WO2018034422A1 - Composite de mandrin sous vide et procédé de préparation correspondant - Google Patents

Composite de mandrin sous vide et procédé de préparation correspondant Download PDF

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WO2018034422A1
WO2018034422A1 PCT/KR2017/006616 KR2017006616W WO2018034422A1 WO 2018034422 A1 WO2018034422 A1 WO 2018034422A1 KR 2017006616 W KR2017006616 W KR 2017006616W WO 2018034422 A1 WO2018034422 A1 WO 2018034422A1
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weight
parts
asf
alumina
composite
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PCT/KR2017/006616
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Korean (ko)
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김종영
조우석
최광민
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한국세라믹기술원
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0038—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter

Definitions

  • the present invention relates to a vacuum chuck composite and a method for manufacturing the same, more specifically Al 2 O 3 , SiO 2 Since the carbon-based material is dispersed in the ceramic material, the electrical resistance is reduced, and thus it has an antistatic function, excellent mechanical properties, porosity, simple manufacturing process without complicated manufacturing process, and low manufacturing vacuum
  • the present invention relates to a chuck complex and a method of manufacturing the same.
  • the manufacturing process of a semiconductor device includes a process of forming or stacking a pattern on dozens of different kinds of layers.
  • the patterns formed on each layer should be formed as designed and perform the intended electrical operation.
  • a small amount of triboelectric static electricity is generated when the wafer or glass that has been adsorbed and fixed on a fixing chuck of a semiconductor wafer or liquid crystal display (LCD) glass is separated.
  • LCD liquid crystal display
  • Patterns printed on semiconductor wafers and display substrates are being miniaturized, so that static electricity generated in the process of mounting and separating semiconductor wafers and display substrates onto porous ceramic substrates is charged to electronic components such as semiconductor devices integrated on semiconductor wafers and display substrates.
  • defects such as a short circuit of the printed pattern or a process of separating the wafer and the display substrate from the chuck frequently cause cracks in the wafer due to static electricity.
  • the antistatic work stage is coated with a carbon nanotube coating on the stage of the metal material to minimize the generation of static electricity on the surface meeting the substrate of the stage.
  • Carbon nanotube coating stage is to prevent the antistatic by applying a conductive carbon nanotube coating film on the stage body through a separate coating process of a metal material such as aluminum rather than a porous ceramic.
  • Korean Patent Laid-Open Publication No. 10-2010-0121895 'Substrate having an antistatic function and a manufacturing method thereof' has an antistatic function by crystallizing a titanium dioxide (TiO 2 ) doped with impurities in a base layer made of a glass material. It is characterized by one.
  • Korean Patent Application Publication No. 10-2010-0121895 discloses a glass material base, which is similar to an antistatic work stage described above, in which the base body is a glass material and undergoes a separate deposition and heat treatment process. An antistatic layer is formed on the layer.
  • the antistatic coating stage on the carbon nanotube coating and the glass material is complicated in manufacturing process and takes a lot of manufacturing cost, and if the carbon nanotube coating film coated on the stage body is damaged, the entire stage needs to be replaced.
  • the carbon nanotube coating and the antistatic coating stage on the glass material have a limitation in adsorbing a large area of thin wafer or display glass since a sealed coating film is formed on the upper surface of the main body.
  • the problem to be solved by the present invention Al 2 O 3 , SiO 2 Since the carbon-based material is dispersed in the ceramic material, the electrical resistance is reduced, and thus it has an antistatic function, excellent mechanical properties, porosity, simple manufacturing process without complicated manufacturing process, and low manufacturing vacuum
  • the present invention provides a chuck complex and a method of manufacturing the same.
  • the present invention provides a vacuum chuck composite comprising 75 to 93% by weight of alumina, 7 to 25% by weight of silica, and 0.01 to 5 parts by weight of carbonaceous material based on 100 parts by weight of the total content of the alumina and the silica.
  • the vacuum chuck composite may further include 0.5 to 6.5 parts by weight of Fe ⁇ Co-based oxide based on 100 parts by weight of the total content of the alumina and the silica.
  • the Fe ⁇ Co-based oxide may include Fe 2 O 3 , Co 3 O 4, and Mn-based compounds as chemical components.
