WO2019069939A1 - Corps en alumine frittée et procédé de fabrication associé - Google Patents

Corps en alumine frittée et procédé de fabrication associé Download PDF

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Publication number
WO2019069939A1
WO2019069939A1 PCT/JP2018/036914 JP2018036914W WO2019069939A1 WO 2019069939 A1 WO2019069939 A1 WO 2019069939A1 JP 2018036914 W JP2018036914 W JP 2018036914W WO 2019069939 A1 WO2019069939 A1 WO 2019069939A1
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Prior art keywords
sintered body
alumina
content
less
converted
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PCT/JP2018/036914
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English (en)
Japanese (ja)
Inventor
早侑 吉田
宮下　幸久
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クアーズテック株式会社
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Priority claimed from JP2018178652A external-priority patent/JP7154912B2/ja
Priority claimed from JP2018180299A external-priority patent/JP7231367B2/ja
Application filed by クアーズテック株式会社 filed Critical クアーズテック株式会社
Priority to CN201880065428.0A priority Critical patent/CN111201208B/zh
Priority to US16/753,756 priority patent/US11760694B2/en
Priority to KR1020207009705A priority patent/KR102354650B1/ko
Publication of WO2019069939A1 publication Critical patent/WO2019069939A1/fr

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Definitions

  • the present invention relates to an alumina-based sintered body and a method for producing the same, which is suitably used or coated on, for example, a member used in a plasma processing apparatus, an etcher for manufacturing a semiconductor / liquid crystal display, a CVD apparatus, etc.
  • the present invention relates to an alumina sintered body suitably used as a base material or the like of a plasma property member, and a method for producing the alumina sintered body.
  • Alumina-based sintered bodies are excellent in heat resistance, chemical resistance, plasma resistance, and have a small dielectric loss tangent (tan ⁇ ) in a high frequency region, so, for example, plasma processing devices, etchers for manufacturing semiconductor / liquid crystal display devices, It is used for the member etc. which are used for a CVD apparatus etc., and the base material etc. of the plasma-resistant member to be coated.
  • various proposals have been made to improve the corrosion resistance and dielectric loss tangent (dielectric loss) in this alumina sintered body.
  • Patent Document 1 provides an alumina sintered body having a low dielectric loss tangent while having a high corrosion resistance and containing an oxide of Na, a member for a semiconductor manufacturing apparatus, and a member for a liquid crystal panel manufacturing apparatus. the purpose, of all components 100% by weight, or less 500ppm content 30ppm or more and the Na Na 2 and O terms, it is the Al Al 2 O 3-converted content of 99.4% by mass or more, 8 An aluminous sintered body is proposed in which the value of the dielectric loss tangent at 5 GHz is not more than 0.5 times the value of the Na 2 O converted content.
  • an object of the invention to provide an alumina sintered body and a manufacturing method thereof can be reduced variations in dielectric loss tangent in accordance with the difference in position, Al 2 O 3 content of 99.4 mass % Is contained in the range of 99.8 mass%, the Si content is contained in the range of 0.11 mass% to 0.38 mass% in terms of SiO 2 , and the deviation of the crystal particle diameter in each of the surface layer part
  • An alumina sintered body is proposed in which the deviation of the occupation ratio of crystals having a particle diameter of 6.5 ⁇ m or more in each of the surface layer portion and the inside is 0.6% or less. .
  • Patent Document 3 while improving ease of processing, stably and to provide an alumina sintered body it is possible to reduce the dielectric loss tangent and its manufacturing method, the Al 2 O 3
  • the purity is 99.3 wt% or more
  • Ti is dissolved in Al 2 O 3 crystal particles in the range of 0.08 wt% to 0.20 wt% in terms of TiO 2
  • Si is a sintered body in terms of SiO 2
  • An aluminous sintered body contained in the range of 0.05 wt% to 0.40 wt% has been proposed.
  • Patent Document 4 in the plasma-resistant member, when cost or strength of the substrate is required, a film having plasma resistance made of Y 2 O 3 or YAG is formed on the surface of the alumina ceramic substrate. It is proposed to form. Furthermore, regarding film formation, for example, Patent Document 5 discloses that a ceramic spray-coated film having a thickness of 200 ⁇ m or less is formed on the surface of a base member for forming a semiconductor manufacturing apparatus. Patent Document 5 shows that the porosity of the sprayed film is 5% to 10%.
  • the sprayed coating has a thickness of about 200 ⁇ m, and the porosity of the sprayed film is 5% to 10 Since it is%, when it is used under plasma exposure, the thermal spray coating may be exfoliated to generate particles.
  • the thickness of the sprayed film tends to be reduced to about several ⁇ m, and when the sprayed film formed on the substrate is formed, pores are present in the substrate. There has been a problem that uniform film formation is hindered.
  • Patent Documents 1 to 3 Although there are several proposals for corrosion resistance and dielectric loss tangent (dielectric loss) of an alumina-based sintered body, as far as the present applicant knows, a dense sprayed film can be made uniform. It has not been proposed about the alumina-based sintered body which can be formed into a film.
  • the present inventors diligently studied an alumina sintered body suitable as a substrate of a plasma resistant member to be coated.
  • the present invention also contemplates an alumina-based sintered body having corrosion resistance and low dielectric loss characteristics, and capable of uniformly forming a dense film, as an alumina-based sintered body. completed.
  • the present invention provides an alumina-based sintered body having corrosion resistance, low dielectric loss characteristics, and capable of uniformly forming a dense film, and a method for producing the alumina-based sintered body. Purpose.
  • the present invention is an alumina sintered body having a content of 70 wt% or more in terms of Al converted to Al 2 O 3 as a first aspect, which comprises Zr in the alumina sintered body
  • an aluminous sintered body having a ZrO 2 converted content of 30 wt% or less, a Si converted content of SiO 2 of 170 ppm to 600 ppm, and a Na converted content of Na 2 O of 27 ppm or less.
