CN115710119A - Preparation method of ceramic arm based on water-based injection molding process - Google Patents
Preparation method of ceramic arm based on water-based injection molding process Download PDFInfo
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- CN115710119A CN115710119A CN202211510379.1A CN202211510379A CN115710119A CN 115710119 A CN115710119 A CN 115710119A CN 202211510379 A CN202211510379 A CN 202211510379A CN 115710119 A CN115710119 A CN 115710119A
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- 238000001746 injection moulding Methods 0.000 title claims abstract description 128
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 108
- 238000005245 sintering Methods 0.000 claims abstract description 60
- 239000002245 particle Substances 0.000 claims abstract description 58
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 54
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 43
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 36
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- 238000000034 method Methods 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000010345 tape casting Methods 0.000 claims abstract description 26
- 238000000498 ball milling Methods 0.000 claims abstract description 25
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 23
- 238000012545 processing Methods 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 12
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005498 polishing Methods 0.000 claims abstract description 11
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 11
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 11
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 9
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 9
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 80
- 239000003570 air Substances 0.000 claims description 54
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 34
- 238000002347 injection Methods 0.000 claims description 24
- 239000007924 injection Substances 0.000 claims description 24
- 238000005266 casting Methods 0.000 claims description 22
- 238000000465 moulding Methods 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 12
- 239000004705 High-molecular-weight polyethylene Substances 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 9
- 238000003754 machining Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 239000004353 Polyethylene glycol 8000 Substances 0.000 claims description 7
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 7
- 229940085678 polyethylene glycol 8000 Drugs 0.000 claims description 7
- 235000019446 polyethylene glycol 8000 Nutrition 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- 239000011230 binding agent Substances 0.000 description 9
- 235000015895 biscuits Nutrition 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000004321 preservation Methods 0.000 description 9
- 238000000227 grinding Methods 0.000 description 7
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- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 3
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a preparation method of a ceramic arm based on a water-based injection molding process, which comprises the following steps: mixing polyethylene glycol, polymethyl methacrylate and ceramic raw materials, adding polyvinyl butyral and/or ethylene-vinyl acetate copolymer, and mixing to obtain a ceramic feed; cooling and crushing the ceramic feed to obtain feed particles; ball milling ethanol, ethyl acetate, butyl acetate, polyvinyl butyral, a plasticizer and sodium carbonate to obtain slurry; carrying out tape casting on the slurry to obtain a sodium carbonate-based tape casting sheet, and processing the sodium carbonate-based tape casting sheet into an air passage; and (3) performing injection molding on the feed particles and the sodium carbonate-based tape casting sheet with the shape of the air passage twice to obtain an injection molding blank, performing water degreasing, drying and sintering to obtain a ceramic sintered body with the air passage, and processing and polishing to obtain the ceramic arm. The method has simple process, can improve the yield, reduce the processing cost and obviously prolong the service life of the ceramic arm.
Description
Technical Field
The invention relates to the technical field of ceramic arm preparation, in particular to a preparation method of a ceramic arm based on a water-based injection molding process.
Background
The semiconductor chip is a device manufactured by taking a series of processing measures on a semiconductor substrate, plays a very key role in various industries at present, is the guarantee of the modern information society, and is widely applied to the aspects of life, industry, military, aerospace and the like. The manipulator is the core of the wafer transmission system and takes on the task of transmitting the wafer quickly, stably and efficiently. When the wafer is conveyed, the grabbing and placing actions of the ceramic arm are generally realized through vacuum adsorption and release, the wafer is required not to be damaged in the grabbing and placing processes of the arm, and any pollution cannot be brought to the whole production operation room.
Advanced ceramic materials are widely used for manufacturing ceramic arms for wafer transfer systems due to their excellent properties such as high melting point, high hardness, low thermal conductivity, chemical stability, and corrosion resistance. The existing ceramic arm preparation method mainly comprises the steps of firstly carrying out finish machining on ceramic plates by using a numerical control machine tool, and then combining the ceramic plates to form the ceramic arm with the air passage, wherein the ceramic plates are usually fixed by using a bonding agent. However, the high hardness and brittleness of the ceramic make the processing of the ceramic difficult, on one hand, brittle fracture easily occurs in the processing process, and on the other hand, the abrasion of the cutter makes the processing cost of the ceramic arm always high; in addition, the adhesive is gradually aged with the increase of the service time and is difficult to be used in severe environments such as high temperature, corrosion and the like, so that the service life of the ceramic arm is short.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a ceramic arm based on a water-based injection molding process, which has the advantages of simple process, capability of improving the yield, reducing the processing cost and obviously prolonging the service life of the ceramic arm.
In order to solve the above technical problems, the present invention proposes the following technical solutions.