  • the Fe-Co oxide may include 24 to 34% by weight of Fe 2 O 3, 10 to 18% by weight of Co 3 O 4, and 50 to 64% by weight of Mn-based compound.
  • the vacuum chuck composite may further include 0.01 to 5 parts by weight of frit based on 100 parts by weight of the total content of the alumina and the silica.
  • the carbon-based material may include at least one material selected from graphene oxide, graphene, and graphite.
  • the present invention (a) 75 to 93% by weight of alumina powder and 7 to 25% by weight of silica powder to form a first slurry, (b) drying the first slurry to alumina-silica powder Forming a second slurry by mixing a carbonaceous material with the alumina-silica powder, (d) drying the second slurry to form a composite powder, and (e) ) (F) sintering the molded product, and (c) mixing 0.01 to 5 parts by weight of the carbonaceous material with respect to 100 parts by weight of the alumina-silica powder. It provides a method for producing a composite for vacuum chuck, characterized in that.
  • 0.5 to 6.5 parts by weight of Fe ⁇ Co-based oxide may be further mixed with respect to 100 parts by weight of the total content of the alumina powder and the silica powder.
  • the Fe ⁇ Co-based oxide may include Fe 2 O 3 , Co 3 O 4, and Mn-based compounds as chemical components.
  • the Fe-Co oxide may include 24 to 34% by weight of Fe 2 O 3, 10 to 18% by weight of Co 3 O 4, and 50 to 64% by weight of Mn-based compound.
  • frit 0.01 to 5 parts by weight of frit may be further mixed with respect to 100 parts by weight of the alumina-silica powder.
  • the carbon-based material may include at least one material selected from graphene oxide, graphene, and graphite.
  • the dispersing agent and the binder may be further mixed in the step (a), the dispersing agent is preferably mixed 0.01 to 3 parts by weight based on 100 parts by weight of the total content of the alumina powder and the silica powder, the binder is the alumina It is preferable to mix 3-15 weight part with respect to 100 weight part of total content of a powder and the said silica powder.
  • the dispersant may include polycarboxylate ammonium.
  • the binder may include polyvinyl alcohol.
  • the sintering is preferably carried out at a temperature of 1200 ⁇ 1600 °C by supplying nitrogen or argon gas in a reducing furnace.
  • the carbon-based material is dispersed in the ceramic material, the electrical resistance is reduced, thereby having an antistatic function, excellent mechanical properties, porosity, manufacturing process is not complicated, simple manufacturing, and low manufacturing cost.
  • FIG. 1 is a view showing an X-ray diffraction (XRD) pattern of the sintered body prepared according to the experimental examples.
  • XRD X-ray diffraction
  • FIG. 2 is a scanning electron microscope (SEM) image of an ASF sintered body (in an atmosphere, Ar atmosphere, 1500 ° C.), showing a microstructure magnified 1000 times
  • FIG. 3 is an ASF sintered body (reducing element, N 2 atmosphere, 1500 ° C.). Scanning electron microscopy (SEM) of shows microstructure magnified 5000 times.
  • FIG. 4 is a scanning electron microscope (SEM) image of an ASF sintered body (in an atmosphere, Ar atmosphere, 1250 ° C.) and shows a microstructure magnified 1000 times.
  • FIG. 5 is an ASF sintered body (reducing element, N 2 atmosphere, 1250 ° C.). Scanning electron microscopy (SEM) of shows microstructure magnified 5000 times.
  • FIG. 6 is a scanning electron microscope (SEM) image of an ASF sintered body (reducing furnace, N 2 atmosphere, 1250 ° C.), showing a microstructure magnified 1000 times
  • FIG. 9 is an ASF sintered body (reducing firing furnace, N 2 atmosphere, 1250 ° C.). Scanning electron microscopy (SEM) photograph of) shows the microstructure magnified 5000 times.
  • FIG. 8 is a scanning electron microscope (SEM) image of an ASF sintered body (reducing furnace, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times
  • FIG. 9 is an ASF sintered body (reducing furnace, N 2 atmosphere, 1300 ° C.). Scanning electron microscopy (SEM) photograph of) shows the microstructure magnified 5000 times.
  • FIG. 10 is a graph showing the density of the ASF sintered body according to the sintering conditions.
