WO2018034422A1 - Vacuum chuck composite and preparation method therefor - Google Patents

Abstract

The present invention relates to: a vacuum chuck composite comprising 75-93 wt% of alumina, 7-25 wt% of silica, and 0.01-5 parts by weight of a carbon-based material on the basis of 100 parts by weight of the total amounts of the alumina and the silica; and a preparation method therefor. According to the present invention, a carbon-based material is dispersed in Al₂O₃ and SiO₂ ceramic materials, and thus the present invention has reduced electrical resistance so as to have an antistatic function, has excellent mechanical properties, exhibits porosity, can be prepared easily without a complex preparation process, and has low preparation costs.

Description

Composite for vacuum chuck and manufacturing method thereof

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.

In order for the semiconductor device to operate to the designed electrical specification, 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.

Conventionally, since the thickness of a semiconductor wafer is so thick that it is hardly affected by such static electricity, defects caused by static electricity rarely occur, which is not a big problem.

Recently, as electronic products such as smart phones and smart TVs are becoming lighter and thinner, the thicknesses of semiconductor wafers and various display substrates used are becoming thinner and larger in size.

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. As a result, 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.

Thus, the need for a porous ceramic substrate having an electrical resistance control function has emerged.

In order to solve the problems caused by static electricity generated in chucks or stages in existing semiconductor and LCD production equipment, chucks or stages having an antistatic function have been developed. Among them, Korean Patent Application Publication No. 10-2010-0109098 ' Antistatic work stage.

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.

[Preceding technical literature]

[Patent Documents]

Republic of Korea Patent Publication No. 10-2010-0109098

Republic of Korea Patent Publication No. 10-2010-0121895

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.

In addition, 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.

In the step (a), 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.

In the step (c), 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 ℃ by supplying nitrogen or argon gas in a reducing furnace.

According to 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, thereby having an antistatic function, excellent mechanical properties, porosity, manufacturing process is not complicated, simple manufacturing, and low manufacturing cost.

1 is a view showing an X-ray diffraction (XRD) pattern of the sintered body prepared according to the experimental examples.

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, and FIG. 3 is an ASF sintered body (reducing element, N ₂ atmosphere, 1500 ° C.). Scanning electron microscopy (SEM) of shows microstructure magnified 5000 times.

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, and 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, and 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.

10 is a graph showing the density of the ASF sintered body according to the sintering conditions.

11 is a graph showing the surface resistance of the ASF sintered body according to the sintering conditions.

12 is a graph showing the strength of the ASF sintered body according to the sintering conditions.

13 is a graph showing density of ASF / GO and ASF / EG sintered bodies according to sintering conditions.

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.

30 is a graph showing the density of the ASF / SC (0.5 wt%) / Fri sintered body according to the sintering conditions.

31 is a graph showing the surface resistance of the ASF / SC (0.5 wt%) / Fri sintered body according to the sintering conditions.

32 is a graph showing the strength of the ASF / SC (0.5 wt%) / Fri sintered body according to the sintering conditions.

33 is a graph showing the density of the ASF / SC (3.0 wt%) / Fri sintered body according to the sintering conditions.

34 is a graph showing the surface resistance of the ASF / SC (3.0 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 according to a preferred embodiment of the present invention 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.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the following embodiments are provided to those skilled in the art to fully understand the present invention, and may be modified in various forms, and the scope of the present invention is limited to the embodiments described below. It doesn't happen.

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 according to a preferred embodiment of the present invention 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.

In the step (a), 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.

In the step (c), 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 ℃ by supplying nitrogen or argon gas in a reducing furnace.

Hereinafter, the manufacturing method of the vacuum chuck composite according to a preferred embodiment of the present invention will be described in more detail.

Alumina (Alumina, Al ₂ O ₃ ) powder and silica (Silica, SiO ₂ ) powder are mixed to form a first slurry.

It is preferable to mix 75-93 weight% of the said alumina powders, and 7-25 weight% of the said silica powders. It is preferable that 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.

At this time, 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 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. Al ₂ O ₃ , SiO ₂ By dispersing transition metal oxides such as Fe, Co, and Mn in a ceramic material, 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.

At this time, 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.

