope with such problems, and stably and effectively suppress the generation of particles such as particle dropping by improving the plasma resistance and corrosion resistance of the coating itself during the etching process, It is possible to prevent contamination due to impurities by suppressing the decrease in productivity and the increase in etching and film formation costs due to equipment cleaning and parts replacement, as well as preventing film peeling and the generation of fine particles. It is an object of the present invention to provide a plasma device component and a plasma device component that do not cause damage such as corrosion or deformation to a member by chemical solution processing or blast processing in a regenerating process.
- a plasma device component having an aluminum nitride coating formed by the impact sintering method of the present invention contains aluminum nitride particles in an aluminum nitride (AlN) coating, the coating thickness is 10 ⁇ m or more, and the coating density is The area ratio of aluminum nitride particles in which the grain boundaries existing in the unit area of 20 ⁇ m ⁇ 20 ⁇ m of the coating structure can be confirmed is 0 to 90%, while the area ratio of aluminum nitride particles in which the grain boundaries cannot be confirmed is 90% or more. It is characterized by being 10 to 100%.
- the aluminum nitride film has a thickness of 10 to 200 ⁇ m, and the density of the film is preferably 99% or more and 100% or less.
- the aluminum nitride particles include fine particles having a size of 1 ⁇ m or less, and the aluminum nitride particles in which the grain boundaries can be confirmed preferably have an average particle size of 2 ⁇ m or less.
- the average average particle size of the aluminum nitride particles is preferably 5 ⁇ m or less.
- the ratio of the strongest peak Im of AlN to the strongest peak Ic of Al 2 O 3 (Im / Ic) is preferably 8 or more.
- the aluminum nitride film is preferably polished to have a surface roughness Ra of 0.5 ⁇ m or less.
- the method of manufacturing a plasma device component in which an aluminum nitride film is formed by the shock sintering method of the present invention includes a step of supplying a slurry containing aluminum nitride particles to a combustion flame, and an aluminum nitride particle injection speed of 400 to 1000 m. And a step of spraying onto the substrate after adjusting to / sec.
- the average particle diameter of the aluminum nitride particles is preferably 0.05 to 5 ⁇ m.
- the thickness of the aluminum nitride film is preferably 10 ⁇ m or more. Moreover, it is preferable to supply the slurry containing aluminum nitride particles to the center of the combustion flame.
- the plasma resistance of the component can be improved, and the amount of particles and impurity contamination can be greatly suppressed.
- the chemical treatment or blast treatment in the regeneration treatment does not damage the member such as corrosion or deformation, so that the number of times of cleaning the device or replacing parts can be greatly reduced.
- the reduction in the amount of generated particles greatly contributes to the improvement of the yield of various thin films to be plasma-treated, and elements and components using the thin films.
- the reduction in the number of device cleanings and part replacements greatly contributes to the improvement of productivity and the reduction of etching costs and film formation costs.
- generation of fine particles generated from a component is stably and effectively suppressed, and a decrease in productivity and an increase in component cost due to frequent device cleaning and component replacement are suppressed. That can be applied to the manufacture of highly integrated semiconductor devices, and that can improve the operating rate of the plasma apparatus and can reduce etching and film formation costs, and a method for manufacturing the same. Can be provided.
- the component for a plasma device having an aluminum nitride coating formed on the surface of a substrate according to the present invention by an impact sintering method contains aluminum nitride particles in the aluminum nitride coating, and the coating thickness is 10 ⁇ m or more.
- the area ratio of the aluminum nitride particles in which the grain boundaries existing in the unit area 20 ⁇ m ⁇ 20 ⁇ m of the coating structure can be confirmed is 0 to 90%, while the grain boundaries are not confirmed.
- the area ratio is 10 to 100%.
- FIG. 1 shows an embodiment of a plasma device component according to the present invention.
- reference numeral 1 denotes a plasma device component
- 3 denotes a base material
- 2 denotes an aluminum nitride film integrally formed on the surface of the base material 3.
- AlN aluminum nitride having strong resistance to plasma attack or radical attack (for example, active F radical or Cl radical) and particularly chlorine plasma or fluorine plasma is preferable.
- the aluminum nitride particles whose grain boundaries can be confirmed can be confirmed by an enlarged photograph of the coating structure. For example, an enlarged photograph of 5000 times is taken with a scanning electron micrograph.
- FIG. 2 shows an organization chart (enlarged photograph) showing an example of the aluminum nitride coating.