  • FIG. 11 is a graph showing the surface resistance of the ASF sintered body according to the sintering conditions.
  • FIG. 13 is a graph showing density of ASF / GO and ASF / EG sintered bodies according to sintering conditions.
  • FIG. 14 is a graph showing the surface resistance of the ASF / GO, ASF / EG sintered body according to the sintering conditions.
  • 15 is a graph showing the density of ASF / SC sintered compact according to the sintering conditions.
  • 16 is a graph showing the surface resistance of the ASF / SC sintered body according to the sintering conditions.
  • 17 is a graph showing the strength of the ASF / SC sintered body according to the sintering conditions.
  • FIG. 18 is a scanning electron microscope (SEM) photograph of an ASF / SC (0.5 wt%) / Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 19 is a scanning electron microscope (SEM) photograph of an ASF / SC (0.5 wt%) / Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a magnification of 5000 times.
  • 20 is a scanning electron microscope (SEM) image of an ASF / SC (0.5 wt%) / Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times.
  • 21 is a scanning electron microscope (SEM) photograph of an ASF / SC (0.5 wt%) / Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a magnification of 5000 times.
  • FIG. 22 is a scanning electron microscope (SEM) photograph of an ASF / SC (0.5 wt%) / Frit (2.0 wt%) sintered body (reduction element furnace, N 2 atmosphere, 1200 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 23 is a scanning electron microscope (SEM) image of an ASF / SC (0.5 wt%) / Frit (2.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a magnification of 5000 times.
  • FIG. 24 is a scanning electron microscope (SEM) photograph of an ASF / SC (0.5 wt%) / Frit (2.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 25 is a scanning electron microscope (SEM) image of an ASF / SC (0.5 wt%) / Frit (2.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a magnification of 5000 times.
  • FIG. 26 is a scanning electron microscope (SEM) image of an ASF / SC (0.5 wt%) / Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 27 is a scanning electron microscope (SEM) image of an ASF / SC (0.5 wt%) / Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a magnification of 5000 times.
  • FIG. 28 is a scanning electron microscope (SEM) image of an ASF / SC (0.5 wt%) / Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 29 shows a scanning electron microscope (SEM) image of an ASF / SC (0.5 wt%) / Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), and shows a magnification of 5000 times.
  • FIG. 30 is a graph showing the density of the ASF / SC (0.5 wt%) / Fri sintered body according to the sintering conditions.
  • FIG. 31 is a graph showing the surface resistance of the ASF / SC (0.5 wt%) / Fri sintered body according to the sintering conditions.
  • 35 is a graph showing the strength of the ASF / SC (3.0 wt%) / Fri sintered body according to the sintering conditions.
  • the vacuum chuck composite according to a preferred embodiment of the present invention includes 75 to 93% by weight of alumina, 7 to 25% by weight of silica, and 0.01 to 5 parts by weight of carbonaceous material based on 100 parts by weight of the total content of the alumina and the silica. .
  • Method for producing a composite for vacuum chuck comprises the steps of (a) mixing 75 to 93% by weight of alumina powder and 7 to 25% by weight of silica powder to form a first slurry, and (b) the Drying the first slurry to form an alumina-silica powder, (c) mixing a carbon-based material with the alumina-silica powder to form a second slurry, and (d) drying the second slurry Forming a composite powder, (e) molding the composite powder, and (f) sintering the molded product, wherein in step (c), 100 parts by weight of the alumina-silica powder is used. 0.01-5 weight part of carbonaceous materials are mixed.
  • the vacuum chuck composite according to a preferred embodiment of the present invention includes 75 to 93% by weight of alumina, 7 to 25% by weight of silica, and 0.01 to 5 parts by weight of carbonaceous material based on 100 parts by weight of the total content of the alumina and the silica. .
  • the vacuum chuck composite may further include 0.5 to 6.5 parts by weight of Fe ⁇ Co-based oxide based on 100 parts by weight of the total content of the alumina and the silica.
  • the Fe ⁇ Co-based oxide may include Fe 2 O 3 , Co 3 O 4, and Mn-based compounds as chemical components.
  • the Fe-Co oxide may include 24 to 34% by weight of Fe 2 O 3, 10 to 18% by weight of Co 3 O 4, and 50 to 64% by weight of Mn-based compound.