A preparation method of a ceramic arm based on a water-based injection molding process comprises the following steps:
(1) Mixing polyethylene glycol, polymethyl methacrylate and ceramic raw materials, adding polyvinyl butyral and/or ethylene-vinyl acetate copolymer, and mixing to obtain a ceramic feed; the polyethylene glycol is high molecular weight polyethylene glycol or a mixture of high molecular weight polyethylene glycol and low molecular weight polyethylene glycol, the high molecular weight polyethylene glycol is selected from one or more of polyethylene glycol 2000 to polyethylene glycol 8000, the low molecular weight polyethylene glycol is selected from one or more of polyethylene glycol 200 to polyethylene glycol 600, wherein, according to the mass fraction, the high molecular weight polyethylene glycol is 5-35%, the low molecular weight polyethylene glycol is 0-5%, polymethyl methacrylate is 1-10%, ceramic raw material is 60-90%, polyvinyl butyral is 0-5%, ethylene-vinyl acetate copolymer is 0-5%, and the polyvinyl butyral and the ethylene-vinyl acetate copolymer are not 0 at the same time;
(2) Cooling and crushing the ceramic feed to obtain feed particles;
(3) Mixing ethanol, ethyl acetate, butyl acetate, polyvinyl butyral, a plasticizer and sodium carbonate, and carrying out ball milling to obtain slurry; wherein the mass ratio of ethanol to ethyl acetate to butyl acetate is 1: 0.2-1, the mass ratio of sodium carbonate to (ethanol + ethyl acetate + butyl acetate) to a ball milling medium is 1: 0.5-1.5: 1-3, the mass of the polyvinyl butyral is 5-15% of the mass of the sodium carbonate, and the mass of the plasticizer is 10-50% of the mass of the polyvinyl butyral;
(4) Carrying out tape casting on the slurry to obtain a sodium carbonate-based tape casting sheet, and then processing the sodium carbonate-based tape casting sheet into a preset air passage shape to obtain the sodium carbonate-based tape casting sheet with the air passage shape;
(5) Injecting and molding part of the feeding particles to obtain an injection molding semi-blank, then arranging a sodium carbonate-based tape casting sheet with an air flue shape on the injection molding semi-blank, and adding the other part of the feeding particles for secondary injection molding to obtain an injection molding blank;
(6) Soaking the injection molding blank body in water for water degreasing;
(7) And drying the blank after water degreasing, sintering at 1300-1700 ℃ to obtain a ceramic sintered body with an air passage, and processing and polishing the ceramic sintered body with the air passage to obtain the ceramic arm.
In the above method for preparing a ceramic arm based on a water-based injection molding process, preferably, the low molecular weight polyethylene glycol is polyethylene glycol 200, and the high molecular weight polyethylene glycol is polyethylene glycol 2000 and/or polyethylene glycol 8000.
In the above method for preparing a ceramic arm based on a water-based injection molding process, preferably, the specific process in step (5) is as follows:
(5.1) performing injection molding on part of the feed particles to obtain an injection molding semi-blank, wherein the injection molding temperature is 120-180 ℃, the injection pressure of the injection molding is 8-12 MPa, the molding pressure maintaining pressure is 6-8 MPa, and the molding pressure maintaining time is 5-30 s;
(5.2) after demolding, sticking the sodium carbonate based casting sheet with the shape of the air channel on the injection molding semi-blank;
(5.3) performing secondary injection molding on the other part of the feed particles by taking an injection molding semi-blank body adhered with the sodium carbonate based tape casting sheet with the shape of the air flue as a substrate to obtain an injection molding blank body, wherein the temperature of the secondary injection molding is 120-180 ℃, the injection pressure of the secondary injection molding is 8-12 MPa, the molding pressure maintaining pressure is 6-8 MPa, and the molding pressure maintaining time is 5-30 s.
In the above method for manufacturing a ceramic arm based on a water-based injection molding process, preferably, in the step (5), the mass ratio of one part of the feed particles to the other part of the feed particles is 0.3-0.7: 0.3-0.7.
In the above method for preparing a ceramic arm based on a water-based injection molding process, preferably, in step (1), the ceramic raw material includes one or more of alumina, zirconia, zinc oxide and titanium oxide.
In the above method for manufacturing a ceramic arm based on a water-based injection molding process, preferably, in step (3), the plasticizer is at least one of dibutyl phthalate, diethyl phthalate and dioctyl phthalate.
In the above preparation method of the ceramic arm based on the water-based injection molding process, preferably, in the step (6), the temperature of the water is 40-60 ℃, and the soaking time is 12-24 hours.
Preferably, in the step (1), the mixing temperature is 120-180 ℃, and the mixing time is 2-5 h; in the step (2), the crushing refers to crushing until the particle size is 3-5 mm.
Preferably, in the step (3), the ball milling medium is alumina balls or zirconia balls, and the ball milling time is 6 to 24 hours.
Preferably, in the step (4), in the casting process, the height of the scraper is 1 mm-3 mm, and the casting speed is 5 mm/s-30 mm/s.
In the above preparation method of the ceramic arm based on the water-based injection molding process, preferably, in the step (7), the drying temperature is 40-80 ℃, the sintering heat preservation time is 2-10 h, the sintering mode is vacuum sintering or normal pressure sintering, and the sintering atmosphere is at least one of air, nitrogen, argon and hydrogen; the machining is precise machining of a numerical control machine tool.