  • the alumina sintered body having the specific configuration according to the first aspect of the present invention has corrosion resistance and low dielectric loss characteristics. Specifically, when the dielectric loss tangent tan ⁇ is 10 -3 or less, the number of pores of the alumina sintered body is small, and the film is formed on the surface, the number of voids in the surface of the thin film in the range of about 200 ⁇ m ⁇ 200 ⁇ m is 100. The average diameter can be 5 ⁇ m or less, and a uniform dense film can be formed on the substrate. Further, the alumina-based sintered body according to the first aspect has a large bending strength, and specifically, the three-point bending strength has a strength of 320 MPa or more.
  • the average crystal grain size of the Al 2 O 3 crystal in the alumina sintered body is 3 ⁇ m or more and 15 ⁇ m or less.
  • a uniform film can be formed on the surface of the alumina sintered body.
  • the present invention is, as a second aspect, an alumina sintered body containing 70 wt% or more of Al converted to Al 2 O 3 , and in the alumina sintered body,
  • the content of Zr converted into ZrO 2 is 30 wt% or less
  • the content of Y converted into Y 2 O 3 is 1 wt% or more and 10 wt% or less
  • the content of Si converted into SiO 2 is 170 ppm or more and 600 ppm or less
  • Na Na 2
  • An aluminous sintered body is provided, wherein the O-converted content is 27 ppm or less, and the Y-converted Y 2 O 3 converted content is equal to or less than the Zr 2 ZrO 2 converted content.
  • the alumina-based sintered body having the specific constitution according to the second aspect of the present invention has corrosion resistance and low dielectric loss characteristics. Specifically, when the dielectric loss tangent tan ⁇ is 10 -3 or less, the number of pores of the alumina sintered body is small, and the film is formed on the surface, the number of voids in the surface of the thin film in the range of about 200 ⁇ m ⁇ 200 ⁇ m is 100. The average diameter can be 5 ⁇ m or less, and a uniform dense film can be formed on the substrate. Further, the alumina-based sintered body has high bending strength, and specifically, the three-point bending strength has a strength of 320 MPa or more.
  • the average crystal grain size of the Al 2 O 3 crystal in the alumina sintered body is 3 ⁇ m or more and 15 ⁇ m or less.
  • a uniform film can be formed on the surface of the alumina sintered body.
  • the present invention provides, as a third aspect, an alumina sintered body having a content of 99.8 wt% or more in terms of Al converted to Al 2 O 3 , wherein the alumina sintered
  • the content of Si in the body converted to SiO 2 is 170 ppm to 600 ppm
  • the content of Na converted to Na 2 O is 27 ppm or less
  • the density of the aluminous sintered body is 3.96 g / cm 3 or more
  • An alumina-based sintered body is provided.
  • the alumina-based sintered body having the specific configuration according to the third aspect of the present invention has corrosion resistance and low dielectric loss characteristics.
  • the density of the alumina sintered body is 3.96 g / cm 3 or more, and has a compactness. As a result, when the film is formed on the surface with few pores of the alumina sintered body, a uniform dense film can be formed on the substrate.
  • the content ratio of Mg in the aluminous sintered body in terms of MgO is 1.0 or more and 4.0 or less with respect to the content of the above Si in terms of SiO 2. Is desirable. Further, it is preferable that the content ratio of Ca in the alumina-based sintered body in terms of CaO be 3.0 or less with respect to the content of the above-described Si in SiO 2 conversion.
  • the average pore diameter of the alumina sintered body is preferably 5 ⁇ m or less.
  • the average crystal grain size of Al 2 O 3 crystals in the alumina sintered body is preferably 3 ⁇ m or more and 40 ⁇ m or less.
  • a corrosion resistant film or a corrosion resistant layer may be formed on at least a part of the alumina sintered body.
  • the alumina-based sintered body according to the present invention is manufactured by granulating the raw material powder and sintering the molded body obtained by molding at 1600 ° C. to 1900 ° C. in a hydrogen atmosphere.
  • an alumina sintered body having corrosion resistance and low dielectric loss characteristics can be obtained. Further, according to the present invention, when a film is formed on the surface of an alumina sintered body, an alumina sintered body capable of uniformly forming a dense film can be obtained.
  • FIG. 1 is a view showing a cross-sectional photograph according to Example 1A.
  • the alumina sintered body of the first embodiment according to the first aspect of the present invention will be described.
  • the alumina-based sintered body according to the first embodiment is an alumina-based sintered body in which the content of Al converted to Al 2 O 3 is 70 wt% or more, and the Zr in the alumina-based sintered body is converted to ZrO 2.
  • the content is 30 wt% or less, the content of Si converted to SiO 2 is 170 ppm or more and 600 ppm or less, and the content of Na converted to Na 2 O is 27 ppm or less.
  • This alumina sintered body is characterized in that it has a high flexural strength, corrosion resistance, low dielectric loss characteristics, and a base material capable of forming a uniform dense film.
  • the content of Al converted to Al 2 O 3 in this alumina sintered body is 70 wt% or more. Further, the content of Zr in terms of ZrO 2 is 30 wt% or less.
  • a crystal phase of ZrO 2 is formed in addition to the main crystal of Al 2 O 3 .
  • the crystal phase of ZrO 2 acts to reduce pores, suppresses abnormal grain growth and has a small particle size, and thus acts to increase high strength.