- reference numeral 4 denotes aluminum nitride particles whose grain boundaries cannot be confirmed
- reference numeral 5 denotes aluminum nitride particles whose grain boundaries can be confirmed.
- the unit area serving as a visual field for observing the tissue state of the coating was 20 ⁇ m ⁇ 20 ⁇ m. Further, this unit area is measured at three arbitrary points, and the average value is defined as the area ratio of “aluminum nitride particles whose grain boundaries can be confirmed” and “aluminum nitride particles whose grain boundaries cannot be confirmed”.
- FIG. 2 shows a state where a particle group of “aluminum nitride particles whose grain boundaries can be confirmed” and a particle group of “aluminum nitride particles whose grain boundaries cannot be confirmed” are mixed.
- the impact sintering method is a coating method in which particles are ejected by a combustion flame flame to form a film.
- the particles collide with the substrate at a high speed, and the particles are sintered and bonded by the crushing heat of the particles due to the collision. It is a method of forming.
- the aluminum nitride particles tend to form a film having a crushed shape rather than the particle shape of the raw material powder.
- the aluminum nitride particles can be formed without melting and decomposing, and the particle shape of the raw material powder is almost the same. An aluminum nitride film having a high film density that is maintained can be obtained.
- the impact sintering method enables high-speed injection, it is easy to obtain a structure in which “aluminum nitride particles whose grain boundaries can be confirmed” and “aluminum nitride particles whose grain boundaries cannot be confirmed” are mixed.
- aluminum nitride particles whose grain boundaries can be confirmed When the total area ratio of “aluminum nitride particles whose grain boundaries can be confirmed” and “aluminum nitride particles whose grain boundaries cannot be confirmed” is 100%, “aluminum nitride particles whose grain boundaries can be confirmed” is 0 to It is important that the aluminum nitride particles having a grain boundary of 90% with no grain boundary confirmed have an area ratio of 10 to 100%.
- the impact sintering method is a film forming method in which aluminum nitride particles are jetted at a high speed and the particles are deposited by destructive heat when colliding with a substrate.
- Aluminum nitride particles in which grain boundaries cannot be confirmed are formed by bonding of aluminum nitride particles by heat during deposition by destructive heat.
- the raw material powder is not melted and sprayed unlike spraying, so that the powder can be deposited while maintaining the powder shape of the aluminum nitride particles as the raw material powder. Therefore, a dense film having a strong bonding force can be formed without generating stress inside the film.
- the area ratio of “aluminum nitride particles whose grain boundaries can be confirmed” is preferably 0 to 50%. This is the same meaning that the area ratio of “aluminum nitride particles whose grain boundaries cannot be confirmed” is preferably in the range of 50 to 100%.
- the film thickness of the aluminum nitride film needs to be 10 ⁇ m or more. If the film thickness is less than 10 ⁇ m, the effect of providing the aluminum nitride film cannot be obtained sufficiently, and there is a possibility that the film may peel off.
- the upper limit of the thickness of the aluminum nitride film is not particularly limited, but if it is excessively thick, no further effect can be obtained and the cost increases. Therefore, the thickness of the aluminum nitride film is in the range of 10 to 200 ⁇ m, more preferably in the range of 50 to 150 ⁇ m.
- the density of the coating needs to be 90% or more.
- the coating density is a term opposite to the porosity, and the coating density of 90% or more has the same meaning as the porosity of 10% or less.
- the film density is measured by taking a cross-sectional structure photograph of the aluminum nitride film in the film thickness direction, taking an enlarged photograph of 500 times with an optical microscope, and calculating the area ratio of pores reflected therein.
- “Membrane density (%) 100 ⁇ pore area ratio”
- the film density is calculated by the following formula. For the calculation of the film density, an area of a unit area of 200 ⁇ m ⁇ 200 ⁇ m of the coating structure is analyzed. When the film thickness is small, a plurality of locations are measured until the total unit area becomes 200 ⁇ m ⁇ 200 ⁇ m.
- the density of the coating is 90% or more, more preferably 95% or more, and further preferably 99% or more and 100% or less. If there are many pores (voids) in the aluminum nitride coating, erosion such as plasma attack proceeds from the pores and the life of the aluminum nitride coating is reduced. In particular, it is important that the surface of the aluminum nitride film has few pores.
- the surface roughness of the aluminum nitride film is preferably Ra 0.5 ⁇ m or less by polishing treatment.
- the surface roughness after the polishing process is Ra 0.5 ⁇ m or less, the wafer comes into close contact with the dielectric layer and the etching uniformity is improved.