  • the vacuum chuck composite may further include 0.01 to 5 parts by weight of frit based on 100 parts by weight of the total content of the alumina and the silica.
  • the carbon-based material may include at least one material selected from graphene oxide, graphene, and graphite.
  • Method for producing a composite for vacuum chuck comprises the steps of (a) mixing 75 to 93% by weight of alumina powder and 7 to 25% by weight of silica powder to form a first slurry, and (b) the Drying the first slurry to form an alumina-silica powder, (c) mixing a carbon-based material with the alumina-silica powder to form a second slurry, and (d) drying the second slurry Forming a composite powder, (e) molding the composite powder, and (f) sintering the molded product, wherein in step (c), 100 parts by weight of the alumina-silica powder is used. 0.01-5 weight part of carbonaceous materials are mixed.
  • 0.5 to 6.5 parts by weight of Fe ⁇ Co-based oxide may be further mixed with respect to 100 parts by weight of the total content of the alumina powder and the silica powder.
  • the Fe ⁇ Co-based oxide may include Fe 2 O 3 , Co 3 O 4, and Mn-based compounds as chemical components.
  • the Fe-Co oxide may include 24 to 34% by weight of Fe 2 O 3, 10 to 18% by weight of Co 3 O 4, and 50 to 64% by weight of Mn-based compound.
  • frit 0.01 to 5 parts by weight of frit may be further mixed with respect to 100 parts by weight of the alumina-silica powder.
  • the carbon-based material may include at least one material selected from graphene oxide, graphene, and graphite.
  • the dispersing agent and the binder may be further mixed in the step (a), the dispersing agent is preferably mixed 0.01 to 3 parts by weight based on 100 parts by weight of the total content of the alumina powder and the silica powder, the binder is the alumina It is preferable to mix 3-15 weight part with respect to 100 weight part of total content of a powder and the said silica powder.
  • the dispersant may include polycarboxylate ammonium.
  • the binder may include polyvinyl alcohol.
  • the sintering is preferably carried out at a temperature of 1200 ⁇ 1600 °C by supplying nitrogen or argon gas in a reducing furnace.
  • Alumina (Alumina, Al 2 O 3 ) powder and silica (Silica, SiO 2 ) powder are mixed to form a first slurry.
  • the said alumina powder has an average particle diameter of 50 nm-20 micrometers. It is preferable that the said silica powder has an average particle diameter of 50 nm-20 micrometers.
  • the Fe-Co oxide may be an oxide including Fe 2 O 3 , Co 3 O 4, and a Mn-based compound as a chemical component.
  • the Fe-Co oxide may include 24 to 34% by weight of Fe 2 O 3, 10 to 18% by weight of Co 3 O 4, and 50 to 64% by weight of Mn-based compound.
  • the Mn-based compound may be an Mn-based carbonate such as MnCO 3 , an Mn-based oxide such as MnO 2 , an Mn-based acetate such as Mn (CH 3 CO 2 ) 2 , or the like.
  • transition metal oxides such as Fe, Co, and Mn
  • electrical resistance can be reduced to provide an antistatic function.
  • the MnCO 3 , Mn (CH 3 CO 2 ) 2, etc. are changed to Mn-based oxides (eg, MnO 2 , Mn 3 O 4 , MnO, etc.) in the sintering process described later. It is preferable that the said Fe-Co oxide powder has an average particle diameter of 50 nm-20 micrometers.
  • the dispersant and the binder may be further mixed.
  • the dispersing agent is preferably mixed 0.01 to 3 parts by weight based on 100 parts by weight of the total content of the alumina powder and the silica powder
  • the binder is 3 to 15 parts by weight based on 100 parts by weight of the total content of the alumina powder and the silica powder. It is preferable to mix the weight parts.
  • the dispersant may include polycarboxylate ammonium.
  • the binder may include polyvinyl alcohol.
  • the first slurry preferably has a solid content (eg, the alumina powder and the silica powder) of about 50 to 70% in the solvent.
  • the solvent may be methanol, alcohol such as ethanol, distilled water, or the like.
  • the mixing may use a variety of methods such as a ball mill, planetary mill, attrition mill and the like.
  • the mixing process by a ball mill method is demonstrated concretely, for example.