  • the content of Zr converted to ZrO 2 exceeds 30 wt%, the content of Al converted to Al 2 O 3 becomes less than 70 wt%, and the corrosion resistance is high against highly reactive halogen-based corrosive gases and their plasmas. Is not preferable because it can not be obtained. Further, when the content of Zr in terms of ZrO 2 exceeds 30 wt%, the amount of the crystal phase of ZrO 2 increases, whereby the strength of the aluminous sintered body decreases. Furthermore, it is not preferable because the dielectric loss tangent tan ⁇ exceeds 10 ⁇ 3 .
  • the content of Al converted to Al 2 O 3 is 70 wt% or more, and the content of Zr converted to ZrO 2 is 30 wt% or less.
  • Components other than Al 2 O 3 and ZrO 2 contained in the alumina-based sintered body are substances which are inevitably mixed in the alumina production process, and examples thereof include substances such as Si, Mg, Na, Ca, etc. .
  • the content of Si converted to SiO 2 in this alumina sintered body is 170 ppm or more and 600 ppm or less. If the content of Si converted to SiO 2 is less than 170 ppm, the silicate required for the expression of low dielectric loss characteristics is not uniformly formed, the dielectric loss increases, and the effect of power saving can not be obtained. Not desirable. On the other hand, when the content of Si converted into SiO 2 exceeds 600 ppm, the density of the aluminous sintered body is small and it is not preferable because it does not become compact.
  • the content of Na converted to Na 2 O is 27 ppm or less. If the content of Na converted to Na 2 O exceeds 27 ppm, the dielectric loss increases and the effect of power saving can not be obtained, which is not preferable.
  • the content ratio of Mg converted to MgO is 1.0 or more and 4.0 or less with respect to the content of Si converted to SiO 2.
  • a silicate may be formed at the grain boundary of the aluminous sintered body Since it is possible, an alumina sintered body having high density and low dielectric loss can be obtained.
  • the content ratio of Ca converted to CaO is preferably 3.0 or less with respect to the content of Si converted to SiO 2 .
  • To content of Ca content ratio was calculated as CaO and the said Si SiO 2 converted, by more than 3.0, since the silicate is formed in the grain boundary, the low dielectric loss alumina sintered You can get the body.
  • the average crystal grain size of the Al 2 O 3 crystal in the alumina sintered body according to the first embodiment is preferably 3 ⁇ m or more and 15 ⁇ m or less.
  • the average crystal grain size of Al 2 O 3 crystals in the alumina sintered body is 3 ⁇ m or more and 15 ⁇ m or less, the presence of pores of the alumina sintered body can be reduced, and a sintered body with higher density can be obtained.
  • an alumina sintered body having a three-point bending strength of 320 MPa or more can be obtained.
  • the water absorption rate of the alumina sintered body concerning 1st Embodiment is 0.2% or less.
  • the average pore diameter of the alumina sintered body according to the first embodiment is preferably 5 ⁇ m or less. When the average pore diameter of the alumina sintered body is 5 ⁇ m or less, a thin film can be formed more uniformly on the surface of the alumina sintered body.
  • the alumina-based sintered body according to the first embodiment may be used by itself, but a sintered body having a dense film formed on the surface may be used.
  • This film is obtained, for example, by depositing yttria material on the aluminous sintered body using an aerosol deposition method or a PVD method.
  • the alumina-based sintered body in which the yttria material is formed into a film as described above has high plasma resistance, is excellent in low dusting property, and can achieve power saving and the like due to the low dielectric loss characteristics of the base material.
  • the thin film when the thin film is formed on the surface of the aluminous sintered body, the water absorption rate is 0.2% or less, the thin film can be formed uniformly.
  • a thin film of yttria when the average pore diameter of the alumina sintered body is 5 ⁇ m or less, a thin film of yttria can be formed more uniformly on the surface of the alumina sintered body.
  • the film formed on the surface of the alumina sintered body is not limited to the yttria material, and a composite oxide of yttrium oxide and aluminum oxide (YAG), erbium oxide, other rare earth oxides or rare earth oxides It may be a composite oxide containing an oxide.
  • the surface roughness Ra of the surface of the alumina sintered body on which the film is formed is desirably less than 0.1 ⁇ m.
  • the surface of the alumina sintered body may be mirror-polished to have a surface roughness of less than 0.1 ⁇ m. That is, it is desirable that the average pore diameter of the surface of the alumina sintered body on which the film is formed be 5 ⁇ m or less, and the surface roughness Ra be less than 0.1 ⁇ m.
  • the thin film can be formed more uniformly, peeling of the thin film can be suppressed, and generation of particles can be suppressed.
  • the film formed on the surface of the alumina sintered body may be formed on a part of the surface of the alumina sintered body.
  • the film thickness is not particularly limited, but is preferably 1 ⁇ m to 20 ⁇ m.
  • an alumina-based sintered body can be manufactured by the general manufacturing method of an alumina-based sintered body, if an example is mentioned, it can be manufactured by the following method. First, a ZrO 2 powder or an aqueous solution thereof is added to an Al 2 O 3 powder having a predetermined median diameter, and a binder or the like (for example, PVA) is added to prepare a raw material powder. A raw material slurry obtained by stirring and mixing the raw material powder with a mixer is granulated.
  • a binder or the like for example, PVA
  • a molded body is produced.
  • various methods such as uniaxial press molding, CIP molding, wet molding, pressure casting and the like can be used.
  • the above-mentioned compact is sintered in a hydrogen atmosphere at a temperature range of 1600 ° C. to 1900 ° C. for 6 hours or more to obtain an aluminous sintered body.
  • a high density alumina sintered body can be obtained.
  • the alumina-based sintered body according to the second embodiment is an alumina-based sintered body in which the content of Al converted to Al 2 O 3 is 70 wt% or more, and the Zr in the alumina-based sintered body is ZrO 2
  • the converted content is 30 wt% or less
  • the content of Y converted to Y 2 O 3 is 1 wt% or more and 10 wt% or less
  • the content of Si converted to SiO 2 is 170 ppm to 600 ppm or less
  • the content of Y converted to Y 2 O 3 is less than the content of Zr converted to ZrO 2 .