- the surface roughness after the polishing process exceeds Ra 0.5 ⁇ m, the wafer is deformed, the adhesion is lowered, the etching property becomes non-uniform, and particles are liable to be generated.
- the average particle diameter of the aluminum nitride particles that can confirm the grain boundary is 2 ⁇ m or less, and the average particle diameter of the entire aluminum nitride particles including the aluminum nitride particles that cannot confirm the grain boundary is 5 ⁇ m or less.
- the aluminum nitride powder as the raw material powder used in the impact sintering method preferably has an average particle size in the range of 0.05 to 5 ⁇ m. If the average particle size of the aluminum nitride particles as the raw material powder exceeds 5 ⁇ m, when the particles collide, it will not be crushed and it will be difficult to form a coating, and the coating will be damaged by the blasting action of the particles themselves and cracks will occur. May occur.
- the aluminum nitride particles are 5 ⁇ m or less
- crushing proceeds moderately when the fine particles collide with each other, and particle bonding is promoted by heat generated by crushing, and a film is easily formed.
- the formed film has a high bonding force between particles, wear due to plasma attack and radical attack is reduced, the amount of generated particles is reduced, and plasma resistance is improved.
- a more preferable value of the particle size of the aluminum nitride particles is 0.05 ⁇ m or more and 3 ⁇ m or less.
- the application range of the fine particle diameter is preferably 0.05 to 5 ⁇ m.
- the fine particles having a particle size of less than 0.05 ⁇ m are less than 5% of the entire aluminum nitride particles, the film formation is not deteriorated, so that powder containing fine particles of less than 0.05 ⁇ m may be used.
- the method for obtaining the average particle size of the aluminum nitride particles is carried out using an enlarged photograph as shown in FIG.
- the aluminum nitride particles whose grain boundaries can be confirmed have the longest diagonal line as the particle size in the individual particles shown in the photograph.
- the hypothetical circle of each particle is used to make the diameter the particle size. This operation is measured for each of 50 particles for a total of 100 particles, and the average value is taken as the average particle size.
- the ratio of the strongest peak Im of AlN to the strongest peak Ic of Al 2 O 3 is preferably 8 or more.
- a method for manufacturing a plasma device component in which an aluminum nitride film is formed on a substrate surface by an impact sintering method a step of supplying a slurry containing aluminum nitride particles to a combustion flame, and injection of aluminum nitride particles And adjusting the speed to 400 to 1000 m / sec and spraying onto the base material.
- the average particle diameter of the aluminum nitride particles is preferably 0.05 to 5 ⁇ m.
- the film thickness of the aluminum nitride film is preferably 10 ⁇ m or more.
- the slurry containing aluminum nitride particles is preferably supplied to the center of the combustion flame.
- the impact sintering method is a film forming method in which a slurry containing aluminum nitride particles is supplied into a combustion flame to spray aluminum nitride particles at a high speed.
- the film forming apparatus for performing the impact sintering method includes a combustion source supply port for supplying a combustion source and a combustion chamber connected thereto. By burning the combustion source in the combustion chamber, a combustion flame is generated at the combustion flame opening. There is a slurry supply port in the vicinity of the combustion flame, and the aluminum nitride particle slurry supplied from the slurry supply port is sprayed from the combustion flame to the base material through the nozzle and is formed into a film.
- the combustion source oxygen, acetylene, kerosene or the like is used, and two or more kinds may be used as necessary.
- the temperature of the combustion flame is controlled by adjusting the combustion conditions such as the mixing ratio of the combustion source and the amount of cooling gas introduced so that the temperature is lower than the boiling point of the aluminum nitride particles to be deposited.
- the temperature of the combustion flame is higher than the boiling point, the aluminum nitride particles supplied as a slurry evaporate, decompose, or melt as a result of vaporization, decomposition, or melting even in high-speed injection. turn into.
- the spray speed of the aluminum nitride particles is in the range of 400 m / sec to 1000 m / sec. If the spray speed is as low as less than 400 m / sec, pulverization when particles collide becomes insufficient, and a film having a high film density may not be obtained. On the other hand, when the injection speed exceeds 1000 m / sec, the impact force becomes excessive, the blast effect due to the aluminum nitride particles is likely to occur, and the intended film is hardly obtained.