In the present invention, the molecular weight of the polyethylene glycol is generally an index average molecular weight, i.e., a molecular weight described in conventional commercial products, the high molecular weight polyethylene glycol is selected from one or more of polyethylene glycols having a molecular weight of 2000 to 8000, and the low molecular weight polyethylene glycol is selected from one or more of polyethylene glycols having a molecular weight of 200 to 600.
In the invention, the air passage is a conventional air passage in a ceramic arm, the shape of the air passage comprises a U shape, a Y shape, an I shape and the like, the cross section width of the air passage is between 0.5 and 1mm, and the cross section length is between 5 and 20mm, but the invention is not limited to the air passage.
Compared with the prior art, the invention has the advantages that:
(1) The invention uses polyethylene glycol as a binder with relatively low molecular weight, and polymethyl methacrylate, polyvinyl butyral and ethylene-vinyl acetate copolymer as a skeleton binder to prepare water-based (water-soaked) injection molding ceramic feed with high solid content and good dispersibility. Compared with wax-based injection molding, the low-molecular binder in water-based injection molding can be dissolved and removed by deionized water, a large amount of organic solvent is not used, and the low-molecular binder is harmless to human bodies and environment.
(2) Compared with the traditional method, the ceramic arm prepared by the injection molding process has the advantages of short molding period, high production efficiency and easiness in realizing automation, and is easy to realize batch production; more importantly, the injection molding can realize the molding with a near-static size, the ceramic arm can be obtained only by a small amount of processing after sintering, the ceramic arm processed by the prior art is mainly a processed ceramic plate, the appearance difference between the ceramic plate and the ceramic arm is large, and the ceramic arm can be processed by a plurality of procedures such as CNC (computerized numerical control) and plane grinding.
(3) The invention takes sodium carbonate and polyvinyl butyral as main raw materials, prepares the water-soluble film core through tape casting, combines the secondary injection molding process to obtain the injection molding blank body containing the ultrathin core, and can realize the ultrathin air passage of the ceramic arm after binder removal and sintering.
(4) The ceramic arm provided by the invention is prepared by an integral forming process, a bonding agent is not needed for bonding a ceramic plate to form an air passage, the air tightness is good, the corrosion resistance is more excellent, and the service life is longer.
Detailed Description
The invention is further described below with reference to specific preferred embodiments, without thereby limiting the scope of protection of the invention. The materials and equipment used in the following examples are commercially available.
Example 1
The invention relates to a preparation method of a ceramic arm based on a water-based injection molding process, which comprises the following steps:
(1) 18g of polyethylene glycol 200 (0.9%), 216g of polyethylene glycol 2000 (10.8%), 90g of polymethyl methacrylate (4.5%), 36g of ethylene-vinyl acetate copolymer (1.8%) and 1640g of alumina powder (82%) were weighed and mixed in an internal mixer at a temperature of 150 ℃ for 3 hours to obtain an alumina feed.
(2) The alumina feed was removed from the internal mixer and cooled and subsequently crushed using a jaw crusher into feed particles of 3-5mm in size.
(3) 60g of ethanol, 60g of ethyl acetate, 60g of butyl acetate, 20g of polyvinyl butyral, 8g of dioctyl phthalate, 180g of sodium carbonate and 540g of alumina balls are weighed and placed in a ball mill for ball milling to obtain slurry, wherein the ball milling time is 12 hours.
(4) The slurry was cast using a casting machine to obtain a sodium carbonate-based cast sheet having a thickness of 0.7mm and a width of 8mm, and then cut into a predetermined air passage shape using a cutting device (e.g., a wire cutter) with a blade height of 2mm and a casting speed of 20mm/s to obtain a sodium carbonate-based cast sheet having an air passage shape.
(5) And (3) injection molding the feed particles obtained in the step (2) and the sodium carbonate-based casting sheet with the airway shape obtained in the step (4) by using an injection molding machine to obtain an injection molding blank, wherein the injection molding blank comprises the following specific steps:
(5.1) pouring part of the feeding particles into a charging barrel of an injection molding machine, setting parameters, and performing injection molding to obtain an injection molding semi-blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the molding pressure maintaining pressure is 7MPa, and the pressure maintaining time is 15s;
(5.2) after demoulding, using a binder (such as 502 glue) to paste the sodium carbonate based casting sheet with the shape of the air flue on the injection molding semi-blank;
(5.3) pouring the other part of the feeding particles into the charging barrel of the injection molding machine again, and performing secondary injection molding by taking the injection molding semi-blank adhered with the sodium carbonate based tape casting sheet as a substrate to obtain an injection molding blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the molding pressure maintaining pressure is 7MPa, and the pressure maintaining time is 15s.
Wherein the mass ratio of one part of the feeding particles to the other part of the feeding particles is within the range of 0.3-0.7: 0.3-0.7.
(6) And soaking the injection molding blank in deionized water for water degreasing to remove sodium carbonate and polyethylene glycol, wherein the temperature of the deionized water is 40 ℃, and the soaking time is 18h.