  • the starting material including the alumina powder and the silica powder is charged and mixed with a solvent in a ball milling machine.
  • the starting material is mixed evenly by rotating at a constant speed using a ball mill.
  • the ball used in the ball mill may use a ball made of ceramics such as alumina and zirconia, and the balls may be all the same size or may be used with balls having two or more sizes. Mix by adjusting the size of the ball, milling time, revolution per minute of the ball mill, etc.
  • the size of the ball can be set in the range of about 1 to 50 mm, and the rotational speed of the ball mill can be set in the range of about 100 to 500 rpm.
  • the ball mill is preferably carried out for 1 to 48 hours in consideration of the target particle size and the like.
  • the first slurry is dried to form alumina-silica powder.
  • the drying may use a spray dryer. For example, it drys using a spray dryer on the conditions of 150-210 degreeC of hot air temperatures, 60-100 degreeC of air blowing temperatures, 5000-10000 rpm of disk rotation speeds, and 0.01-2 L / min of 1st slurry input amount.
  • the spray dry process can make alumina-silica powder into a spherical shape, pumping the slurry with a hose and feeding it onto a circular disk that rotates in the chamber, allowing the slurry to scatter towards the edge of the chamber by centrifugal force.
  • the slurry is dried to obtain a granular powder.
  • the dried powder may be classified through a sieve and again subjected to a drying process.
  • the carbon-based material is mixed with the alumina-silica powder to form a second slurry.
  • frit 0.01 to 5 parts by weight of frit may be further mixed with respect to 100 parts by weight of the alumina-silica powder.
  • the carbon-based material may include at least one material selected from graphene oxide, graphene, and graphite.
  • the graphene may be made of a single layer, a double layer or a multi-layered form.
  • the graphene is used to include graphene oxide (rGO) as well as graphene, which generally means.
  • the addition of the carbonaceous material can increase the electrical conductivity of the composite for vacuum chuck.
  • mechanical properties and physical properties of the vacuum chuck composite may be improved. Al 2 O 3 , SiO 2
  • the second slurry preferably has a content of solids in the solvent of about 50 to 70%.
  • the solvent may be methanol, alcohol such as ethanol, distilled water, or the like.
  • the second slurry is dried to form a composite powder.
  • the drying is preferably carried out in an oven at a temperature of 60 to 150 °C for 1 to 48 hours.
  • the composite powder is molded.
  • the molding can be done in a variety of ways.
  • the composite powder may be charged into a mold and subjected to uniaxial press molding.
  • the molded result is sintered.
  • the sintering is preferably performed at a temperature of 1200 to 1600 ° C. by supplying a gas such as nitrogen (N 2 ) or argon (Ar) in a reducing furnace.
  • the sintering is preferably performed for 10 minutes to 48 hours.
  • the water, the dispersant, and the binder inside the molded body (molded product) are burned out and disappeared.
  • pores are formed in the space occupied by the water, the dispersant, and the binder, thereby forming a composite for vacuum chuck showing porosity. .
  • the Mn-based compound may be composed of Mn-based carbonates such as MnCO 3 , Mn-based oxides such as MnO 2 , Mn-based acetates such as Mn (CH 3 CO 2 ) 2, and the like, and MnCO 3 , Mn (CH 3 CO 2 ) 2 and the like are converted to Mn-based oxides (eg, MnO 2 , Mn 3 O 4 , MnO, etc.) during the sintering process.
  • Mn-based carbonates such as MnCO 3
  • Mn-based oxides such as MnO 2
  • Mn-based acetates such as Mn (CH 3 CO 2 ) 2, and the like
  • MnCO 3 , Mn (CH 3 CO 2 ) 2 and the like are converted to Mn-based oxides (eg, MnO 2 , Mn 3 O 4 , MnO, etc.) during the sintering process.
  • the vacuum chuck composite prepared by the above-mentioned method comprises 75 to 93% by weight of alumina, 7 to 25% by weight of silica, and 0.01 to 5 parts by weight of carbonaceous material based on 100 parts by weight of the total content of the alumina and the silica, and Al 2 O 3 , SiO 2 Since the carbon-based material is dispersed in the ceramic material, the electrical resistance is reduced, thereby having an antistatic function, excellent mechanical properties, porosity, manufacturing process is not complicated, simple manufacturing, and low manufacturing cost.