Hereinafter, 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. For example, in consideration of the particle size, 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. It is made in the form of spherical granules in the slurry state by the spray drying process, which improves the fluidity between particles in the molding process, which is the next process, and facilitates the molding, and serves to make the pores between the particles have a uniform shape. 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.

In this case, 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.

It is preferable to mix 0.01 to 5 parts by weight of the carbonaceous material 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. In addition, when the carbon-based material is mixed, mechanical properties and physical properties of the vacuum chuck composite may be improved. Al ₂ O ₃ , SiO ₂ By dispersing the carbon-based material in the ceramic material, it is possible to reduce the electrical resistance to impart an antistatic function.

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 ℃ for 1 to 48 hours.

The composite powder is molded. The molding can be done in a variety of ways. For example, 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. During the sintering process, the water, the dispersant, and the binder inside the molded body (molded product) are burned out and disappeared. At this time, 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.

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.

Hereinafter, experimental examples according to the present invention are specifically presented, and the present invention is not limited by the following experimental examples.

Experimental Example 1 Preparation of ASF Powder

To prepare the slurry, 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) in distilled water %, Co ₃ O ₄ -14%) were added in a mass ratio of 84 wt%, 12.63 wt% and 3.37 wt%, respectively, and 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 Ø2 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 μm 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').

Experimental Example 2 Manufacture of ASF Sintered Body

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. Hereinafter, the sintered compact thus manufactured is referred to as an 'ASF sintered compact'.

Experimental Example 3 Preparation of ASF-Carbon Composite

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') (GO-V30-100, Standard Graphene) and graphene (hereinafter referred to as 'EG') (Nanostructured Graphite-400, Graphite to increase electrical conductivity supermarket) was added to 0.2 to 5.0 wt% of solids, respectively, to form a slurry. To prepare a uniform slurry, ball milling was performed at 110 rpm for 6 hours using a Ø2 alumina ball.

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 μm 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.

Experimental Example 4 Preparation of ASF-Carbon Composite

The ASF powder prepared according to Experimental Example 1 was added to distilled water so as to have a solid content of 60 wt%. In order to increase the electrical conductivity, graphite (superior carbon, hereinafter referred to as 'SC') (manufactured by Superior Graphite) was added to 0.5 to 3.0 wt% of solids to form a slurry. To prepare a uniform slurry, ball milling was performed at 110 rpm for 6 hours using a Ø2 alumina ball.

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 μm 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.

Experimental Example 5 Preparation of ASF-Carbon Composite

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) and frit (14-3982M, TOMATEC) to increase electrical conductivity were added at 0.5 to 5.0 wt% of solids, respectively, to form a slurry. To prepare a uniform slurry, ball milling was performed at 110 rpm for 6 hours using a Ø2 alumina ball.

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 μm 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.

An 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.

1 is a view showing an X-ray diffraction (XRD) pattern of the sintered body prepared according to the experimental examples. In Figure 1 (a) is for the ASF sintered body (reduction element, N ₂ atmosphere, 1250 ℃), (b) is for the ASF sintered body (reduction element, N ₂ atmosphere, 1300 ℃), (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 atmosphere, 1250 ° C.), and (h) is the ASF-GO (0.2 wt%) sintered body (reducing element furnace, N ₂ atmosphere, 1300 ° C.) (I) is for ASF-GO (0.5 wt%) sintered body (reducing furnace, N ₂ atmosphere, 1250 ° C.), and (j) is for ASF-GO (0.2 wt%) sintered body (reducing element furnace, N ₂ atmosphere, are for the 1300 ℃), (k) is ASF-SC (0.5wt%) - Frit (1.0wt%) sintered body (sintering furnace reduction, N ₂ atmosphere, 1300 ℃) Is for, (l) is ASF-SC (0.5wt%) - Frit (2.0wt%) sintered body are for the (reduced sintering furnace, N ₂ atmosphere, 1300 ℃), (m) is ASF-SC (0.5 wt%) -Frit (5.0 wt%) for sintered bodies (reduction furnace, N ₂ atmosphere, 1300 ° C).

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, and FIG. 3 is an ASF sintered body (reducing element, N ₂ atmosphere, 1500 ° C.). Scanning electron microscopy (SEM) of shows microstructure magnified 5000 times.

