CN111533540A - Preparation method of alumina ceramic with complex shape - Google Patents
Preparation method of alumina ceramic with complex shape Download PDFInfo
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- CN111533540A CN111533540A CN202010361831.7A CN202010361831A CN111533540A CN 111533540 A CN111533540 A CN 111533540A CN 202010361831 A CN202010361831 A CN 202010361831A CN 111533540 A CN111533540 A CN 111533540A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000919 ceramic Substances 0.000 claims abstract description 54
- 239000002002 slurry Substances 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000005266 casting Methods 0.000 claims abstract description 29
- 235000015895 biscuits Nutrition 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 239000000178 monomer Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 239000002270 dispersing agent Substances 0.000 claims abstract description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000005350 fused silica glass Substances 0.000 claims description 9
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical group CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 9
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical group CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 8
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 3
- 235000011046 triammonium citrate Nutrition 0.000 claims description 3
- 239000001393 triammonium citrate Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract description 4
- 238000005303 weighing Methods 0.000 description 17
- 238000000498 ball milling Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000462 isostatic pressing Methods 0.000 description 5
- 238000007569 slipcasting Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention belongs to the technical field of alumina ceramic molding, and particularly relates to a preparation method of alumina ceramic with a complex shape. The method comprises the following steps: (1) preparing a premixed solution: mixing water, a monomer, a cross-linking agent and a dispersing agent, and stirring for dissolving to obtain a premixed solution; (2) preparation of alumina gel casting slurry: uniformly mixing alumina powder, silica powder and premixed liquid to obtain slurry, wherein the mass ratio of the alumina powder to the silica powder to the premixed liquid is 60:40-95: 5; (3) adding a catalyst and an initiator: adding a catalyst and an initiator into the slurry, and uniformly mixing; (4) gel casting: transferring the slurry obtained in the step (3) into a mold, curing at room temperature or heating for curing, cooling, demolding and drying to obtain a ceramic biscuit; (5) firing the ceramic: and sintering the ceramic biscuit. The product prepared by the method has the shrinkage rate of less than 5 percent, higher density and strength, low production cost and high yield.
Description
Technical Field
The invention belongs to the technical field of alumina ceramic molding, and particularly relates to a preparation method of alumina ceramic with a complex shape.
Background
The alumina ceramic is prepared from alumina (Al)2O3) Ceramic materials, which are the main body, are widely used in many industrial fields due to their excellent properties, and have outstanding advantages of high hardness (second to diamond), good wear resistance, corrosion resistance, and the like. The high-purity alumina ceramic can be made into a high-temperature crucible, can be used for preparing a sodium lamp tube by utilizing the characteristics of high temperature resistance and corrosion resistance, and can also be applied to the electronic industry as an integrated circuit substrate and the like. The common alumina ceramic can be used as refractory material for making ceramic bearings, valve plates, etc.
The existing ceramic forming technology mainly comprises: dry pressing, plastic forming, isostatic pressing, slip casting, gel casting, and the like. The dry pressing forming is mainly applied to the forming preparation of simple and regular sheet-shaped and block-shaped ceramics, and the forming process has the characteristics of simple and quick forming and has the defects of low strength of a formed blank body and incapability of forming ceramic products with complex shapes. The plastic forming needs the ceramic raw material to have certain plasticity for use, and can only form regular barrel-shaped or sheet-shaped ceramics, and the complicated special-shaped ceramics cannot use the method. In view of the current ceramic development, more and more products require ceramics to have a profiled structure. Isostatic compaction, slip casting and gel casting can be used for forming and preparing ceramics with complex shapes. Isostatic pressing requires relatively complicated isostatic pressing equipment, the price of the isostatic pressing equipment is increased when the ceramic is large in size, and trimming of the ceramic blank is generally required after isostatic pressing. Slip casting is a method for molding ceramics with complex shapes by applying more methods, but the method has the inherent defects of long slurry drying time and low production efficiency, and when the ceramic with a larger size is molded, the uniformity of the ceramic is adversely affected by different drying rates inside and outside a blank. Gel casting is a ceramic forming technique developed on the basis of slip casting. The method has the advantages that the complicated special-shaped ceramics can be formed, expensive equipment is not needed, only corresponding dies are needed, and the method realizes forming through organic matter curing, has no problem of drying rate compared with slip casting, has high forming efficiency and large blank strength, and can carry out proper machining treatment. The product size is not limited by the equipment size, and the large-size and complex-shape ceramic can be prepared.
