CN113045328B - Preparation method of porous ceramic plate and high-precision ceramic porous platform - Google Patents
Preparation method of porous ceramic plate and high-precision ceramic porous platform Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 63
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000000197 pyrolysis Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000011148 porous material Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 15
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 7
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 239000004579 marble Substances 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000011112 process operation Methods 0.000 abstract 1
- 239000004973 liquid crystal related substance Substances 0.000 description 5
- 239000007770 graphite material Substances 0.000 description 3
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- 239000010409 thin film Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
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- 238000005452 bending Methods 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 238000011900 installation process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a porous ceramic plate and a high-precision ceramic porous platform, wherein the preparation of the porous ceramic plate comprises the following steps: the method comprises the steps of taking a ceramic material, a resistance regulation factor material and a thermal expansion coefficient adjusting material as raw materials, mixing the materials, adding a pore-forming agent, stirring and grinding, pre-pressing and forming, heating and pyrolyzing, sintering without pressure and maintaining pressure to obtain the porous ceramic plate, adjusting the porous ceramic plate by adding the resistance regulation factor material and the thermal expansion coefficient adjusting material to reduce the electrical conductivity and the thermal conductivity of the ceramic, adding the pore-forming agent simultaneously, and making holes in a pyrolysis mode to control the aperture of the manufactured high-precision ceramic porous platform connecting through hole to be 1-100 microns and the hole content to be 10-60%, ensuring the precision in the process operation and preventing the product from being worn.
Description
Technical Field
The invention relates to the technical field of ceramic materials and processes thereof, in particular to a preparation method of a porous ceramic plate and a high-precision ceramic porous platform.
Background
In the process of manufacturing the display panel, a carrier is usually used to support and fix the liquid crystal display panel for the convenience of the manufacturing operation. The traditional carrying platform structure is made of metal, the top surface of the carrying platform is provided with a plurality of negative pressure air holes, one side surface of the carrying platform is provided with an air port communicated with the negative pressure air holes for connecting with a negative pressure device, and then the negative pressure device can be utilized to enable the negative pressure air holes to generate suction force for adsorbing and fixing the liquid crystal display panel on the carrying platform so as to facilitate the operation of each process of the liquid crystal display panel. However, since the metal carrier has thermal and electrical conductivity, when it carries the liquid crystal display panel to perform Rubbing (Rubbing) process, large temperature variation and frictional force are generated, which affects the liquid crystal alignment, and thus the quality and density of the Rubbing are not easy to control and the display panel is worn.
In recent years, with the development of light weight and intelligence of electronic products, the thickness and size of semiconductor chips and various display substrates in 3C electronic products are gradually becoming thinner and larger, and the development of this trend has led to the increasing demand for mounting devices of electronic products. In the processes of processing wafers such as cutting, photoetching, exposure and the like, the requirement on the flatness is controlled within 3 mu m, but the aperture of the platform deck can only be controlled between 0.1mm and 0.5mm and is larger because the traditional platform deck adopts a mode of directly drilling on an aluminum alloy or marble platform and then carrying out negative pressure adsorption, and the materials are easy to bend and break when the thin-film materials such as wafers or flexible screens are adsorbed.
Disclosure of Invention
Therefore, in order to solve the above problems, the present invention utilizes the characteristics of poor conductivity and wear resistance of the ceramic, so that the ceramic is not easy to wear the product in the manufacturing process. Meanwhile, the porous ceramic plate material and the preparation process are improved, so that the aperture of the porous ceramic plate connecting through hole is reduced to 1 mu m-100 mu m, and the bending and the crushing of the thin film materials such as a round or flexible screen and the like in the installation process can be effectively prevented.
The invention is realized by the following technical scheme:
a method of making a porous ceramic plate, comprising the steps of:
s1, preparing materials by using a ceramic material, a resistance regulating factor material and a thermal expansion coefficient regulating material as raw materials to obtain a mixed material, and sieving the mixed material to control the particle size of the mixed material to be between 2 and 75 micrometers;
s2, under the stirring condition, mixing the mixed material with a pore-forming agent, and putting the mixture into a roller ball mill or a planetary ball mill for grinding and mixing for 1-12 hours to obtain a mixture;
s3, placing the mixture into a mold, placing the mold into a one-way press machine for prepressing, keeping the prepressing pressure between 50 and 100 MPa for 1 to 5 minutes, and performing press forming to obtain a green body;
s4, at a temperature of 250 DEG C o C～600 o C, the heat preservation time is 0.5 to 3 hours, and the heating rate is 1 o Pyrolyzing the green body under the condition of C/min;
s5, sintering the green body under vacuum or inert atmosphere protection without pressure, wherein the temperature rise rate is 1-30 DEG o Between C/min, the sintering temperature is 800 o C～1600 o C, sintering under the parameter condition that the heat preservation time is between 0.5 and 8 hours;
and S6, after heat preservation and pressure maintaining, cooling to room temperature to obtain the porous ceramic plate.