  • alumina powder 99.8%, AES-11, Sumitomo
  • silica powder CA-20, Sibelco Korea
  • Fe ⁇ Co oxide powder MnCO 3 -57%, Fe 2 O 3 -29
  • distilled water % distilled water %
  • Co 3 O 4 -14% distilled water %, Co 3 O 4 -14%
  • the dispersant and the binder were 1 wt each of the solids (alumina powder, silica powder and Fe ⁇ Co oxide powder).
  • %, 10wt% was added and mixed to prepare a slurry.
  • the dispersant was polycarboxylate ammonium (5468-CF, Cerasperce), and the binder was polyvinyl alcohol (PVA-205, Kuraray).
  • Ball milling was carried out using a ⁇ 2 alumina ball at 110 rpm for 6 hours to produce a uniform slurry.
  • the prepared slurry was dried using a spray dryer (HCSY-01, sunny window) under conditions of a hot air temperature of 180 ° C., a back air temperature of 80 ° C., a disk rotation speed of 8500 rpm, and a slurry input amount of 0.3 L / min.
  • the granulated powder prepared after spray drying showed excellent flowability and uniform spherical shape. It was passed through a 154 ⁇ m sieve and completely dried at 100 ° C. for 24 hours to obtain an alumina-silica-Fe.Co-based oxide powder (hereinafter referred to as 'ASF powder').
  • the ASF powder prepared according to Experimental Example 1 was uniaxially press-molded (45 g, 3 ton, 2 min) using a bar metal mold (30 mm x 60 mm) to obtain a molded body.
  • the molded body was degreased at a temperature of 600 * ° C. in an argon (Ar) atmosphere using a melting furnace (Thermal System & technology), and 1250 ° C., 1300 ° C., and 1500 ° C. in an argon (Ar) atmosphere after degreasing using Polynanotech. Sintered at atmospheric pressure.
  • the sintered compact thus manufactured is referred to as an 'ASF sintered compact'.
  • the ASF powder prepared according to Experimental Example 1 was added to distilled water so as to have a solid content of 60 wt%.
  • Graphene oxide hereinafter referred to as 'GO'
  • 'EG' graphene
  • 'EG' Nanostructured Graphite-400, Graphite to increase electrical conductivity supermarket
  • the slurry was placed in an oven and dried at 100 ° C. for 24 hours to evaporate distilled water, and ethanol was sprayed for a predetermined time during the drying process. It was passed through a 154 ⁇ m sieve and completely dried at 100 ° C. for 24 hours to obtain a powder.
  • the powder thus prepared is referred to as an ASF-carbon composite powder.
  • the ASF-carbon composite powder was uniaxially pressed (45 g, 3 ton, 2 min) using a bar-shaped metal mold (30 mm x 60 mm), and compressed into a bar to obtain a molded product.
  • the molded body was degreased at a temperature of 600 ° C. in an argon (Ar) atmosphere using a melting furnace (Thermal System & technology), and after degreasing, at a pressure of 1250 ° C. and 1300 ° C. in a N 2 atmosphere using a reducing firing furnace (Heewoong ENG, Korea), respectively. Sintered.
  • the ASF powder prepared according to Experimental Example 1 was added to distilled water so as to have a solid content of 60 wt%.
  • graphite superiorior carbon, hereinafter referred to as 'SC'
  • Superior Graphite manufactured by Superior Graphite
  • the slurry was placed in an oven and dried at 100 ° C. for 24 hours to evaporate distilled water, and ethanol was sprayed for a predetermined time during the drying process. It was passed through a 154 ⁇ m sieve and completely dried at 100 ° C. for 24 hours to obtain a powder.
  • the powder thus prepared is referred to as an ASF-carbon composite powder.
  • the ASF-carbon composite powder was uniaxially pressed (45 g, 3 ton, 2 min) using a bar-shaped metal mold (30 mm x 60 mm), and compressed into a bar to obtain a molded product.
  • the molded body was degreased at a temperature of 600 ° C. in an argon (Ar) atmosphere using a melting furnace (Thermal System & technology), and after degreasing, at a pressure of 1250 ° C. and 1300 ° C. in a N 2 atmosphere using a reducing firing furnace (Heewoong ENG, Korea), respectively. Sintered.