  • the alumina sintered body according to the second embodiment has a large flexural strength, corrosion resistance, low dielectric loss characteristics, and can be a substrate capable of forming a uniform dense film. There is a feature.
  • the content of Al converted to Al 2 O 3 is 70 wt% or more. Further, the content of Zr in terms of ZrO 2 is 30 wt% or less. Furthermore, the content of Y converted into Y 2 O 3 is 1 wt% or more and 10 wt% or less.
  • a crystal phase of ZrO 2 is formed in addition to the main crystal of Al 2 O 3 . The crystal phase of ZrO 2 acts to reduce pores, suppresses abnormal grain growth and has a small particle size, and thus acts to increase high strength.
  • the content of Zr converted to ZrO 2 exceeds 30 wt%, the content of Al converted to Al 2 O 3 becomes less than 70 wt%, and the corrosion resistance is high against highly reactive halogen-based corrosive gases and their plasmas. Is not preferable because it can not be obtained. Further, when the content of Zr in terms of ZrO 2 exceeds 30 wt%, the amount of the crystal phase of ZrO 2 increases, whereby the strength of the aluminous sintered body decreases. Furthermore, it is not preferable because the dielectric loss tangent tan ⁇ exceeds 10 ⁇ 3 .
  • the content of Al converted to Al 2 O 3 is 70 wt% or more, and the content of Zr converted to ZrO 2 is 30 wt% or less.
  • the content of Y converted into Y 2 O 3 is 1 wt% or more and 10 wt% or less.
  • This Y has the effect of suppressing the occurrence of cracks due to the addition of Zr. If the content of Y converted to Y 2 O 3 is less than 1 wt%, the crack suppressing effect is small, and if it exceeds 10 wt%, Y reacts with Al 2 O 3 in the firing process, resulting in YAG Generate When the amount of YAG present is large, the three-point bending strength is reduced, so the content is 10 wt% or less.
  • the content of Y converted to Y 2 O 3 is larger than the content of Zr converted to ZrO 2 , the three-point bending strength decreases, which is not preferable. Therefore, it is preferable that the content that the Y Y 2 O 3 in terms is less than the content of which the Zr ZrO 2 in terms.
  • the components other than Al 2 O 3 , ZrO 2 and Y 2 O 3 contained in the alumina sintered body according to the second embodiment are unavoidably unavoidable in the alumina production process, as in the first embodiment. It is a substance to be mixed, and examples thereof include substances such as Si, Mg, Na, Ca and the like.
  • the content of Si converted to SiO 2 in this alumina sintered body is 170 ppm or more and 600 ppm or less.
  • the content and the Na Na 2 to O terms is less than 27 ppm.
  • Mg content ratio was calculated as MgO, compared content with the Si SiO 2 converted, is preferably 1.0 to 4.0.
  • the content ratio of Ca to CaO in terms of the relative content of which the Si SiO 2 converted, is preferably 3.0 or less.
  • the average crystal grain size of the Al 2 O 3 crystal in the alumina sintered body in the second embodiment is preferably 3 ⁇ m or more and 15 ⁇ m or less, as in the first embodiment.
  • the water absorption rate of the alumina sintered body in the second embodiment is preferably 0.2% or less.
  • the average pore diameter of this alumina sintered body is preferably 5 ⁇ m or less.
  • the alumina sintered body according to the second embodiment may be used by itself, but a dense film is formed on the surface of the alumina sintered body. May be used.
  • This film can be obtained, for example, by depositing an yttria material on the aluminous sintered body using an aerosol deposition method or a PVD method, as in the first embodiment.
  • the water absorption rate is 0.2% or less, the thin film can be formed uniformly.
  • a thin film of yttria can be formed more uniformly on the surface of the alumina sintered body.
  • the film formed on the surface of the alumina sintered body is not limited to the yttria material, and a composite oxide of yttrium oxide and aluminum oxide (YAG), erbium oxide, other rare earth oxides or rare earth oxides It may be a composite oxide containing an oxide.
  • the surface roughness Ra of the surface of the alumina sintered body on which the film is formed be less than 0.1 ⁇ m.
  • the surface of the alumina sintered body may be mirror-polished to have a surface roughness of less than 0.1 ⁇ m. That is, it is desirable that the average pore diameter of the surface of the alumina sintered body on which the film is formed be 5 ⁇ m or less, and the surface roughness Ra be less than 0.1 ⁇ m.
  • the thin film can be formed more uniformly, peeling of the thin film can be suppressed, and generation of particles can be suppressed.
  • the film formed on the surface of the alumina sintered body may be formed on a part of the surface of the alumina sintered body.
  • the film thickness is not particularly limited, but is preferably 1 ⁇ m to 20 ⁇ m.
  • the alumina-based sintered body can be manufactured by a general manufacturing method of the alumina-based sintered body, but for example, it can be manufactured by the following method.
  • a raw material slurry obtained by stirring and mixing the raw material powder with a mixer is granulated.
  • a molded body is produced.
  • various methods such as uniaxial press molding, CIP molding, wet molding, pressure casting and the like can be used.
  • the above-mentioned compact is sintered in a hydrogen atmosphere at a temperature range of 1600 ° C. to 1900 ° C. for 6 hours or more to obtain an aluminous sintered body.
  • the three-point bending strength is 320 MPa or more
  • the average crystal grain diameter of Al 2 O 3 crystal is 3 ⁇ m to 15 ⁇ m
  • the water absorption is 0.2% or less
  • An alumina sintered body of The present alumina-based sintered body can obtain an alumina-based sintered body having a low dielectric loss characteristic which exhibits a dielectric loss tangent tan ⁇ of 10 ⁇ 3 or less at 10 MHz to 20 MHz.