Although the declaration of the method in the early stage of the development of gel-casting can realize near-net-size forming, the current academic papers and engineering practice are that the organic matter is removed in the form of gas during the gel-discharging process due to the presence of solvent and organic matter in the gel-casting slurry, and the size shrinkage of the gel-casting green body after sintering is inevitable compared with the size of the mold. For simple shaped ceramic articles, the effect of shrinkage can be partially offset by appropriate enlargement of the die size, leaving a margin in advance. However, for the ceramic products with complex shapes, the shrinkage rate of the blank in each direction is different, which inevitably causes the distortion of the product shape, and the preparation of products with ideal shapes cannot be well completed. Therefore, how to achieve low-shrinkage preparation of ceramic products using the gel-casting method is a very important scientific and engineering problem.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the preparation method of the alumina ceramic with the complex shape, the shrinkage rate of the product prepared by the method is less than 5%, and the product has higher density and strength, low production cost and high yield.
The technical scheme adopted by the invention is as follows:
the preparation method of the alumina ceramic with the complex shape can prepare the special-shaped ceramic with the complex shape by adopting a gel casting process, the solid content of the gel casting slurry is high, and the alumina ceramic powder is added with proper silica powder to realize the preparation of the alumina ceramic with the complex shape and low shrinkage.
According to the preparation method of the alumina ceramic with the complex shape, after the alumina ceramic manufactured by the method is molded and sintered, the shrinkage rate of a product is less than 5%, and the method comprises the following steps:
(1) preparing a premixed solution: mixing water, a monomer, a cross-linking agent and a dispersing agent, and stirring for dissolving to obtain a premixed solution;
(2) preparation of alumina gel casting slurry: uniformly mixing alumina powder, silica powder and premixed liquid to obtain slurry, wherein the mass ratio of the alumina powder to the silica powder to the premixed liquid is 60:40-95: 5;
(3) adding a catalyst and an initiator: adding a catalyst and an initiator into the slurry, and uniformly mixing;
(4) gel casting: transferring the slurry obtained in the step (3) into a mold, curing at room temperature or heating for curing, cooling, demolding and drying to obtain a ceramic biscuit;
(5) firing the ceramic: and sintering the ceramic biscuit.
Wherein:
complex shapes refer to regular shapes other than simple long sheets, cylinders, discs, blocks, etc., which typically have variable cross-sections, such as variable cross-section round or square tubes. The complex shape also includes the combination of complex curved surfaces, such as heating tiles with semi-arc shaped configuration and sawtooth grooves on the outer side, impeller shape, gear shape and the like.
In the step (1), the monomer is methacrylamide, the cross-linking agent is N, N' -methylene bisacrylamide, and the dispersing agent is one or more of polyvinylpyrrolidone, polyvinyl alcohol, ammonium polyacrylate or triammonium citrate, preferably polyvinylpyrrolidone. The content of each component in the premix is as follows: 69-93.2 wt% of water, 5-20 wt% of monomer, 0.3-3 wt% of cross-linking agent and 1.5-8 wt% of dispersing agent. The mass ratio of the monomer to the cross-linking agent is about 5-20: 1.
In the step (2), the mass ratio of the alumina powder, the silica powder and the premixed liquid is 65:35-95: 5. Preferably, the silicon oxide powder is fused quartz, and the mass ratio of the fused quartz to the aluminum oxide powder is 5-40%.
In the step (2), when the alumina gel casting slurry is prepared, the premixed solution is added into the alumina powder and the silicon oxide powder, and the mixture is stirred and mixed uniformly by adopting a ball mill or a mechanical stirrer, wherein the ball milling or mechanical stirring time is 0.3-24 h.