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, and 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, and 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.

Compound	Sintering Condition	Density (g / cm 3 ) /%	Surface restance (Ω)	Strengtjh (MPa)
ASF	Atmosphere, 1250 ℃, Ar	2.07 / 52	2.05 E11	20.94
ASF	Atmosphere, 1500 ℃, Ar	2.39 / 60	5.53 E11	61.72
ASF	Reduction firing furnace, 1250 ° C, N 2	2.16 / 54	1.05 E6	-
ASF	Reduction firing furnace, 1300 ° C, N 2	2.23 / 56	-	-

10 shows the density of the ASF sintered body according to the sintering conditions.

11 shows the surface resistance of the ASF sintered body according to the sintering conditions.

12 shows the strength 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.

Compound	Sintering Condition	Density (g / cm 3 ) /%	Surface resistance (Ω)
ASF-GO 0.2 wt%	Reduction firing furnace, 1250 ° C, N 2	2.11 / 53	1.65 E11
ASF-GO 0.2 wt%	Reduction firing furnace, 1300 ° C, N 2	2.24 / 57	2.33 E11
ASF-GO 0.5 wt%	Reduction firing furnace, 1250 ° C, N 2	2.09 / 53	5.03 E11
ASF-GO 0.5 wt%	Reduction firing furnace, 1300 ° C, N 2	2.22 / 56	5.71 E11
ASF-GO 1.0 wt%	Atmosphere, 1250 ℃, Ar	2.05 / 52	5.14 E4
ASF-GO 3.0 wt%	Atmosphere, 1250 ℃, Ar	-	1.05 E6
ASF-GO 5.0 wt%	Atmosphere, 1250 ℃, Ar	-	1.05 E6
ASF-EG 0.2 wt%	Reduction firing furnace, 1300 ° C, N 2	2.33 / 59	6.88 E9
ASF-EG 0.5 wt%	Reduction firing furnace, 1300 ° C, N 2	2.24 / 57	1.26 E10
ASF-EG 1.0 wt%	Reduction firing furnace, 1300 ° C, N 2	2.09 / 53	1.05 E10

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.

Compound	Sintering Condition	Density (g / cm 3 ) /%	Surface resistance (Ω)	Strength (MPa)
ASF-SC 0.2 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	2.39 / 60	2.86 E10	76.56
ASF-SC 0.5 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	2.34 / 59	9.74 E9	84.48

15 shows the density of the ASF-SC sintered compact according to the sintering conditions.

Figure 16 shows the surface resistance of the ASF-SC sintered body according to the sintering conditions.

17 shows the strength 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 below shows the density, surface resistance, and strength of the ASF-SC (0.5 wt%)-Frit sintered body according to the sintering conditions.

Compound	Sintering Condition	Density (g / cm 3 ) /%	Surface resistance (Ω)	Strength (MPa)
ASF-SC (0.5 wt%)-Frit 1 wt%	Reduction firing furnace, 1200 ℃, N 2, 10 ℃ / min	2.26 / 57	1.88 E10	-
ASF-SC (0.5 wt%)-Frit 2 wt%	Reduction firing furnace, 1200 ℃, N 2, 10 ℃ / min	2.24 / 57	2.44 E10	-
ASF-SC (0.5 wt%)-Frit 5 wt%	Reduction firing furnace, 1200 ℃, N 2, 10 ℃ / min	2.23 / 56	5.23 E10	-
ASF-SC (0.5 wt%)-Frit 1 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	2.63 / 67	3.28 E10	106.46
ASF-SC (0.5 wt%)-Frit 2 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	2.57 / 65	4.97 E10	106.04
ASF-SC (0.5 wt%)-Frit 5 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	2.96 / 75	5.41 E10	163.02

30 shows the density of the ASF-SC (0.5 wt%)-Frit sintered body according to the sintering conditions.

31 shows the surface resistance of the ASF-SC (0.5 wt%)-Frit sintered body according to the sintering conditions.

32 shows the strength of the ASF-SC (0.5 wt%)-Frit sintered body according to the sintering conditions.

Table 5 below shows the density, surface resistance, and strength of the ASF-SC (3.0 wt%)-Frit sintered body according to the sintering conditions.