  • the alumina-based sintered body according to the third embodiment is an alumina-based sintered body in which the content of Al converted to Al 2 O 3 is 99.8 wt% or more, and the Si in the alumina-based sintered body is It is characterized in that the content in terms of SiO 2 is 170 ppm or more and 600 ppm or less, the content in terms of Na converted to Na 2 O is 27 ppm or less, and the density of the aluminous sintered body is 3.96 g / cm 3 or more. .
  • the alumina sintered body according to the third embodiment is characterized in that it has corrosion resistance, low dielectric loss characteristics, and a base material capable of forming a uniform dense film.
  • the content of Al converted to Al 2 O 3 in the alumina sintered body of the third embodiment is 99.8 wt% or more. If the content of Al converted to Al 2 O 3 is less than 99.8 wt%, high corrosion resistance to highly reactive halogen-based corrosive gases and their plasmas can not be obtained, which is not preferable.
  • Components other than Al 2 O 3 contained in the alumina sintered body according to the third embodiment are substances which are inevitably mixed in the alumina production process, and for example, substances such as Si, Mg, Na, Ca, etc. It can be mentioned.
  • the content of Si converted to SiO 2 in the alumina sintered body of the third embodiment is 170 ppm or more and 600 ppm or less. If the content of Si converted to SiO 2 is less than 170 ppm, the silicate required for the expression of low dielectric loss characteristics is not uniformly formed, the dielectric loss increases, and the effect of power saving can not be obtained. Not desirable.
  • the density of the aluminous sintered body is small and it is not preferable because it does not become compact.
  • the density of the alumina sintered body according to the third embodiment is 3.96 g / cm 3 or more.
  • the content of Na converted to Na 2 O is 27 ppm or less. If the content of Na converted to Na 2 O exceeds 27 ppm, the dielectric loss increases and the effect of power saving can not be obtained, which is not preferable.
  • the content ratio of Mg converted to MgO is 1.0 or more and 4.0 or less with respect to the content of Si converted to SiO 2.
  • a silicate may be formed at the grain boundary of the aluminous sintered body Since it is possible, an alumina sintered body having high density and low dielectric loss can be obtained.
  • the content ratio of Ca converted to CaO is preferably 3.0 or less with respect to the content converted to Si 2 .
  • To content of Ca content ratio was calculated as CaO and the said Si SiO 2 converted, by more than 3.0, since the silicate is formed in the grain boundary, the low dielectric loss alumina sintered You can get the body.
  • the average crystal grain size of the Al 2 O 3 crystal in the alumina sintered body of the third embodiment is preferably 3 ⁇ m to 40 ⁇ m, and more preferably 10 ⁇ m to 25 ⁇ m.
  • the average crystal grain size of Al 2 O 3 crystals in the alumina-based sintered body is 3 ⁇ m or more and 40 ⁇ m or less, the presence of pores of the alumina-based sintered body can be reduced, and a sintered body with higher density can be obtained.
  • an alumina sintered body having a three-point bending strength of 250 MPa or more can be obtained.
  • the average pore diameter of the alumina sintered body of the third embodiment is 5 ⁇ m or less. When the average pore diameter of the alumina sintered body is 5 ⁇ m or less, a thin film can be uniformly formed on the surface of the alumina sintered body.
  • the alumina-based sintered body according to the third embodiment may be used by itself, but may be one having a dense film formed on the surface of the alumina-based sintered body.
  • This film is obtained, for example, by depositing yttria material on the aluminous sintered body using an aerosol deposition method or a PVD method.
  • the alumina-based sintered body in which the yttria material is formed into a film as described above has high plasma resistance, is excellent in low dusting property, and can achieve power saving and the like due to the low dielectric loss characteristics of the base material.
  • a thin film of yttria can be uniformly formed on the surface of the alumina sintered body.
  • the film formed on the surface of the alumina sintered body is not limited to the yttria material, and a composite oxide of yttrium oxide and aluminum oxide (YAG), erbium oxide, other rare earth oxides or rare earth oxides It may be a composite oxide containing an oxide.
  • the surface of the alumina sintered body may be mirror-polished to have a surface roughness of less than 0.1 ⁇ m. That is, it is desirable that the average pore diameter of the surface of the alumina sintered body on which the film is formed be 5 ⁇ m or less, and the surface roughness Ra be less than 0.1 ⁇ m.
  • the thin film can be formed more uniformly, peeling of the thin film can be suppressed, and generation of particles can be suppressed.
  • the film formed on the surface of the alumina sintered body may be formed on a part of the surface of the alumina sintered body.
  • the film thickness is not particularly limited, but is preferably 1 ⁇ m to 20 ⁇ m.
  • an alumina-based sintered body can be manufactured by the general manufacturing method of an alumina-based sintered body, if an example is given, it can be manufactured by the following method.
  • a binder or the like for example, PVA
  • PVA PVA
  • Al 2 O 3 powder having a predetermined median diameter to prepare a raw material powder.
  • a raw material slurry obtained by stirring and mixing the raw material powder with a mixer is granulated.
  • a molded body is produced.
  • various methods such as uniaxial press molding, CIP molding, wet molding, pressure casting and the like can be used.
  • the above-mentioned compact is sintered in a hydrogen atmosphere at a temperature range of 1600 ° C. to 1900 ° C. for 6 hours or more to obtain an aluminous sintered body.
  • a high density alumina sintered body can be obtained.