(7) And (3) drying the blank degreased by water in an oven, and sintering in a sintering furnace to obtain the alumina ceramic sintered body with the air passage, wherein the oven temperature is 50 ℃, the sintering temperature is 1650 ℃, the heat preservation time is 5 hours, the sintering mode is normal-pressure sintering, and the sintering atmosphere is air. And (3) precisely machining and polishing the ceramic sintered body with the air passage by using a numerical control machine tool to obtain the alumina ceramic arm.
Example 2
The invention relates to a preparation method of a ceramic arm based on a water-based injection molding process, which comprises the following steps:
(1) 240g of polyethylene glycol 2000 (12%), 80g of polymethyl methacrylate (4%), 40g of polyvinyl butyral (2%), 40g of ethylene-vinyl acetate copolymer (2%) and 1600g of alumina powder (80%) are weighed and placed in an internal mixer for mixing to obtain an alumina feed, wherein the temperature of the internal mixer is 160 ℃, and the mixing time is 3 hours.
(2) The alumina feed was removed from the internal mixer and cooled and subsequently crushed using a jaw crusher into feed particles of 3-5mm in size.
(3) Weighing 90g of ethanol, 45g of ethyl acetate, 45g of butyl acetate, 18g of polyvinyl butyral, 6g of dibutyl phthalate, 180g of sodium carbonate and 360g of alumina balls, and placing the mixture in a ball mill for ball milling to obtain slurry, wherein the ball milling time is 24 hours.
(4) The slurry was cast using a casting machine to obtain a sodium carbonate-based cast sheet, which was then cut into a gas channel shape using a cutting device with a blade height of 2mm and a casting speed of 20mm/s.
(5) And (2) injection molding the feed particles and the sodium carbonate based tape casting sheet with the shape of the air flue by using an injection molding machine to obtain an injection molding blank, which comprises the following specific steps:
(5.1) pouring part of the feeding particles into a charging barrel of an injection molding machine, setting parameters, and performing injection molding to obtain an injection molding semi-blank, wherein the injection temperature is 150 ℃, the injection pressure is 12MPa, the pressure maintaining pressure is 8MPa, and the pressure maintaining time is 15s;
(5.2) after demolding, using a binder to paste the sodium carbonate based casting sheet with the shape of the air flue on the injection molding semi-blank;
(5.3) pouring the other part of the feeding particles into the charging barrel of the injection molding machine again, and performing secondary injection molding by taking the injection molding semi-blank adhered with the sodium carbonate based tape casting sheet as a substrate to obtain an injection molding blank, wherein the injection temperature is 150 ℃, the injection pressure is 12MPa, the pressure maintaining pressure is 8MPa, and the pressure maintaining time is 15s.
(6) And soaking the injection molding blank in deionized water for water degreasing to remove sodium carbonate and polyethylene glycol, wherein the temperature of the deionized water is 40 ℃, and the soaking time is 24 hours.
Wherein the mass ratio of one part of the feeding particles to the other part of the feeding particles is within the range of 0.3-0.7: 0.3-0.7.
(7) And (3) drying the blank degreased by water in an oven, and sintering in a sintering furnace to obtain the alumina ceramic sintered body with the air passage, wherein the oven temperature is 60 ℃, the sintering temperature is 1650 ℃, the heat preservation time is 5 hours, the sintering mode is normal-pressure sintering, and the sintering atmosphere is air. And (3) precisely machining and polishing the ceramic sintered body with the air passage by using a numerical control machine tool to obtain the alumina ceramic arm.
Example 3
The invention relates to a preparation method of a ceramic arm based on a water-based injection molding process, which comprises the following steps:
(1) 221g of polyethylene glycol 2000 (11.1%), 34g of polyethylene glycol 8000 (1.7%), 85g of polymethyl methacrylate (4.3%), 1500g of alumina powder (75.4%) and 150g of titanium oxide powder (7.5%) were weighed and mixed in an internal mixer at 140 ℃ for 3 hours to obtain a ceramic feed.
(2) The ceramic feed was removed from the internal mixer and cooled and subsequently crushed using a jaw crusher into feed particles having a particle size of 3-5 mm.
(3) Weighing 90g of ethanol, 60g of ethyl acetate, 30g of butyl acetate, 20g of polyvinyl butyral, 6g of dibutyl phthalate, 200g of sodium carbonate and 500g of alumina balls, and placing the mixture into a ball mill for ball milling to obtain slurry, wherein the ball milling time is 24 hours.
(4) The slurry was cast using a casting machine to obtain a sodium carbonate-based cast sheet, which was then cut into a gas channel shape using a cutting device with a blade height of 2mm and a casting speed of 20mm/s.
(5) And (2) injection molding the feed particles and the sodium carbonate based tape casting sheet with the shape of the air flue by using an injection molding machine to obtain an injection molding blank, which comprises the following specific steps:
(5.1) pouring part of the feed particles into a charging barrel of an injection molding machine, setting parameters, and performing injection molding to obtain an injection molding semi-blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the pressure maintaining pressure is 6MPa, and the pressure maintaining time is 15s;
(5.2) after demolding, using a binder to paste the sodium carbonate based casting sheet with the shape of the air flue on the injection molding semi-blank;
(5.3) pouring the other part of the feeding particles into the charging barrel of the injection molding machine again, and performing secondary injection molding by taking the injection molding semi-blank adhered with the sodium carbonate based tape casting sheet as a substrate to obtain an injection molding blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the pressure maintaining pressure is 6MPa, and the pressure maintaining time is 15s.