Preferably, the resistance adjusting factor material is nickel, cobalt, zinc, related alloy materials, conductive ceramic MAX phase materials, tin and other materials.
Preferably, the thermal expansion coefficient adjusting material is Zr (P) 1-x V x ) 2 O 7 、(Zr, Hf)W 2 O 8 Materials with negative expansion coefficient or materials with low expansion coefficient such as silicon, quartz, etc.
Preferably, the ceramic material is alumina, and the resistance control factor material is MAX-phase ceramic Ti 3 AlC 2 The thermal expansion coefficient adjusting material is Zr (P) 1-x V x ) 2 O 7 。
Preferably, in the step S1, the mixed material is made of alumina, MAX phase ceramic Ti 3 AlC 2 Powder and Zr (P) 1-x V x ) 2 O 7 According to molar ratio (30-80): (10-20): (10-60) preparing the raw materials.
Preferably, in the step S2, the pore former has a size of 0.1 μm to 100 μm.
Preferably, the pore-forming agent is polyvinyl butyral (PVB) or polymethyl methacrylate (PMMA).
Preferably, in step S2, the pore-forming agent is PVB, and the volume ratio of the mixed material to the pore-forming agent is (40-90): (10-60) batching.
Preferably, in step S4, the PVB pyrolysis temperature is 250 o C～400 o C, keeping the temperature for 0.5 to 2 hours; the pyrolysis temperature of PMMA in the air is 400-600 o C, keeping the temperature for 0.5 to 3 hours.
The high-precision ceramic porous platform comprises a porous ceramic plate prepared by the method and a base arranged below the porous ceramic plate and designed with a negative pressure gas path, wherein the base is a marble platform base, a stainless steel base, a ceramic base and an aluminum alloy base.
Preferably, the porous ceramic plate has a pore diameter of 1 to 100 μm, a pore content of 10 to 60%, and a resistance of 10% 6 Ohm-10 10 Ohm, coefficient of thermal expansion of (0-7). 10 -6 /K。
The preparation method of the porous ceramic plate and the high-precision ceramic porous platform have the beneficial effects that:
1. in the scheme, the MAX-phase ceramic Ti3AlC2 powder material is used as the resistance regulation factor material, and the MAX-phase ceramic Ti3AlC2 powder material is a few conductive ceramics, has good conductivity compared with other materials, and has good thermal compatibility with alumina and other ceramics.
2. The thermal expansion coefficient adjusting material is added in the scheme, the thermal conductivity of the porous ceramic plate is reduced, and the high-precision ceramic porous platform made of the porous ceramic plate cannot generate large temperature change during operation.
3. In the scheme, the pore-forming agent is used for preparing the pores, so that the pore diameter of the prepared high-precision ceramic porous platform connecting through hole is controlled to be 1-100 micrometers, the pore content is controlled to be 10-60 percent, and the bending and the crushing of thin film materials such as attached wafers or flexible screens caused by overlarge pore diameter are prevented.
Drawings
FIG. 1: is the microstructure of the alumina ceramic based porous material of the present invention;
FIG. 2: is the microstructure of the porous material based on silicon carbide ceramics in the invention;
FIG. 3: is the microstructure of the cordierite ceramic-based porous material of the present invention.
Detailed Description
In order that the objects, advantages and features of the invention may be more clearly and specifically shown and described, there shall now be seen and explained, by way of non-limiting illustration of preferred embodiments. The embodiment is only a typical example of the technical solution of the present invention, and any technical solution formed by adopting equivalent replacement or equivalent transformation falls within the scope of the present invention.
It is also stated that in the description of the schemes, it is to be noted that the terms "center", "upper", "lower", "left", "right", "front", "rear", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Furthermore, the terms "first" and "second" in this document are used for descriptive purposes only and are not to be construed as indicating or implying a ranking of importance or an implicit indication of the number of technical features shown. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the present invention, "a plurality" means two or more unless specifically defined otherwise.