  • Example 1A As shown in Table 1, ZrO 2 powder was added to alumina powder having a median diameter of 2 ⁇ m or less using water as a solvent, and PVA was added to prepare a raw material powder. Then, the raw material powder was stirred and mixed for 16 hours or more to obtain a raw material slurry. And this raw material slurry was granulated, the granulated powder was filled in the shaping
  • the average crystal grain size of the alumina crystal particles was obtained by mirror-polishing a sample cross section and performing thermal etching, then taking a cross-sectional photograph with a scanning electron microscope (SEM) and calculating the image by image analysis.
  • SEM scanning electron microscope
  • the cross-sectional photograph by the scanning electron microscope (SEM) in Example 1A is shown in FIG.
  • the three-point bending strength was measured in accordance with JIS R 1601: 2008, and the sintered body purity was measured by ICP emission analysis.
  • the dielectric loss tangent tan ⁇ measurement at a frequency of 10 MHz to 20 MHz was measured using an impedance analyzer.
  • the surfaces of the samples (alumina sintered bodies) of Examples 1A to 7A and Comparative Examples 1A to 6A obtained above were mirror-polished to Ra ⁇ 0.1 ⁇ m, and aerosol deposition was performed on the polished surface.
  • the yttrium oxide material was coated 1 ⁇ m using the method.
  • the film formation performed drying for 12 hours or more at 270 degreeC as pre-processing of the film-forming material, and performed aerosol injection on condition of the following.
  • Examples 1A to 7A show three-point bending strength of 320 MPa or more and tan ⁇ of less than 10 -3 , average crystal grain size of alumina crystal particles is 3 ⁇ m to 15 ⁇ m, and water absorption coefficient is 0.2 %, It was confirmed that the sintered body was an alumina sintered body having high strength, high density, and low dielectric loss characteristics. In addition, as shown in FIG. 1, it can be recognized that ZrO 2 crystal particles having a small diameter enter between alumina crystal particles, thereby suppressing the presence of pores.
  • the number of voids in a range of about 200 ⁇ m ⁇ 200 ⁇ m on the thin film surface is 100 or less, and the average diameter is 5 ⁇ m or less, and a uniform film can be formed.
  • Comparative Example 3A since the Si content is large, the three-point bending strength is small, and the average grain size of Al 2 O 3 crystals in the aluminous sintered body is large, and the surface of the aluminous sintered body is large. It has proved difficult to form a uniform film.
  • Comparative Example 4A since the contents of Si and Na were large, the three-point bending strength was small, and tan ⁇ exceeded 10 ⁇ 3 . It was also found that the average grain size of Al 2 O 3 crystals in the alumina-based sintered body was large, and it was difficult to form a uniform film on the surface of the alumina-based sintered body.
  • Comparative Example 5A it was found that it is difficult to form a uniform film on the surface of the aluminous sintered body, because tan ⁇ is more than 10 -3 because the Si content is small.
  • Example 2A Next, as shown in Table 2, using water as a solvent, ZrO 2 powder and Y 2 O 3 powder were added to alumina powder having a median diameter of 2 ⁇ m or less, and PVA was added to prepare a raw material powder. Then, the raw material powder was stirred and mixed for 16 hours or more to obtain a raw material slurry. And this raw material slurry was granulated, the granulated powder was filled in the shaping
  • the surfaces of the samples (alumina sintered bodies) of Examples 8A to 12A and Comparative Examples 7A and 8A obtained above were mirror-polished to Ra ⁇ 0.1 ⁇ m, and polished surfaces
  • the yttrium oxide material was coated to 1 ⁇ m using an aerosol deposition method.
  • film-forming the drying for 12 hours or more was performed at 270 degreeC as pre-processing of the film-forming material, and the aerosol injection was performed on the conditions same as Example 1A.
  • Examples 8A to 12A exhibit a three-point bending strength of 320 MPa or more and a tan ⁇ of less than 10 ⁇ 3 , an average crystal grain size of alumina crystal particles of 4 ⁇ m to 10 ⁇ m, and a water absorption of 0.2 %, It was confirmed that the sintered body was an alumina sintered body having high strength, high density, and low dielectric loss characteristics. In addition, it was confirmed that the number of voids in a range of about 200 ⁇ m ⁇ 200 ⁇ m on the thin film surface is 100 or less, and the average diameter is 5 ⁇ m or less, and a uniform film can be formed.
  • Comparative Examples 7A and 8A since the content of Y is large, the average grain size of Al 2 O 3 crystals in the alumina sintered body is large, and the alumina sintered body having small three-point bending strength It turned out to be.
  • Example 1B As shown in Table 3, PVA was added to alumina powder having a purity of 99.7 wt% to 99.9 wt% and a median diameter of 2 ⁇ m or less to prepare a raw material powder. Then, the raw material powder was stirred and mixed for 16 hours or more to obtain a raw material slurry. And this raw material slurry was granulated, the granulated powder was filled in the shaping
  • Example 1B to 4B, 7B, Comparative Examples 1B to 4B 1700 ° C.
  • Example 5B, Comparative Example 5B 1900
  • Each sample of Examples 1B to 7B and Comparative Examples 1B to 6B was manufactured by baking at ° C. (Example 6B, Comparative Example 6B).
  • Si in the sintered body the respective content of Na was added SiO 2, Na 2 O to be in the range of the present invention as needed. Further, the median diameter of the alumina powder was changed so that the density of the sintered body was within the range of the present invention.
  • the density was measured in accordance with JIS R 1634: 1998 in Experiment 1B and Experiments 2B to 4B described below. Also, tan ⁇ measurement at a frequency of 10 MHz to 20 MHz was measured using an impedance analyzer. Furthermore, the average crystal grain size of the alumina crystal particles was calculated by mirror image polishing of the sample cross section and thermal etching, then taking a cross-sectional photograph with a scanning electron microscope (SEM) and image analysis. The three-point bending strength was measured in accordance with JIS R 1601: 2008, and the sintered body purity was measured by ICP emission analysis.