In the step (3), the catalyst is tetramethylethylenediamine which accounts for 0.01-0.4 wt% of the premixed liquid according to the mass ratio, and the initiator is ammonium persulfate or potassium persulfate which accounts for 0.02-1 wt% of the premixed liquid according to the mass ratio. And during mixing, ball milling is carried out by adopting a ball mill or stirring is carried out by adopting a mechanical stirrer, and the mixing time of ball milling or mechanical stirring is 3-30 minutes.
Preferably, before or after step (3), exhausting is performed in a manner that: ultrasonic or vacuum exhaust.
In the step (4), after the slurry is transferred to the die, the die is placed in an environment with the temperature of 40-80 ℃, and the temperature is kept for 10 minutes to 6 hours until the blank is completely cured. The curing temperature can also be adjusted to finally achieve room temperature curing by the catalyst.
In the step (4), drying can be selected from room temperature drying and controllable drying. Preferably, the green body is dried in an environment with controllable temperature and humidity, wherein the environment humidity is more than 85%, and after drying for 2-48 hours, the green body is dried in the air for 2-72 hours at room temperature.
In the step (5), the sintering temperature of the ceramic biscuit is 1200-1650 ℃, and the temperature is kept for 1-6 h.
Preferably, after the alumina ceramic manufactured by the method is formed and sintered, the shrinkage rate of the product is less than 3%.
Compared with the prior art, the invention has the following beneficial effects:
1. the alumina slurry has high solid content, reduces the size shrinkage and cracking in the sintering process of ceramic biscuit, can conveniently realize the molding sintering of the ceramic with complex shape, and avoids the problem that the ceramic with complex shape cannot be molded with accurate size due to excessive shrinkage, and even the product is deformed and deviates from the design due to shrinkage. The solid content is improved, the solvent amount in the biscuit can be reduced, the volume shrinkage in the drying process of the biscuit body is effectively reduced, the shrinkage rate of the product prepared by the method is less than 5%, the deformation of the biscuit body due to shrinkage is avoided, the compactness and the strength are higher, the production cost is low, and the yield is high.
2. And a proper amount of silicon oxide powder is added as an expanding agent, mullite is synthesized in the sintering process, a certain amount of volume expansion is generated, the shrinkage of a green body in the sintering process is counteracted, the shrinkage of a sintered body is reduced, meanwhile, the generated mullite is also a high-temperature phase, the high-temperature performance of a product is not influenced, the expansion coefficient of the mullite phase is low, and the thermal shock resistance of the material is better facilitated.
3. And the methacrylamide monomer is adopted, so that the toxic acrylamide monomer is avoided, and the industrial production is more friendly.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
The starting materials used in the examples are all commercially available except where otherwise indicated.
The gear shape is exemplified as a complex shape in the embodiment.
Example 1
The preparation method of the gear-shaped alumina ceramic comprises the following steps:
(1) preparing a premixed solution: 20mL of water is weighed, 3g of methacrylamide, 0.3g of N, N' -methylene bisacrylamide and 0.9g of ammonium polyacrylate are weighed and placed in a beaker to be stirred and dissolved at room temperature, and a premixed solution is obtained.
(2) Preparation of alumina gel casting slurry: weighing 40g of alumina powder, 3g of fused quartz and the premixed liquid obtained in the step (1), adding into a ball mill, and ball-milling and mixing for 3h to obtain alumina ceramic slurry.
(3) Adding a catalyst and an initiator: weighing 0.012g of potassium persulfate, weighing 12 mu L of tetramethylethylenediamine, adding into the alumina ceramic slurry obtained in the step (2), ball-milling and mixing for 20min, and vacuumizing and exhausting for 15 min.
(4) Gel casting: and (4) transferring the slurry obtained in the step (3) into a gear mold, heating to 50 ℃, curing for 40min, and cooling and demolding after complete curing. And (3) dehydrating the demoulded blank body for 20h at the humidity of 90%, and then placing the demoulded blank body at room temperature for continuously drying for 20h to obtain a ceramic biscuit.