The preparation method of the porous ceramic plate and the high-precision ceramic porous platform disclosed by the invention are explained by combining the drawings as follows:
example 1:
s1, using alumina and MAX phase ceramic Ti 3 AlC 2 Powder and Zr (P) 1-x V x ) 2 O 7 Is prepared from the following raw materials in a molar ratio of 60:20:20, preparing materials to obtain a mixed material, and sieving the mixed material to control the particle size of the mixed material to be between 2 and 75 mu m;
s2, mixing the mixed material with PVB (polyvinyl butyral) according to a ratio of 60:40, and putting the mixture into a roller ball mill for grinding and mixing for 1 to 12 hours to obtain a mixture
S3, placing the mixture into a mold, wherein the mold can be made of graphite materials and is square or round, placing the mold into a one-way press machine for prepressing, keeping the prepressing pressure between 50 and 100 MPa for 1 to 5 minutes, and performing press forming to obtain a green body;
s4, at the temperature of 300 DEG C o C, the heat preservation time is 2 hours, and the heating rate is 1 o Pyrolyzing the green body under the condition of C/min;
s5, sintering the green body under the protection of nitrogen atmosphere without pressure, wherein the temperature rise rate is 1-30 DEG o The sintering temperature is 1400 ℃ between C/min o C, sintering under the parameter condition that the heat preservation time is 4 hours, wherein the pore content of the porous ceramic plate sintered according to the method is about 39 percent, the average pore diameter is 5.2 +/-0.6 microns, and the resistance is (4.8 +/-1.2) multiplied by 10 8 Ohm, coefficient of thermal expansion of (4.2 + -0.8) × 10 -6 /K
And S6, after heat preservation and pressure maintaining, cooling to room temperature to obtain the porous ceramic plate.
Example 2:
s1, silicon carbide and MAX phase ceramic Ti 3 AlC 2 Powder and (Zr, hf) W 2 O 8 Is prepared from the following raw materials in a molar ratio of 80:10:10, preparing materials to obtain a mixed material, and sieving the mixed material to control the particle size of the mixed material to be between 2 and 75 microns;
s2, mixing the mixed material and PMMA (methyl methacrylate) according to a ratio of 50: mixing the materials according to the proportion of 50, putting the mixture into a roller ball mill, grinding and mixing the materials for 1 to 12 hours to obtain a mixture;
s3, placing the mixture into a mold, wherein the mold can be made of graphite materials and is square or round, placing the mold into a one-way press machine for prepressing, keeping the prepressing pressure between 50 and 100 MPa for 1 to 5 minutes, and performing press forming to obtain a green body;
s4, at the temperature of 500 DEG C o C, the heat preservation time is 2 hours, and the heating rate is 1 o Pyrolyzing the green body under the condition of C/min;
s5, sintering the green body under the protection of nitrogen atmosphere and without pressure, wherein the temperature rise rate is 1-30 o The sintering temperature is 1200 ℃ between C/min o C, sintering under the parameter condition that the heat preservation time is 3 hours, and sintering according to the modeThe hole content of the porous ceramic plate is about 48 percent, the average pore diameter is 9.8 +/-2.6 microns, and the resistance is (5 +/-0.8) multiplied by 10 6 Ohm, coefficient of thermal expansion of (3.4 + -0.6) x 10 -6 /K。
And S6, after heat preservation and pressure maintaining, cooling to room temperature to obtain the porous ceramic plate.
Example 3:
cordierite, MAX phase ceramic Ti 3 AlC 2 Powder and Zr (P) 1-x V x ) 2 O 7 Is prepared from the following raw materials in a molar ratio of 40:35:25, preparing materials to obtain a mixed material, and sieving the mixed material to control the particle size of the mixed material to be between 2 and 75 microns;
s2, mixing the mixed material with PVB (polyvinyl butyral) under the stirring condition in a ratio of 70:30, and putting the mixture into a roller ball mill for grinding and mixing for 1 to 12 hours to obtain a mixture;
s3, placing the mixture into a mold, wherein the mold can be made of graphite materials and is square or round, placing the mold into a one-way press machine for prepressing, keeping the prepressing pressure between 50 and 100 MPa for 1 to 5 minutes, and performing press forming to obtain a green body;
s4, at the temperature of 300 DEG C o C, the heat preservation time is 2 hours, and the heating rate is 1 o Pyrolyzing the green body under the condition of C/min;
s5, sintering the green body under the protection of nitrogen atmosphere and without pressure, wherein the temperature rise rate is 1-30 o The sintering temperature is 1000 ℃ between C/min o C, sintering under the parameter condition that the heat preservation time is 3 hours, wherein the pore content of the porous ceramic plate sintered according to the method is about 32 percent, the average pore diameter is 5.7 +/-1.4 microns, and the resistance is (6.2 +/-0.6) multiplied by 10 9 Ohm, coefficient of thermal expansion of (2.2 + -0.6) x 10 -6 /K 。
And S6, after heat preservation and pressure maintaining, cooling to room temperature to obtain the porous ceramic plate.