- the aluminum nitride particle slurry When the aluminum nitride particle slurry is introduced into the slurry supply port, it is preferable to supply the slurry so that the slurry is positioned at the center of the combustion flame. If the aluminum nitride particle slurry is supplied to the outside of the combustion flame, the injection speed is not stable. Also, some aluminum nitride particles are injected outside the combustion flame, and some are injected after reaching the center. Even with the same flame flame, the temperature is slightly different between the outside and inside. By forming films at the same temperature and the same injection speed as much as possible, it is possible to control the structure of “particles whose grain boundaries can be confirmed” and “particles whose grain boundaries cannot be confirmed”.
- the impact sintering method is a coating method in which particles are jetted by a combustion flame, and the particles collide at a high speed, and a film is formed by sinter bonding with the crushing heat of the particles caused by the collision. is there. For this reason, the aluminum nitride particles in the coating film tend to form a crushed film rather than the particle shape of the raw material powder.
- the aluminum nitride particles can be formed without melting and decomposing, and the film density is high.
- An aluminum nitride coating can be obtained.
- An aluminum nitride film in which the area ratio of aluminum nitride particles in which grain boundaries can be confirmed as in the present invention is 0 to 90%, while the area ratio of aluminum nitride particles in which grain boundaries cannot be confirmed is 10 to 100% efficiently. Obtainable.
- the impact sintering method is a method in which aluminum nitride particles are jetted at high speed using a combustion flame, and are bonded by sintering using the heat of fracture of the particles at the time of collision.
- the injection distance L is 100 to 400 mm.
- the spray distance L is less than 100 mm, it is difficult to obtain a coating that is sintered and bonded without being crushed because the distance is too short.
- the spray distance L exceeds 400 mm, it is too far away, so that the impact force becomes weak and it is difficult to obtain the intended aluminum nitride coating.
- the injection distance L is 100 to 200 mm.
- the nitride particle slurry is preferably a slurry containing nitride particles having an average particle diameter of 0.05 to 5 ⁇ m as a raw material powder.
- the solvent to be slurried is preferably a solvent that is relatively volatile, such as methyl alcohol and ethyl alcohol.
- the nitride particles are preferably mixed with a solvent after being sufficiently pulverized to have no coarse particles. For example, when coarse particles having a particle size of 20 ⁇ m or more are present, it is difficult to obtain a uniform film.
- the ratio of nitride particles in the slurry is preferably 30 to 80 vol%. In the case of a slurry having appropriate fluidity, the supply to the supply port becomes smoother and the supply amount is stabilized, so that a uniform film can be obtained.
- the plasma resistance of the plasma device parts is remarkably improved, and it is possible to reduce particles, reduce impurity contamination, and extend the service life of the parts. For this reason, if it is an apparatus installation using the components for such a plasma etching apparatus, generation
- exchange are attained.
- the slurry particles are sprayed onto the substrate at a high speed by the impact sintering method and the particles are deposited with the collision energy, blasting is not necessary when depositing a film on the component parts. Since there is no residual or surface defects, the adhesion of the coating is greatly improved. This is because the surface oxide film of the component is destroyed by high-speed collision of particles, and the active surface is exposed, so that a film is formed directly on the surface of the part. It is thought that this occurs and is formed as a film.
- An electrostatic chuck as a plasma device component is prepared by forming an aluminum nitride film on an alumina substrate (300 mm x 3 mm) under the conditions shown in Table 1 by impact sintering using a combustion frame type injection device. did.
- a solvent for preparing a slurry in which aluminum nitride (AlN) particles as raw material powder having an average particle diameter shown in Table 1 were dispersed ethyl alcohol was used.
- the raw material powder used was high-purity aluminum nitride particles having a purity of 99.9% or more.
- the aluminum nitride particles as the raw material powder a raw material powder having no coarse particles having a particle diameter exceeding 10 ⁇ m after carrying out sufficient pulverization and sieving operations was used.
- Comparative Example 1 is a part having a coating made of an aluminum nitride sintered body to which a sintering aid is added.
- Comparative Example 1 was a comparative material in which 0.5% of Y 2 O 3 sintering aid was added and a film was formed of a sintered body obtained by a sintering method.
- the film density was obtained from the ratio of pores appearing in an enlarged photograph (500 times) so that the total unit area of the film cross section was 200 ⁇ m ⁇ 200 ⁇ m.
- the area ratio between the particles where the grain boundaries can be confirmed and the particles where the grain boundaries cannot be confirmed is such that a grain boundary of one aluminum nitride particle can be distinguished by taking an enlarged photograph (5000 times) of a unit area 20 ⁇ m ⁇ 20 ⁇ m on the film surface.