  • SEM scanning electron microscope
  • the surfaces of the samples (alumina sintered bodies) of Examples 1B to 7B and Comparative Examples 1B to 6B obtained above were mirror-polished to Ra ⁇ 0.1 ⁇ m, and aerosol deposition was performed on the polished surface.
  • the yttrium oxide material was coated 1 ⁇ m using the method.
  • the film formation performed drying for 12 hours or more at 270 degreeC as pre-processing of the film-forming material, and performed aerosol injection on condition of the following.
  • the surfaces of the samples of Examples 1B to 7B and Comparative Examples 1B to 6B on which the thin films obtained above were formed were observed in the range of about 200 ⁇ m ⁇ 200 ⁇ m using a scanning electron microscope, and the obtained images were obtained.
  • the diameter and number of voids were measured using image analysis software. Then, as described in Table 3, when the number of voids satisfies 100 or less, uniform film formation was performed as A, and when not satisfying, B as uneven film formation.
  • AA was added when the average diameter of the voids was 5 ⁇ m or less and the number of voids was less than 80. Therefore, the number of voids in A is 80 or more and 100 or less.
  • the criteria for the notation of AA, A, and B are the same as in Tables 4 to 6 below.
  • each of Examples 1B to 7B is an alumina sintered body having a density of 3.96 g / cm 3 or more, a tan ⁇ of less than 10 -3 and having a low dielectric loss characteristic. confirmed.
  • Comparative Example 1B the density was less than 3.96 g / cm 3 because the content of Na was high. Also, tan ⁇ exceeded 10 -3 . As a result, it was found that the compactness and dielectric loss characteristics were inferior.
  • Comparative Example 3B the Si content was large, and the density was less than 3.96 g / cm 3 . That is, it was found that this alumina sintered body is inferior in compactness.
  • Comparative Example 4B densification was inhibited due to the excessive Si content, and the density was less than 3.96 g / cm 3 . That is, it was found that this alumina-based sintered body was inferior in compactness, and it was difficult to form a dense film on the surface of the alumina-based sintered body.
  • Comparative Example 5B the alumina purity was low, the density was less than 3.96 g / cm 3 , and tan ⁇ was more than 10 ⁇ 3 . That is, it was found that this alumina-based sintered body is inferior in compactness.
  • Comparative Example 6B the alumina purity was low, the density was less than 3.96 g / cm 3 , and tan ⁇ was more than 10 ⁇ 3 . That is, it was found that this alumina-based sintered body is inferior in compactness.
  • the surface condition of the thin film formed in each sample of Examples 1B to 7B and Comparative Example 2B is that the average diameter of the voids is 5 ⁇ m or less, and the number of voids is 100 or less (less than 80) in the range of about 200 ⁇ m ⁇ 200 ⁇ m. It turned out that a uniform film can be formed.
  • Example 2B PVA was added to an alumina powder having a purity of 99.8 wt% to 99.9 wt% and a median diameter of 2 ⁇ m or less to prepare a raw material powder. Then, the raw material powder was stirred and mixed for 16 hours or more to obtain a raw material slurry. And this raw material slurry was granulated, the granulated powder was filled in the shaping
  • Each of the samples of Examples 8B, 10B, 12B, and 14B was manufactured by firing the molded body at 1900 ° C. in a hydrogen atmosphere through a degreasing process in an air atmosphere.
  • SiO 2 and Na 2 O are added so that the content of each of Si and Na in the sintered body falls within the range of the present invention
  • the content ratio of Mg converted to MgO is MgO is added so as to be 0.9 or more and 4.1 or less with respect to the content obtained by converting the Si into SiO 2, and the median diameter of the alumina powder such that the density of the sintered body falls within the range of the present invention Changed.
  • Example 8B, 9B, 12B, as shown in 13B the density of the sintered body is 3.99 g / cm 3, and 4.00 g / cm 3, that the higher density of the sintered body is obtained found.
  • the surfaces of the samples (alumina sintered bodies) of Examples 8B to 15B were mirror-polished to Ra ⁇ 0.1 ⁇ m, and the polished surfaces were oxidized using an aerosol deposition method.
  • the yttrium material was coated 1 ⁇ m, and the state of the thin film surface was observed.
  • Table 4 the surface condition of the thin film formed in each sample of Examples 8B to 15B was that the average diameter of the voids was 5 ⁇ m or less, and the number of voids was 100 or less (about 80 or less) in the range of about 200 ⁇ m ⁇ 200 ⁇ m. ) And was found to be able to form a uniform film.
  • Example 3B Next, as shown in Table 5, PVA was added to an alumina powder having a purity of 99.8 wt% to 99.9 wt% and a median diameter of 2 ⁇ m or less to prepare a raw material powder. Then, the raw material powder was stirred and mixed for 16 hours or more to obtain a raw material slurry. And this raw material slurry was granulated, the granulated powder was filled in the shaping
  • Example 16B, 17B, 18B, and 19B were evaluated. Further, Example 8B described above, 10B, 12B, were also evaluated an average grain size and three-point bending strength of Al 2 O 3 crystals of each sample 14B. The results are shown in Table 5.
  • the average crystal grain size of the alumina crystal particles was calculated by mirror image polishing of the sample cross section and thermal etching, then taking a cross-sectional photograph with a scanning electron microscope (SEM) and image analysis.
  • SEM scanning electron microscope
  • the three-point bending strength was measured in accordance with JIS R 1601: 2008, and the sintered body purity was measured by ICP emission analysis. As a result, as shown in Examples 8B and 16B and Examples 12B and 18B of Table 5, the sintered body has a density of 3.97 g / cm 3 or more and a three-point bending strength of 250 MPa or more. Was found to be obtained.