The invention has various embodiments, and all technical solutions formed by adopting equivalent transformation or equivalent transformation are within the protection scope of the invention.
Claims (9)
1. The preparation method of the porous ceramic plate is characterized by comprising the following steps of:
s1, preparing materials by taking a ceramic material, a resistance regulating factor material and a thermal expansion coefficient regulating material as raw materials to obtain a mixed material, and sieving the mixed material to control the particle size of the mixed material to be between 2 and 75 microns;
s2, under the stirring condition, mixing the mixed material with a pore-forming agent, and putting the mixture into a roller ball mill or a planetary ball mill for grinding and mixing for 1-12 hours to obtain a mixture;
s3, placing the mixture into a mold, placing the mold into a one-way press for prepressing at the prepressing pressure of 50-100 MPa for 1-5 minutes, and performing press forming to obtain a green body;
s4, at a temperature of 250 DEG C o C～600 o C, the heat preservation time is 0.5 to 3 hours, and the heating rate is 1 o C/min, pyrolyzing the green body;
s5, sintering the green body under the protection of vacuum environment or inert atmosphere without pressure, wherein the temperature rise rate is 1-30 DEG o Between C/min, the sintering temperature is 800 o C～1600 o C, sintering under the parameter condition that the heat preservation time is between 0.5 and 8 hours;
s6, after heat preservation and pressure maintaining, cooling to room temperature to obtain a porous ceramic plate;
the thermal expansion coefficient adjusting material is Zr (P) 1-x V x ) 2 O 7 、(Zr, Hf)W 2 O 8 The material with negative expansion coefficient or the material with low thermal expansion coefficient of silicon and quartz, the ceramic material is alumina, and the material with resistance regulating factor is MAX phase ceramic Ti 3 AlC 2 And (3) powder.
2. A method of manufacturing a porous ceramic plate according to claim 1, characterized in that: the thermal expansion coefficient adjusting material is Zr (P) 1-x V x ) 2 O 7 。
3. A method of manufacturing a porous ceramic plate according to claim 2, characterized in that: in the step S1, the mixed material is alumina and MAX phase ceramic Ti 3 AlC 2 Powder and Zr (P) 1-x V x ) 2 O 7 According to molar ratio (30-80): (10-20): (10-60) preparing the raw materials.
4. A method of making a porous ceramic plate according to claim 1, wherein: in the step S2, the size of the pore-forming agent is between 0.1 and 100 microns.
5. A method of manufacturing a porous ceramic plate according to claim 1, characterized in that: the pore-forming agent is polyvinyl butyral PVB or polymethyl methacrylate PMMA.
6. A method of manufacturing a porous ceramic plate according to claim 5, characterized in that: in step S2, the pore-forming agent is PVB, and the volume ratio of the mixed material to the pore-forming agent is (40-90): (10-60) batching.
7. A method of manufacturing a porous ceramic plate according to claim 5, characterized in that: in step S4, the PVB pyrolysis temperature is 250 o C～400 o C, keeping the temperature for 0.5 to 2 hours; the pyrolysis temperature of PMMA in air is 400 o C～600 o C, keeping the temperature for 0.5 to 3 hours.
8. A high-precision ceramic porous platform, comprising a porous ceramic plate prepared by the method of any one of claims 1 to 7, and a base containing a negative pressure gas path design disposed thereunder, wherein the base is a marble platform base, a stainless steel base, a ceramic base, or an aluminum alloy base.
9. The high-precision ceramic porous platform of claim 8, wherein: the above-mentionedThe porous ceramic plate has a pore diameter of 1-100 μm, a pore content of 10-60%, and a resistance of 10% 6 Ohm-10 10 Ohm, coefficient of thermal expansion of (0-7) x 10 -6 /K。
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