(5) Firing the ceramic: and (4) placing the ceramic biscuit obtained in the step (4) in a sintering furnace, heating to 1600 ℃, preserving heat for 3h, and cooling along with the furnace to obtain the alumina ceramic gear.
Example 2
The preparation method of the gear-shaped alumina ceramic comprises the following steps:
(1) preparing a premixed solution: 40mL of water is measured, 8g of methacrylamide, 0.5g of N, N' -methylenebisacrylamide and 3g of triammonium citrate are weighed and placed in a beaker to be stirred and dissolved at room temperature, and a premixed solution is obtained.
(2) Preparation of alumina gel casting slurry: 105g of alumina powder, 21g of fused silica and the premixed liquid obtained in the step (1) were weighed, mechanically stirred and mixed for 4 hours to obtain alumina ceramic slurry.
(3) Adding a catalyst and an initiator: weighing 0.1g of ammonium persulfate, weighing 45 mu L of tetramethylethylenediamine, adding into the alumina ceramic slurry obtained in the step (2), and carrying out ball milling and mixing for 5 min. Vacuumizing and exhausting for 10 min.
(4) Gel casting: and (4) transferring the slurry obtained in the step (3) into a gear mold, heating to 45 ℃, curing for 1h, and cooling and demolding after complete curing. And (5) drying the demoulded blank body at room temperature for 30h to obtain a ceramic biscuit.
(5) Firing the ceramic: and (4) placing the ceramic biscuit obtained in the step (4) in a sintering furnace, heating to 1530 ℃, preserving heat for 5 hours, and cooling along with the furnace to obtain the alumina ceramic gear.
Example 3
The preparation method of the gear-shaped alumina ceramic comprises the following steps:
(1) preparing a premixed solution: 30mL of water was weighed, and 3g of methacrylamide, 0.1g of N, N' -methylenebisacrylamide and 1g of polyvinylpyrrolidone were weighed and placed in a beaker to be dissolved by stirring at room temperature, thereby obtaining a premixed solution.
(2) Preparation of alumina gel casting slurry: weighing 120g of alumina powder, 9g of fused quartz and the premixed liquid obtained in the step (1), adding into a ball mill, and ball-milling and mixing for 2h to obtain alumina ceramic slurry.
(3) Adding a catalyst and an initiator: weighing 0.02g of ammonium persulfate, weighing 12 mu L of tetramethylethylenediamine, adding into the alumina ceramic slurry obtained in the step (2), carrying out ball milling and mixing for 10min, and vacuumizing for 5 min.
(4) Gel casting: and (4) transferring the slurry obtained in the step (3) into a gear mold, curing at room temperature for 2h, and demolding after complete curing. And (5) placing the demoulded blank body at room temperature, and continuously drying for 24h to obtain a ceramic biscuit.
(5) Firing the ceramic: and (4) placing the ceramic biscuit obtained in the step (4) in a sintering furnace, heating to 1550 ℃, preserving heat for 4 hours, and cooling along with the furnace to obtain the alumina ceramic gear.
Example 4
(1) Preparing a premixed solution: 30mL of water was weighed, and 3g of methacrylamide, 0.1g of N, N' -methylenebisacrylamide and 1g of polyvinylpyrrolidone were weighed and placed in a beaker to be dissolved by stirring at room temperature, thereby obtaining a premixed solution.
(2) Preparation of alumina gel casting slurry: weighing 603g of alumina powder, 44g of fused silica and the premixed liquid obtained in the step (1) and adding the weighed materials into a ball mill to perform ball milling and mixing for 2 hours to obtain alumina ceramic slurry.
(3) Adding a catalyst and an initiator: weighing 0.02g of ammonium persulfate, weighing 12 mu L of tetramethylethylenediamine, adding into the alumina ceramic slurry obtained in the step (2), carrying out ball milling and mixing for 10min, and vacuumizing for 5 min.