  • the ASF powder prepared according to Experimental Example 1 was added to distilled water so as to have a solid content of 60 wt%.
  • SC superior carbon, product of Superior Graphite
  • frit 14-3982M, TOMATEC
  • the slurry was placed in an oven and dried at 100 ° C. for 24 hours to evaporate distilled water, and ethanol was sprayed for a predetermined time during the drying process. It was passed through a 154 ⁇ m sieve and completely dried at 100 ° C. for 24 hours to obtain a powder.
  • the powder thus prepared is referred to as an ASF-carbon composite powder.
  • the ASF-carbon composite powder was uniaxially pressed (45 g, 3 ton, 2 min) using a bar-shaped metal mold (30 mm x 60 mm), and compressed into a bar to obtain a molded product.
  • the molded body was degreased at a temperature of 600 ° C. in an argon (Ar) atmosphere using a melting furnace (Thermal System & technology), and after degreasing, at a pressure of 1250 ° C. and 1300 ° C. in a N 2 atmosphere using a reducing firing furnace (Heewoong ENG, Korea), respectively. Sintered.
  • X-ray diffractometer (DAX-2500 / PC, Rigaku, Japan) was used to analyze the crystal phase of the sintered specimen.
  • the X-ray output was measured at a scan rate of 10 ° C / min under the condition that the voltage was 40 kV and 100 mA. For information on each prize, see JCPDS card and literature.
  • FIG. 1 is a view showing an X-ray diffraction (XRD) pattern of the sintered body prepared according to the experimental examples.
  • XRD X-ray diffraction
  • Figure 1 (a) is for the ASF sintered body (reduction element, N 2 atmosphere, 1250 °C), (b) is for the ASF sintered body (reduction element, N 2 atmosphere, 1300 °C), (c) ASF sintered body (In an atmosphere, Ar atmosphere, 1500 ° C.), (d) is for ASF-EG (0.2 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), and (e) is ASF-EG ( 0.5 wt%) for sintered bodies (reduction furnace, N 2 atmosphere, 1300 ° C.), (f) for ASF-EG (1.0 wt%) sintered bodies (reduction furnace, N 2 atmosphere, 1300 ° C.), (g ) Is for the ASF-GO (0.2 wt%) sintered body (reducing furnace, N 2
  • the microstructure of the fractured surface was observed by scanning electron microscopy (SEM (JSM-6710F, Jeol, Japan), and coated with platinum (Pt) on the fractured surface without pretreatment such as cleaning. (SEM) pictures were analyzed and shown in FIGS. 2 to 9.
  • FIG. 2 is a scanning electron microscope (SEM) image of an ASF sintered body (in an atmosphere, Ar atmosphere, 1500 ° C.), showing a microstructure magnified 1000 times
  • FIG. 3 is an ASF sintered body (reducing element, N 2 atmosphere, 1500 ° C.). Scanning electron microscopy (SEM) of shows microstructure magnified 5000 times.
  • FIG. 4 is a scanning electron microscope (SEM) image of an ASF sintered body (in an atmosphere, Ar atmosphere, 1250 ° C.) and shows a microstructure magnified 1000 times.
  • FIG. 5 is an ASF sintered body (reducing element, N 2 atmosphere, 1250 ° C.). Scanning electron microscopy (SEM) of shows microstructure magnified 5000 times.
  • FIG. 6 is a scanning electron microscope (SEM) image of an ASF sintered body (reducing furnace, N 2 atmosphere, 1250 ° C.), showing a microstructure magnified 1000 times
  • FIG. 7 is an ASF sintered body (reducing furnace, N 2 atmosphere, 1250 ° C.). Scanning electron microscopy (SEM) photograph of) shows the microstructure magnified 5000 times.
  • FIG. 8 is a scanning electron microscope (SEM) image of an ASF sintered body (reducing furnace, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times
  • FIG. 9 is an ASF sintered body (reducing furnace, N 2 atmosphere, 1300 ° C.). Scanning electron microscopy (SEM) photograph of) shows the microstructure magnified 5000 times.
  • Table 1 below shows the density, surface resistance and strength of the ASF sintered body according to the sintering conditions.