Wherein the mass ratio of one part of the feeding particles to the other part of the feeding particles is within the range of 0.3-0.7: 0.3-0.7.
(6) And soaking the injection molding blank in deionized water for degreasing to remove sodium carbonate and polyethylene glycol, wherein the temperature of the deionized water is 40 ℃, and the soaking time is 24 hours.
(7) And (3) drying the blank degreased by water in an oven, embedding the dried blank into graphite powder, and sintering the blank in a sintering furnace to obtain the aluminum oxide anti-static ceramic sintered body with the air passage, wherein the oven temperature is 50 ℃, the sintering temperature is 1400 ℃, the heat preservation time is 5 hours, and the sintering mode is vacuum sintering. And precisely processing and polishing the ceramic sintered body with the air passage by using a numerical control machine tool to obtain the alumina-based anti-static ceramic arm.
Example 4
The invention relates to a preparation method of a ceramic arm based on a water-based injection molding process, which comprises the following steps:
(1) 15g of polyethylene glycol 200 (0.75%), 195g of polyethylene glycol 2000 (9.75%), 15g of polyethylene glycol 8000 (0.75), 45g of polymethyl methacrylate (2.25%), 30g of polyvinyl butyral (1.5%) and 1700g of zirconia powder (3YSZ, 85%) were weighed out and mixed in an internal mixer at 140 ℃ for 3 hours to obtain zirconia feed.
(2) The zirconia feed was removed from the internal mixer and cooled and subsequently crushed using a jaw crusher into feed particles of 3-5mm in size.
(3) 60g of ethanol, 60g of ethyl acetate, 60g of butyl acetate, 20g of polyvinyl butyral, 6g of dibutyl phthalate, 200g of sodium carbonate and 600g of zirconia balls are weighed and placed in a ball mill for ball milling to obtain slurry, wherein the ball milling time is 18 hours.
(4) The slurry was cast using a casting machine to obtain a sodium carbonate-based cast sheet, which was then cut into a gas channel shape using a cutting device with a blade height of 2mm and a casting speed of 20mm/s.
(5) And (2) injection molding the feed particles and the sodium carbonate based tape casting sheet with the shape of the air flue by using an injection molding machine to obtain an injection molding blank, which comprises the following specific steps:
(5.1) pouring part of the feeding particles into a charging barrel of an injection molding machine, setting parameters, and performing injection molding to obtain an injection molding semi-blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the pressure maintaining pressure is 8MPa, and the pressure maintaining time is 20s;
(5.2) after demolding, adhering the sodium carbonate based casting sheet with the shape of the air channel to the injection molding semi-blank by using an adhesive;
(5.3) pouring the other part of the feeding particles into the charging barrel of the injection molding machine again, and performing secondary injection molding by taking the injection molding semi-blank adhered with the sodium carbonate based tape casting sheet as a substrate to obtain an injection molding blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the pressure maintaining pressure is 8MPa, and the pressure maintaining time is 20s.
Wherein the mass ratio of one part of the feeding particles to the other part of the feeding particles is within the range of 0.3-0.7: 0.3-0.7.
(6) And soaking the injection molding blank in deionized water for water degreasing to remove sodium carbonate and polyethylene glycol, wherein the temperature of the deionized water is 40 ℃, and the soaking time is 24 hours.
(7) And (3) drying the blank degreased by water in an oven, and sintering in a sintering furnace to obtain the zirconia ceramic sintered body with the air passage, wherein the oven temperature is 50 ℃, the sintering temperature is 1490 ℃, the heat preservation time is 3 hours, the sintering mode is normal-pressure sintering, and the sintering atmosphere is air. And precisely machining and polishing the zirconia sintered body with the air passage by using a numerical control machine tool to obtain the zirconia ceramic arm.
Example 5
The invention relates to a preparation method of a ceramic arm based on a water-based injection molding process, which comprises the following steps:
(1) 15g of polyethylene glycol 200 (0.75%), 195g of polyethylene glycol 2000 (9.75%), 15g of polyethylene glycol 8000 (0.75%), 45g of polymethyl methacrylate (2.25%), 30g of polyvinyl butyral (1.5%), 1350g of zirconia powder (5 YSZ) (67.5%) and 350g of zinc oxide powder (17.5%) were weighed and mixed in an internal mixer at a temperature of 140 ℃ for 3 hours to obtain a ceramic feed.
(2) The ceramic feed was removed from the internal mixer and cooled and subsequently crushed using a jaw crusher into feed particles of 3-5mm in size.
(3) 60g of ethanol, 60g of ethyl acetate, 60g of butyl acetate, 20g of polyvinyl butyral, 6g of dibutyl phthalate, 200g of sodium carbonate and 600g of zirconia balls are weighed and placed in a ball mill for ball milling to obtain slurry, wherein the ball milling time is 24 hours.