(4) Gel casting: and (4) transferring the slurry obtained in the step (3) into a gear mold, curing at room temperature for 2h, and demolding after complete curing. And (5) placing the demoulded blank body at room temperature, and continuously drying for 24h to obtain a ceramic biscuit.
(5) Firing the ceramic: and (4) placing the ceramic biscuit obtained in the step (4) in a sintering furnace, heating to 1550 ℃, preserving heat for 4 hours, and cooling along with the furnace to obtain the alumina ceramic gear.
Comparative example 1
The preparation method of the gear-shaped alumina ceramic comprises the following steps:
(1) preparing a premixed solution: 30mL of water was weighed, and 3g of methacrylamide, 0.1g of N, N' -methylenebisacrylamide and 1g of polyvinylpyrrolidone were weighed and placed in a beaker to be dissolved by stirring at room temperature, thereby obtaining a premixed solution.
(2) Preparation of alumina gel casting slurry: weighing 24g of alumina powder, 4g of fused silica and the premixed liquid obtained in the step (1), adding into a ball mill, and ball-milling and mixing for 2h to obtain alumina ceramic slurry.
(3) Adding a catalyst and an initiator: weighing 0.02g of ammonium persulfate, weighing 12 mu L of tetramethylethylenediamine, adding into the alumina ceramic slurry obtained in the step (2), carrying out ball milling and mixing for 10min, and vacuumizing for 5 min.
(4) Gel casting: and (4) transferring the slurry obtained in the step (3) into a gear mold, curing at room temperature for 2h, and demolding after complete curing. And (5) placing the demoulded blank body at room temperature, and continuously drying for 24h to obtain a ceramic biscuit.
(5) Firing the ceramic: and (4) placing the ceramic biscuit obtained in the step (4) in a sintering furnace, heating to 1550 ℃, preserving heat for 4 hours, and cooling along with the furnace to obtain the alumina ceramic gear.
Comparative example 2
The preparation method of the gear-shaped alumina ceramic comprises the following steps:
(1) preparing a premixed solution: 30mL of water was weighed, and 3g of methacrylamide, 0.1g of N, N' -methylenebisacrylamide and 1g of polyvinylpyrrolidone were weighed and placed in a beaker to be dissolved by stirring at room temperature, thereby obtaining a premixed solution.
(2) Preparation of alumina gel casting slurry: weighing 120g of alumina powder and the premixed liquid obtained in the step (1), adding the weighed alumina powder and the premixed liquid into a ball mill, and ball-milling and mixing for 2 hours to obtain alumina ceramic slurry.
(3) Adding a catalyst and an initiator: weighing 0.02g of ammonium persulfate, weighing 12 mu L of tetramethylethylenediamine, adding into the alumina ceramic slurry obtained in the step (2), carrying out ball milling and mixing for 10min, and vacuumizing for 5 min.
(4) Gel casting: and (4) transferring the slurry obtained in the step (3) into a gear mold, curing at room temperature for 2h, and demolding after complete curing. And (5) placing the demoulded blank body at room temperature, and continuously drying for 24h to obtain a ceramic biscuit.
(5) Firing the ceramic: and (4) placing the ceramic biscuit obtained in the step (4) in a sintering furnace, heating to 1550 ℃, preserving heat for 4 hours, and cooling along with the furnace to obtain the alumina ceramic gear.
The alumina ceramic gears prepared in examples 1 to 4 and comparative examples 1 to 2 were tested for shrinkage, porosity and compressive strength, and the test results are shown in table 1.