- a grain boundary of one aluminum nitride particle can be distinguished by taking an enlarged photograph (5000 times) of a unit area 20 ⁇ m ⁇ 20 ⁇ m on the film surface.
- each coating was investigated by XRD analysis.
- the XRD analysis was carried out using a Cu target under the conditions of tube voltage: 40 kV and tube current: 40 mA, and the ratio of the strongest peak Im of AlN to the strongest peak Ic of Al 2 O 3 (Im / Ic) was investigated.
- the measurement results are shown in Table 2 below.
- the aluminum nitride film of the parts according to each Example has a high film density, and the ratio (area ratio) of “aluminum nitride particles whose grain boundaries can be confirmed” is 0 to 90%. It was within the range.
- the aluminum nitride particles are slightly smaller than the size of the raw material powder. Further, since it was not melted more than necessary, the crystal structure was the same as that of the raw material powder.
- the surface roughness Ra of the aluminum nitride film of the parts according to Examples 1 to 7 was 0.5 ⁇ m or less. Further, the surface roughness Ra of the aluminum nitride film in Comparative Example 1 was 1.5 ⁇ m.
- the electrostatic chuck parts according to the respective examples and comparative examples were placed in a plasma etching apparatus and exposed to a mixed etching gas of CF 4 (50 sccm) + O 2 (20 sccm) + Ar (50 sccm).
- the vacuum degree in the etching chamber is set to 10 mTorr, the output is 300 W (bias 100 W), and the aluminum nitride film is operated continuously for 2 hours.
- the tape was peeled off, and the tape was observed with an SEM to measure the area of aluminum nitride particles present in a 125 ⁇ m ⁇ 95 ⁇ m visual field.
- the weight change of the parts before and after the exposure test to the mixed etching gas was measured to determine the weight reduction per unit area. The measurement results are shown in Table 3 below.
- volume resistivity of each aluminum nitride film was measured by a four-terminal method (conforming to JIS K 7194) at room temperature (25 ° C.), and as a result, it was 2.7 to 3.3 ⁇ 10 11 ⁇ ⁇ cm. .
- particles generated from the component can be stably and effectively prevented. Further, since the corrosion of the coating against the active radicals of the corrosive gas is suppressed, it is possible to prevent the generation of particles from the coating, and it is possible to suppress the generation of particles by reducing the corrosion products and preventing the coating from falling off. Therefore, it is possible to reduce the number of times of cleaning the plasma device parts and replacing the parts.
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Abstract
Description
「膜密度(%)=100-気孔の面積率」
の算式により膜密度を算出する。膜密度の算出には、被膜組織の単位面積200μm×200μmの面積を分析するものとする。なお、膜厚が薄いときは、合計の単位面積が200μm×200μmとなるまで複数個所を測定するものとする。