(4) The slurry was cast using a casting machine to obtain a sodium carbonate-based cast sheet, which was then cut into a gas channel shape using a cutting device with a blade height of 2mm and a casting speed of 20mm/s.
(5) And (2) injection molding the feed particles and the sodium carbonate based tape casting sheet with the shape of the air flue by using an injection molding machine to obtain an injection molding blank, which comprises the following specific steps:
(5.1) pouring part of the feeding particles into a charging barrel of an injection molding machine, setting parameters, and then carrying out injection molding to obtain an injection molding semi-blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the pressure maintaining pressure is 8MPa, and the pressure maintaining time is 20s;
(5.2) after demolding, adhering the sodium carbonate based casting sheet with the shape of the air channel to the injection molding semi-blank by using an adhesive;
(5.3) pouring the other part of the feeding particles into the charging barrel of the injection molding machine again, and performing secondary injection molding by taking the injection molding semi-blank adhered with the sodium carbonate based tape casting sheet as a substrate to obtain an injection molding blank, wherein the injection temperature is 140 ℃, the injection pressure is 10MPa, the pressure maintaining pressure is 8MPa, and the pressure maintaining time is 20s.
Wherein the mass ratio of one part of the feeding particles to the other part of the feeding particles is within the range of 0.3-0.7: 0.3-0.7.
(6) And soaking the injection molding blank in deionized water for water degreasing to remove sodium carbonate and polyethylene glycol, wherein the temperature of the deionized water is 40 ℃, and the soaking time is 24 hours.
(7) And (3) drying the blank degreased by water in an oven, and sintering in a sintering furnace to obtain the zirconia antistatic ceramic sintered body with the air passage, wherein the oven temperature is 50 ℃, the sintering temperature is 1300 ℃, the heat preservation time is 3 hours, the sintering mode is air pressure sintering, the sintering atmosphere is nitrogen, and the sintering pressure is 5MPa. And precisely processing and polishing the ceramic sintered body with the air passage by using a numerical control machine tool to obtain the zirconia anti-static ceramic arm.
Comparative example 1
A preparation method of a ceramic arm comprises the following steps:
(1) Weighing 5000g of alumina powder, 5000g of deionized water, 25g of polyvinyl alcohol and 15000g of alumina balls, placing the weighed materials in a drum-type ball milling tank, and carrying out ball milling for 24 hours to obtain ceramic slurry;
(2) Carrying out spray granulation and drying on the ceramic slurry to obtain spherical alumina raw material particles, wherein the temperature of a spray drying tower is 230 ℃, the temperature of an oven is 50 ℃, and the particle size distribution is 50-150 microns;
(3) Carrying out dry pressing-isostatic pressing on the spherical alumina raw material particles to obtain an alumina ceramic biscuit, wherein the dry pressing pressure is 50MPa, the pressure maintaining time is 5 minutes, the isostatic pressing pressure is 150MPa, the pressure maintaining time is 15 minutes, and the size of the biscuit is 400mm multiplied by 150mm multiplied by 20mm;
(4) Placing the alumina ceramic biscuit in a silicon-molybdenum rod furnace for sintering to obtain an alumina ceramic plate, wherein the sintering temperature is 1650 ℃, the heat preservation time is 3 hours, the sintering mode is normal pressure sintering, and the sintering atmosphere is air;
(5) And taking out the two alumina ceramic plates, grinding the two alumina ceramic plates by using a plane grinder until the thickness of the two alumina ceramic plates reaches 2mm, processing the two alumina ceramic plates by using fine processing and polishing equipment such as a numerical control machine tool and the like after grinding, and finally bonding the two ceramic plates by using a bonding agent to obtain the alumina ceramic arm.
Comparative example 2
A preparation method of a ceramic arm comprises the following steps:
(1) Weighing 5000g of zirconia (3 YSZ) powder, 4000g of deionized water, 25g of polyvinyl alcohol and 15000g of zirconia balls, placing the materials in a roller type ball milling tank, and carrying out ball milling for 24 hours to obtain ceramic slurry;
(2) Carrying out spray granulation and drying on the ceramic slurry to obtain spherical zirconium oxide raw material particles, wherein the temperature of a spray drying tower is 230 ℃, the temperature of an oven is 50 ℃, and the particle size distribution is 50-150 microns;
(3) Carrying out dry pressing-isostatic pressing on the spherical zirconia raw material particles to obtain a zirconia ceramic biscuit, wherein the dry pressing pressure is 50MPa, the pressure maintaining time is 5 minutes, the isostatic pressing pressure is 150MPa, the pressure maintaining time is 15 minutes, and the size of the biscuit is 400mm multiplied by 150mm multiplied by 20mm;
(4) Placing the zirconia ceramic biscuit in a silicon-molybdenum rod furnace for sintering to obtain a zirconia ceramic plate, wherein the sintering temperature is 1490 ℃, the heat preservation time is 3 hours, the sintering mode is normal pressure sintering, and the sintering atmosphere is air;
(5) And taking out the two zirconia ceramic plates, grinding the two zirconia ceramic plates by using a plane grinder to enable the thickness of the two zirconia ceramic plates to reach 2mm, processing the two zirconia ceramic plates by using fine processing and polishing equipment such as a numerical control machine tool and the like after grinding, and finally bonding the two ceramic plates by using a bonding agent to obtain the zirconia ceramic arm.