  • FIG 11 shows the surface resistance of the ASF sintered body according to the sintering conditions.
  • Table 2 below shows the density, surface resistance and strength of the ASF-GO and ASF-EG sintered bodies according to the sintering conditions.
  • FIG. 13 shows the density of ASF-GO and ASF-EG sintered bodies according to the sintering conditions.
  • Figure 14 shows the surface resistance of the ASF-GO, ASF-EG sintered body according to the sintering conditions.
  • Table 3 below shows the density, surface resistance and strength of the ASF-SC sintered body according to the sintering conditions.
  • Figure 16 shows the surface resistance of the ASF-SC sintered body according to the sintering conditions.
  • FIG. 18 is a scanning electron microscope (SEM) image of an ASF-SC (0.5 wt%)-Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 19 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a magnification of 5000 times.
  • FIG. 20 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 21 is a scanning electron microscope (SEM) image of an ASF-SC (0.5 wt%)-Frit (1.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a magnification of 5000 times.
  • FIG. 22 is a scanning electron microscope (SEM) image of an ASF-SC (0.5 wt%)-Frit (2.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 23 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (2.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a magnification of 5000 times.
  • FIG. 24 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (2.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 25 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (2.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a magnification of 5000 times.
  • FIG. 26 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 27 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1200 ° C.), showing a magnification of 5000 times.
  • FIG. 28 is a scanning electron microscope (SEM) image of an ASF-SC (0.5 wt%)-Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a microstructure magnified 1000 times.
  • FIG. 29 is a scanning electron microscope (SEM) photograph of an ASF-SC (0.5 wt%)-Frit (5.0 wt%) sintered body (reducing element, N 2 atmosphere, 1300 ° C.), showing a magnification of 5000 times.
  • Table 4 shows the density, surface resistance, and strength of the ASF-SC (0.5 wt%)-Frit sintered body according to the sintering conditions.
  • Table 5 shows the density, surface resistance, and strength of the ASF-SC (3.0 wt%)-Frit sintered body according to the sintering conditions.
  • the carbon-based material is dispersed in the ceramic material, the electrical resistance is reduced, so that it has an antistatic function, has excellent mechanical properties, exhibits porosity, and the manufacturing process is not complicated. There is a possibility.

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

La présente invention concerne : un composite de mandrin sous vide comprenant de 75 à 93 % en poids d'alumine, de 7 à 25 % en poids de silice, et de 0,01 à 5 parties en poids d'un matériau à base de carbone sur la base de 100 parties en poids des quantités totales de l'alumine et de la silice ; et son procédé de préparation. Selon la présente invention, un matériau à base de carbone est dispersé dans des matériaux céramiques en Al2O3 et SiO2, ce qui fait en sorte que la présente invention présente une résistance électrique réduite de sorte à avoir une fonction antistatique, a d'excellentes propriétés mécaniques, présente une porosité, peut être préparée facilement sans utiliser un procédé de préparation complexe, et a des coûts de préparation faibles.
PCT/KR2017/006616 2016-08-19 2017-06-22 Composite de mandrin sous vide et procédé de préparation correspondant WO2018034422A1 (fr)

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CN108821752A (zh) * 2018-07-24 2018-11-16 合肥岑遥新材料科技有限公司 一种耐高温陶瓷基复合材料及其制备方法

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KR20110116244A (ko) * 2009-02-23 2011-10-25 가부시키가이샤 소딕 착색 세라믹 진공 척 및 그 제조 방법
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KR101073878B1 (ko) 2009-05-11 2011-10-17 서울대학교산학협력단 대전방지 기능을 갖는 기판 및 그 제조방법

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JP2004018354A (ja) * 2002-06-20 2004-01-22 Nisshinbo Ind Inc 高い気孔率を有するカーボン多孔体吸着板、その製造方法及びそれを装着した真空チャック
KR20070037831A (ko) * 2005-10-04 2007-04-09 송영환 진공척
KR20080041090A (ko) * 2006-11-06 2008-05-09 가부시키가이샤 단켄시루세코 흡착 부상 판넬
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JP2012171824A (ja) * 2011-02-21 2012-09-10 National Institute Of Advanced Industrial Science & Technology 炭化ケイ素系耐熱性超軽量多孔質構造材及びその製造方法
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