  • the surfaces of the samples (alumina sintered bodies) of Examples 16B to 19B were mirror-polished to Ra ⁇ 0.1 ⁇ m, and yttrium oxide was applied to the polished surface using an aerosol deposition method.
  • the material was coated at 1 ⁇ m and the state of the thin film surface was observed.
  • Table 5 As shown in Table 5, in the surface state of the thin film formed on each sample of Examples 16B and 18B, the average diameter of the voids is 5 ⁇ m or less, and the number of voids is 100 or less (less than 80) in the range of about 200 ⁇ m ⁇ 200 ⁇ m. ) And was found to be able to form a uniform film.
  • the surface condition of the thin film formed on each sample of Examples 17B and 19B is that the average diameter of the voids is 5 ⁇ m or less, and the number of voids in the range of about 200 ⁇ m ⁇ 200 ⁇ m is 80 or more and 100 or less. It turned out that it could form.
  • Example 4B PVA was added to alumina powder having the same alumina purity and median diameter as in Example 18B to prepare a raw material powder. Then, the raw material powder was stirred and mixed for 16 hours or more to obtain a raw material slurry. And this raw material slurry was granulated, the granulated powder was filled in the shaping
  • the surface state of the thin film formed in each sample of Examples 18B and 20B to 22B was 100 ⁇ m or less in the average diameter of the voids of 5 ⁇ m or less, and about 200 ⁇ m ⁇ 200 ⁇ m. It was found that (less than 80 pieces), a uniform film could be formed.
  • the present invention is used for constituent members of a manufacturing apparatus of a semiconductor manufacturing field, a liquid crystal display device manufacturing field, and the like.
  • a plasma processing apparatus an etcher for manufacturing a semiconductor / liquid crystal display apparatus, a member used for a CVD apparatus and the like.
  • the alumina sintered body according to the present invention may be used by itself, or alternatively, using the alumina sintered body as a substrate, a plasma resistant corrosion resistant film or layer is formed on all or part of the surface. And may be used as a plasma resistant member.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
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  • Composite Materials (AREA)
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Abstract

La présente invention concerne un corps en alumine frittée et son procédé de fabrication ; par exemple, la présente invention concerne un corps en alumine frittée qui est utilisé de manière appropriée pour un élément ou similaire utilisé dans un dispositif de traitement au plasma, un dispositif de gravure pour la fabrication de dispositif d'affichage à cristaux liquides/semi-conducteurs, un dispositif CVD, ou équivalents, ou qui est utilisé de manière appropriée pour un substrat ou équivalents d'un élément résistant au plasma qui doit être revêtu. La présente invention concerne en outre un procédé de fabrication dudit corps en alumine frittée.
PCT/JP2018/036914 2017-10-05 2018-10-02 Corps en alumine frittée et procédé de fabrication associé WO2019069939A1 (fr)

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CN201880065428.0A CN111201208B (zh) 2017-10-05 2018-10-02 氧化铝质烧结体及其制造方法
US16/753,756 US11760694B2 (en) 2017-10-05 2018-10-02 Alumina sintered body and manufacturing method therefor
KR1020207009705A KR102354650B1 (ko) 2017-10-05 2018-10-02 알루미나질 소결체 및 그의 제조 방법

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JP2018178652A JP7154912B2 (ja) 2017-10-05 2018-09-25 アルミナ質焼結体及びその製造方法
JP2018-178652 2018-09-25
JP2018180299A JP7231367B2 (ja) 2018-09-26 2018-09-26 アルミナ質焼結体
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05217946A (ja) * 1992-01-31 1993-08-27 Toshiba Ceramics Co Ltd アルミナ質ベルジヤ−
JPH08143358A (ja) * 1994-11-18 1996-06-04 Kyocera Corp アルミナ質焼結体
JP2000072529A (ja) * 1998-08-26 2000-03-07 Toshiba Ceramics Co Ltd 耐プラズマ部材およびそれを用いたプラズマ処理装置
JP2001240461A (ja) * 2000-02-29 2001-09-04 Kyocera Corp アルミナ質耐食部材及びプラズマ装置
JP2004217478A (ja) * 2003-01-15 2004-08-05 Ngk Insulators Ltd 複合焼結体およびその製造方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005225745A (ja) 2004-01-16 2005-08-25 Toshiba Ceramics Co Ltd 耐プラズマ部材及びその製造方法
JP2013095973A (ja) 2011-11-02 2013-05-20 Tocalo Co Ltd 半導体製造装置用部材
JP5928694B2 (ja) 2012-01-31 2016-06-01 日本特殊陶業株式会社 アルミナ質焼結体及びその製造方法
JP5930380B2 (ja) 2012-02-29 2016-06-08 日本特殊陶業株式会社 アルミナ質焼結体及びその製造方法
JP6352686B2 (ja) 2014-01-30 2018-07-04 京セラ株式会社 アルミナ質焼結体および半導体製造装置用部材ならびに液晶パネル製造装置用部材

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05217946A (ja) * 1992-01-31 1993-08-27 Toshiba Ceramics Co Ltd アルミナ質ベルジヤ−
JPH08143358A (ja) * 1994-11-18 1996-06-04 Kyocera Corp アルミナ質焼結体
JP2000072529A (ja) * 1998-08-26 2000-03-07 Toshiba Ceramics Co Ltd 耐プラズマ部材およびそれを用いたプラズマ処理装置
JP2001240461A (ja) * 2000-02-29 2001-09-04 Kyocera Corp アルミナ質耐食部材及びプラズマ装置
JP2004217478A (ja) * 2003-01-15 2004-08-05 Ngk Insulators Ltd 複合焼結体およびその製造方法

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