TABLE 1 test results
| Shrinkage rate | Porosity of the alloy | Compressive strength/MPa | |
| Example 1 | 2.8％ | 26％ | 120 |
| Example 2 | 2.1％ | 22％ | 134 |
| Example 3 | 1.3％ | 19％ | 146 |
| Example 4 | 1.2％ | 17％ | 152 |
| Comparative example 1 | 5.9％ | 35％ | 62 |
| Comparative example 2 | 5.1％ | 31％ | 72 |
Claims (10)
1. A preparation method of alumina ceramics with complex shapes is characterized by comprising the following steps: after the alumina ceramic manufactured by the method is molded and sintered, the shrinkage rate of a product is less than 5 percent, and the method comprises the following steps:
(1) preparing a premixed solution: mixing water, a monomer, a cross-linking agent and a dispersing agent, and stirring for dissolving to obtain a premixed solution;
(2) preparation of alumina gel casting slurry: uniformly mixing alumina powder, silica powder and premixed liquid to obtain slurry, wherein the mass ratio of the alumina powder to the silica powder to the premixed liquid is 60:40-95: 5;
(3) adding a catalyst and an initiator: adding a catalyst and an initiator into the slurry, and uniformly mixing;
(4) gel casting: transferring the slurry obtained in the step (3) into a mold, solidifying, cooling, demolding and drying to obtain a ceramic biscuit;
(5) firing the ceramic: and sintering the ceramic biscuit.
2. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: after the alumina ceramic manufactured by the method is molded and sintered, the shrinkage rate of the product is less than 3 percent.
3. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: the silicon oxide powder is fused quartz, and the mass ratio of the fused quartz to the aluminum oxide powder is 5-40%.
4. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: the mass ratio of the alumina powder to the silicon oxide powder to the premixed liquid is 65:35-95: 5.
5. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: when the alumina gel casting slurry is prepared, the premixed liquid is added into the alumina powder and the silica powder to be ball-milled or mechanically stirred and uniformly mixed.
6. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: the monomer is methacrylamide and accounts for 5-20 wt% of the premixed liquid according to the mass ratio.
7. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: the cross-linking agent is N, N' -methylene bisacrylamide and accounts for 0.3-3 wt% of the premixed liquid according to the mass ratio.
8. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: the dispersing agent is one or more of polyvinylpyrrolidone, polyvinyl alcohol, ammonium polyacrylate or triammonium citrate, and accounts for 1.5-8 wt% of the premixed liquid according to the mass ratio.
9. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: the catalyst is tetramethylethylenediamine which accounts for 0.01 to 0.4 weight percent of the premixed solution according to the mass ratio.
10. The method for preparing an alumina ceramic having a complicated shape according to claim 1, wherein: the initiator is ammonium persulfate or potassium persulfate, and accounts for 0.02-1 wt% of the premixed liquid according to the mass ratio.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113372101A (en) * | 2021-06-29 | 2021-09-10 | 西安理工大学 | Preparation method of alumina ceramic |
| CN114538897A (en) * | 2020-11-25 | 2022-05-27 | 上海三思电子工程有限公司 | Sintering method of gel-casting ceramic green body |
| CN114538898A (en) * | 2020-11-25 | 2022-05-27 | 上海三思电子工程有限公司 | Preparation method of gel-casting ceramic green body |
| CN115073149A (en) * | 2022-07-27 | 2022-09-20 | 宜昌市禹猫智能科技有限公司 | Sponge ceramic tube and preparation method thereof |
| CN115368116A (en) * | 2022-09-16 | 2022-11-22 | 佛山市东鹏陶瓷有限公司 | Method for rapidly preparing aluminum oxide ceramic wafer and prepared aluminum oxide ceramic wafer |
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2020
- 2020-04-30 CN CN202010361831.7A patent/CN111533540A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538897A (en) * | 2020-11-25 | 2022-05-27 | 上海三思电子工程有限公司 | Sintering method of gel-casting ceramic green body |
| CN114538898A (en) * | 2020-11-25 | 2022-05-27 | 上海三思电子工程有限公司 | Preparation method of gel-casting ceramic green body |
| CN113372101A (en) * | 2021-06-29 | 2021-09-10 | 西安理工大学 | Preparation method of alumina ceramic |
| CN115073149A (en) * | 2022-07-27 | 2022-09-20 | 宜昌市禹猫智能科技有限公司 | Sponge ceramic tube and preparation method thereof |
| CN115368116A (en) * | 2022-09-16 | 2022-11-22 | 佛山市东鹏陶瓷有限公司 | Method for rapidly preparing aluminum oxide ceramic wafer and prepared aluminum oxide ceramic wafer |
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