Compound	Sintering Condition	Density (g / cm 3 ) /%	Surface resistance (Ω)	Strength (MPa)
ASF-SC (3.0 wt%)-Frit 1 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	55	7.75 E8	52.50
ASF-SC (3.0 wt%)-Frit 2 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	54	3.94 E9	41.81
ASF-SC (3.0 wt%)-Frit 5 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	55	3.47 E9	56.88
ASF-SC (3.0 wt%)-Frit 10 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	55	8.14 E9	91.72
ASF-SC (3.0 wt%)-Frit 15 wt%	Reduction firing furnace, 1300 ℃, N 2, 10 ℃ / min	55%	3.29 E9	71.95

33 shows the density of the ASF-SC (3.0 wt%)-Frit sintered body according to the sintering conditions.

34 shows the surface resistance of the ASF-SC (3.0 wt%)-Frit sintered body according to the sintering conditions.

35 shows the strength of the ASF-SC (3.0 wt%)-Frit sintered body according to the sintering conditions.

As mentioned above, although the preferred embodiment of this invention was described in detail, this invention is not limited to the said embodiment, A various deformation | transformation by a person of ordinary skill in the art within the scope of the technical idea of this invention is carried out. This is possible.

Al ₂ O ₃ , SiO ₂ Since 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.

Claims (15)

1. 75 to 93% by weight of alumina;

   7-25 wt% silica; And

   Vacuum chuck composite, characterized in that it comprises 0.01 to 5 parts by weight of the carbon-based material based on 100 parts by weight of the total content of the alumina and the silica.
2. The vacuum chuck composite according to claim 1, further comprising 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.
3. The composite of claim 2, wherein the Fe · Co-based oxide comprises Fe ₂ O ₃ , Co ₃ O _4, and a Mn-based compound as chemical components.
4. The method of claim 2, wherein the Fe-Co-based oxide is characterized in that it comprises 24 to 34% by weight Fe ₂ O _{3, 10 to} 18% by weight Co ₃ O ₄ and 50 to 64% by weight Mn-based compound Composite for vacuum chuck.
5. The composite of claim 1, further comprising 0.01 to 5 parts by weight of frit based on 100 parts by weight of the total amount of the alumina and the silica.
6. The composite of claim 1, wherein the carbon-based material comprises at least one material selected from graphene oxide, graphene, and graphite.
7. (a) mixing 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 form an alumina-silica powder;

   (c) mixing a carbonaceous material with the alumina-silica powder to form a second slurry;

   (d) drying the second slurry to form a composite powder;

   (e) molding the composite powder; And

   (f) sintering the shaped result,

   Method (c) in the step of producing a composite for vacuum chuck composite, characterized in that for mixing 0.01 to 5 parts by weight of the carbon-based material with respect to 100 parts by weight of the alumina-silica powder.
8. The method of claim 7, wherein in step (a), 0.5 to 6.5 parts by weight of Fe · Co-based oxide is further mixed with respect to 100 parts by weight of the total content of the alumina powder and the silica powder. .
9. The method of claim 8, wherein the Fe · Co-based oxide comprises Fe ₂ O ₃ , Co ₃ O _4, and a Mn-based compound as a chemical component.
10. The method of claim 8, wherein the Fe-Co-based oxide is characterized in that it comprises 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 Method for producing a composite for vacuum chuck.
11. The method of claim 7, wherein in step (c), 0.01 to 5 parts by weight of frit is further mixed with respect to 100 parts by weight of the alumina-silica powder.
12. The method of claim 7, wherein the carbon-based material comprises at least one material selected from graphene oxide, graphene, and graphite.
13. The method of claim 7, wherein in step (a) further dispersing agent and binder,

    The dispersant is mixed with 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 a method for producing a composite for vacuum chuck, characterized in that for mixing 3 to 15 parts by weight based on 100 parts by weight of the total content of the alumina powder and the silica powder.
14. The method of claim 13, wherein the dispersant comprises polycarboxylate ammonium,

    The binder is polyvinyl alcohol (polyvinyl alcohol) characterized in that the manufacturing method of the composite for vacuum chuck.
15. The method of claim 7, wherein the sintering is performed at a temperature of 1200 to 1600 ° C. by supplying nitrogen or argon gas in a reducing furnace.

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