Comparative example 3
A preparation method of a ceramic arm comprises the following steps:
(1) Weighing 7500g of zirconia (5 YSZ) powder, 1500g of zinc oxide powder, 7500g of deionized water, 50g of polyvinyl alcohol and 27000g of zirconia balls, placing the materials in a roller type ball milling tank, and performing ball milling for 24 hours to obtain ceramic slurry;
(2) Carrying out spray granulation and drying on the ceramic slurry to obtain spherical anti-static ceramic raw material particles, wherein the temperature of a spray drying tower is 230 ℃, the temperature of an oven is 50 ℃, and the particle size distribution is 50-150 microns;
(3) Carrying out dry pressing-isostatic pressing on the spherical antistatic raw material particles to obtain an antistatic ceramic biscuit, wherein the dry pressing pressure is 50MPa, the pressure maintaining time is 5 minutes, the isostatic pressing pressure is 150MPa, the pressure maintaining time is 15 minutes, and the size of the biscuit is 400mm multiplied by 150mm multiplied by 20mm;
(4) Placing the anti-static ceramic biscuit in a silicon-molybdenum rod furnace for sintering to obtain a zirconia anti-static ceramic plate, wherein the sintering temperature is 1300 ℃, the heat preservation time is 3 hours, the sintering mode is air pressure sintering, and the sintering atmosphere is nitrogen;
(5) And taking out the two zirconia anti-static ceramic plates, grinding the two zirconia anti-static ceramic plates by using a plane grinder to enable the thickness of the two zirconia anti-static ceramic plates to reach 2mm, processing the two zirconia anti-static ceramic plates by using fine processing and polishing equipment such as a numerical control machine tool after grinding, and finally bonding the two ceramic plates by using a bonding agent to obtain the zirconia anti-static ceramic arm.
The density of the ceramics of examples 1 to 5 and comparative examples 1 to 3 was tested by the archimedes drainage method; the bending strength of the ceramics of examples 1 to 5 and comparative examples 1 to 3 was measured by a three-point bending method; the vickers hardness of the ceramics of examples 1 to 5 and comparative examples 1 to 3 was measured using a vickers hardness tester; the ceramic arms provided in examples 1-5 and comparative example 3 were tested for air tightness after 90 days of use; the results are shown in Table 1.
TABLE 1 Performance test tables for examples 1 to 5 and comparative examples 1 to 3
Among the above examples and comparative examples, alumina ceramics were prepared in examples 1 to 3 and comparative example 1, zirconia ceramics were prepared in example 4 and comparative example 2, and zirconia antistatic ceramics were prepared in example 5 and comparative example 3. As can be seen from Table 1, the density of the alumina ceramics of examples 1 to 3 is at least 99.1%, the bending strength is at least 423MPa, the Vickers hardness is at least 16.7GPa, the density of the zirconia ceramics of example 4 is 99.4%, the hardness is 12.4GPa, the bending strength is 912MPa, the density of the zirconia antistatic ceramics provided by example 5 is 97.3%, the hardness is 9.3GPa, and the bending strength is 387MPa, compared with the alumina, zirconia and zirconia antistatic ceramics respectively provided by comparative examples 1 to 3, the mechanical properties of the ceramics provided by examples 1 to 5 are not obviously reduced, which indicates that the method provided by the invention can prepare ceramic materials with excellent performance, and is suitable for industrial production. Comparing the airtightness of the ceramic arms provided in examples 1 to 5 and comparative examples 1 to 3 after 90 days of use, it can be seen that the airtightness was excellent after 90 days of use in examples 1 to 5, while the airtightness was poor after 90 days of use in comparative examples 1 to 3 due to the failure of the binder. Therefore, the ceramic arm preparation method based on water-based injection molding provided by the invention can be used for preparing the ceramic arm with excellent mechanical property, and compared with the ceramic arm prepared by the traditional method, the ceramic arm provided by the invention is simple in production process, suitable for industrial production and capable of saving a large amount of processing cost, and more importantly, the ceramic arm provided by the invention can be used in a harsher environment and has a longer service life.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (10)
1. A preparation method of a ceramic arm based on a water-based injection molding process is characterized by comprising the following steps:
(1) Mixing polyethylene glycol, polymethyl methacrylate and ceramic raw materials, adding polyvinyl butyral and/or ethylene-vinyl acetate copolymer, and mixing to obtain a ceramic feed; the polyethylene glycol is high molecular weight polyethylene glycol or a mixture of high molecular weight polyethylene glycol and low molecular weight polyethylene glycol, the high molecular weight polyethylene glycol is selected from one or more of polyethylene glycol 2000 to polyethylene glycol 8000, the low molecular weight polyethylene glycol is selected from one or more of polyethylene glycol 200 to polyethylene glycol 600, wherein the high molecular weight polyethylene glycol accounts for 5-35% by mass, the low molecular weight polyethylene glycol accounts for 0-5% by mass, the polymethyl methacrylate accounts for 1-10% by mass, the ceramic raw material accounts for 60-90% by mass, the polyvinyl butyral accounts for 0-5% by mass, and the ethylene-vinyl acetate copolymer accounts for 0-5% by mass;