燃焼フレーム型噴射装置を使用して衝撃焼結法により、アルミナ製基材(300mm×3mm)上に、表1示す条件で窒化アルミニウム被膜を形成してプラズマ装置用部品としての静電チャックを調製した。表1示す平均粒径を有する原料粉末としての窒化アルミニウム(AlN)粒子を分散したスラリーを調製するための溶媒は、いずれもエチルアルコールを使用した。また、使用した原料粉末はいずれも純度が99.9%以上である高純度窒化アルミニウム粒子を用いた。また、原料粉末としての窒化アルミニウム粒子としては、十分な粉砕および篩分け操作を実施して粒径が10μmを超えるような粗大粒子が無い原料粉末を使用した。
2…窒化アルミニウム被膜
3…基材
4…粒界が確認できない窒化アルミニウム粒子
5…粒界が確認できる窒化アルミニウム粒子
Claims (16)
- 金属またはセラミックスから成る基材と、この基材上の最表面に形成された窒化アルミニウム被膜とから成るプラズマ装置用部品において、上記窒化アルミニウム被膜の厚さが10μm以上であり、膜密度が90%以上であり、窒化アルミニウム被膜の単位面積20μm×20μm中に存在する粒界が確認できる窒化アルミニウム粒子の面積率が0~90%である一方、粒界が確認できない窒化アルミニウム粒子の面積率が10~100%であることを特徴とするプラズマ装置用部品。
- 前記基材が金属電極を内部に埋設したセラミックスから成り、この基材上の最表面に前記窒化アルミニウム被膜を有していることを特徴とする請求項1に記載のプラズマ装置用部品。
- 前記窒化アルミニウム被膜は、衝撃焼結法により形成された窒化アルミニウム被膜であることを特徴とする請求項1乃至2のいずれか1項に記載のプラズマ装置用部品。
- 前記窒化アルミニウム被膜を形成する粒子全体の平均粒径が5μm以下であることを特徴とする請求項1乃至3のいずれか1項に記載のプラズマ装置用部品。
- 前記窒化アルミニウム被膜を形成する粒子は、粒径1μm以下の微粒子を含むことを特徴とする請求項1乃至4のいずれか1項に記載のプラズマ装置用部品。
- 前記窒化アルミニウム被膜は、膜厚が10~200μmであり、膜密度が99%以上100%以下であることを特徴とする請求項1乃至5のいずれか1項に記載のプラズマ装置用部品。
- 前記粒界が確認できる窒化アルミニウム粒子の平均粒径が2μm以下であることを特徴とする請求項1乃至6のいずれか1項に記載のプラズマ装置用部品。
- 前記窒化アルミニウム粒子の平均粒径が0.05~5μmであることを特徴とする請求項1乃至7のいずれか1項に記載のプラズマ装置用部品。
- 前記窒化アルミニウム被膜をXRD分析したとき、Al2O3の最強ピークIcに対するAlNの最強ピークImの比(Im/Ic)が8以上であることを特徴とする請求項1乃至8のいずれか1項に記載のプラズマ装置用部品。
- 前記窒化アルミニウム被膜は、研磨処理によって表面粗さRaが0.5μm以下に形成されていることを特徴とする請求項1乃至9のいずれか1項に記載のプラズマ装置用部品。
- 金属またはセラミックスから成る基材上の最表面に、衝撃焼結法により窒化アルミニウム被膜を形成したプラズマエッチング装置用部品の製造方法において、燃焼フレーム炎に窒化アルミニウム粒子を含むスラリーを供給する工程と、その窒化アルミニウム粒子を、噴射速度が400~1000m/secとなるように基材上に噴射させる工程とを具備することを特徴とするプラズマ装置用部品の製造方法。
- 前記スラリーに含まれる窒化アルミニウム粒子は、純度が99.9%以上である窒化アルミニウム粒子であることを特徴とする請求項11に記載のプラズマ装置用部品の製造方法。
- 前記窒化アルミニウム粒子の平均粒径が0.05~5μmであることを特徴とする請求項11乃至12のいずれか1項に記載のプラズマ装置用部品の製造方法。
- 前記窒化アルミニウム被膜の膜厚が10μm以上であることを特徴とする請求項11乃至13のいずれか1項に記載のプラズマ装置用部品の製造方法。
- 前記窒化アルミニウム粒子を含むスラリーを燃焼フレーム炎の中心に供給することを特徴とする請求項11乃至14のいずれか1項に記載のプラズマ装置用部品の製造方法。
- 前記窒化アルミニウム粒子を含むスラリーを供給する燃焼フレームの温度は、供給する窒化アルミニウム粒子の沸点未満に調整されていることを特徴とする請求項11乃至15のいずれか1項に記載のプラズマ装置用部品の製造方法。
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JPH07297265A (ja) * | 1994-04-26 | 1995-11-10 | Shin Etsu Chem Co Ltd | 静電チャック |
JP2000158275A (ja) * | 1998-11-27 | 2000-06-13 | Kyocera Corp | 静電チャック |
JP2007508690A (ja) * | 2003-10-09 | 2007-04-05 | エスエヌティー コーポレーション,リミティッド | 無焼結窒化アルミニウム静電チャックおよびその製造方法 |
JP2009293061A (ja) * | 2008-06-03 | 2009-12-17 | Riverstone Kogyo Kk | 微粉末セラミックス衝撃焼結被覆法 |
JP2012191200A (ja) * | 2011-02-25 | 2012-10-04 | Toshiba Corp | プラズマ処理装置 |
WO2013176168A1 (ja) * | 2012-05-22 | 2013-11-28 | 株式会社東芝 | プラズマ処理装置用部品およびプラズマ処理装置用部品の製造方法 |
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KR20160075724A (ko) | 2016-06-29 |
KR101787931B1 (ko) | 2017-10-18 |
JPWO2015080135A1 (ja) | 2017-03-16 |
CN105793467A (zh) | 2016-07-20 |
US10100413B2 (en) | 2018-10-16 |
CN105793467B (zh) | 2018-04-13 |
US20170002470A1 (en) | 2017-01-05 |
JP6526569B2 (ja) | 2019-06-05 |
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