(2) Cooling and crushing the ceramic feed to obtain feed particles;
(3) Mixing ethanol, ethyl acetate, butyl acetate, polyvinyl butyral, a plasticizer and sodium carbonate, and carrying out ball milling to obtain slurry; wherein the mass ratio of ethanol to ethyl acetate to butyl acetate is 1: 0.2-1, the mass ratio of sodium carbonate to (ethanol + ethyl acetate + butyl acetate) to ball milling medium is 1: 0.5-1.5: 1-3, the mass of the polyvinyl butyral is 5-15% of the mass of the sodium carbonate, and the mass of the plasticizer is 10-50% of the mass of the polyvinyl butyral;
(4) Carrying out tape casting on the slurry to obtain a sodium carbonate-based tape casting sheet, and then processing the sodium carbonate-based tape casting sheet into a preset air passage shape to obtain the sodium carbonate-based tape casting sheet with the air passage shape;
(5) Injecting and molding part of the feeding particles to obtain an injection molding semi-blank, then arranging a sodium carbonate-based tape casting sheet with an air flue shape on the injection molding semi-blank, and then adding the other part of the feeding particles for secondary injection molding to obtain an injection molding blank;
(6) Soaking the injection molding blank body in water for water degreasing;
(7) And drying the blank after water degreasing, sintering at 1300-1700 ℃ to obtain a ceramic sintered body with an air passage, and processing and polishing the ceramic sintered body with the air passage to obtain the ceramic arm.
2. The method for preparing a ceramic arm according to claim 1, wherein the low molecular weight polyethylene glycol is polyethylene glycol 200, and the high molecular weight polyethylene glycol is polyethylene glycol 2000 and/or polyethylene glycol 8000.
3. The method for preparing a ceramic arm based on a water-based injection molding process according to claim 1, wherein the specific process in the step (5) is as follows:
(5.1) performing injection molding on part of the feed particles to obtain an injection molding semi-blank, wherein the injection molding temperature is 120-180 ℃, the injection pressure of the injection molding is 8-12 MPa, the molding pressure maintaining pressure is 6-8 MPa, and the molding pressure maintaining time is 5-30 s;
(5.2) after demolding, sticking the sodium carbonate based casting sheet with the shape of the air channel on the injection molding semi-blank;
(5.3) performing secondary injection molding on the other part of the feed particles by taking an injection molding semi-blank body adhered with the sodium carbonate based tape casting sheet with the shape of the air flue as a substrate to obtain an injection molding blank body, wherein the temperature of the secondary injection molding is 120-180 ℃, the injection pressure of the secondary injection molding is 8-12 MPa, the molding pressure maintaining pressure is 6-8 MPa, and the molding pressure maintaining time is 5-30 s.
4. The method for preparing a ceramic arm based on a water-based injection molding process as claimed in claim 1, wherein the mass ratio of the part of the feed particles to the other part of the feed particles in step (5) is 0.3-0.7: 0.3-0.7.
5. The method for preparing a ceramic arm based on a water-based injection molding process according to any one of claims 1 to 3, wherein in the step (1), the ceramic raw material comprises one or more of alumina, zirconia, zinc oxide and titanium oxide; in the step (3), the plasticizer is at least one of dibutyl phthalate, diethyl phthalate and dioctyl phthalate.
6. The method for preparing a ceramic arm based on a water-based injection molding process according to any one of claims 1 to 3, wherein the temperature of the water is 40 ℃ to 60 ℃ and the soaking time is 12h to 24h in step (6).
7. The method for preparing a ceramic arm based on a water-based injection molding process according to any one of claims 1 to 3, wherein in the step (1), the mixing temperature is 120 ℃ to 180 ℃, and the mixing time is 2h to 5h; in the step (2), the crushing refers to crushing until the particle size is 3-5 mm.
8. The method for preparing a ceramic arm based on a water-based injection molding process according to any one of claims 1 to 3, wherein in the step (3), the ball milling medium is alumina balls or zirconia balls, and the ball milling time is 6-24 h.
9. The method for preparing a ceramic arm based on a water-based injection molding process according to any one of claims 1 to 3, wherein in the step (4), the height of the scraper is 1mm to 3mm and the casting speed is 5mm/s to 30mm/s during the casting process.
10. The method for preparing a ceramic arm based on a water-based injection molding process according to any one of claims 1 to 3, wherein in the step (7), the drying temperature is 40 ℃ to 80 ℃, the sintering holding time is 2h to 10h, the sintering mode is vacuum sintering or normal pressure sintering, and the sintering atmosphere is at least one of air, nitrogen, argon and hydrogen; the machining is precise machining of a numerical control machine tool.
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