CN105294160A - Method for preparing porous silicon nitride ceramics through gel casting and microwave sintering - Google Patents
Method for preparing porous silicon nitride ceramics through gel casting and microwave sintering Download PDFInfo
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- CN105294160A CN105294160A CN201510628862.3A CN201510628862A CN105294160A CN 105294160 A CN105294160 A CN 105294160A CN 201510628862 A CN201510628862 A CN 201510628862A CN 105294160 A CN105294160 A CN 105294160A
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Abstract
The invention provides a method for preparing porous silicon nitride ceramics through gel casting and microwave sintering. The method comprises the following main steps of (1) preparing a sizing agent: uniformly mixing premixing liquid, silicon nitride powder, sintering additive powder and the like to prepare the sizing agent; (2) preparing a green body: injection molding the sizing agent and drying to prepare the green body; (3) degreasing: removing additives at a certain temperature; (4) microwave sintering: sintering a shaped compact in a sintering furnace to obtain the porous ceramics. According to the preparation method provided by the invention, the gel casting process is utilized to prepare a porous silicon nitride product with large size and complex shape. The microwave sintering method is adopted to achieve the aims of quick temperature rise and temperature uniformity, and the porous silicon nitride ceramics with a closed pore structure is formed and has good mechanical property.
Description
Technical field
The present invention relates to porous silicon nitride ceramic technical field, be specifically related to a kind of gel injection, method that microwave sintering prepares porous silicon nitride ceramic.
Background technology
Silicon nitride material has good calorifics, electricity and mechanical property.Porous silicon nitride ceramic has the features such as high temperature resistant, corrosion-resistant, intensity is high, thermal shock resistance is good, is widely used in the fields such as petrochemical complex, metallurgical machinery, aerospace.
Gel-casting process is a kind of novel forming method.It utilizes non-punch die, add a small amount of additive in slurry inside thus make ceramic size generation chemical reaction solidify in place become base substrate, have that setting time is adjustable, intensity is high, solid load is high, technique is simple, the advantage of near-net-shape, complicated shape, large-size ceramic goods can be prepared.
Microwave sintering makes material monolithic heat by the coupled characteristic of microwave, reaches the object be rapidly heated with equalizing temperature.Compared with traditional pressureless sintering, gas pressure sintering mode, microwave sintering has the advantages such as sintering quality is good, yield rate is high, sintering temperature is low, sintering time is short, sintering energy consumption is low.Ceramic body after gel injection is by microwave sintering, and the porous silicon nitride ceramic of preparation has good high temperature resistant, corrosion-resistant and feature that intensity is high.
Summary of the invention
A kind of method that the present invention aims to provide gel injection, microwave sintering prepares porous silicon nitride ceramic, can prepare high temperature resistant, corrosion-resistant and intensity much higher hole silicon nitride ceramics.
In order to realize foregoing invention object, the technical scheme of the embodiment of the present invention is as follows:
Gel injection, microwave sintering prepare a method for porous silicon nitride ceramic, comprise the steps:
(1) slurry preparation: monomer, softening agent, linking agent and deionized water are mixed and made into premixed liquid, then add alpha-silicon nitride powders, sintering aid powder etc., adjust ph is 8-12, makes slurry after ball milling 4-15h;
(2) base: add pore-forming material, adds initiator after vacuum stripping and catalyst mix is even, and casting after vacuum stripping makes slurry solidify the demoulding after reaction for some time, obtains base substrate;
(3) degreasing: drying adds thermal debinding in about 10 days in sintering oven, after being heated to 200 DEG C, is warming up to 550 DEG C with the temperature rise rate of 0.2-0.5 DEG C/min with the temperature rise rate of 1 DEG C/min, and at 550 DEG C of insulation 2h;
(4) microwave sintering: base substrate after degreasing is placed in sintering oven, sinters under certain sintering temperature and soaking time, obtains porous ceramics.
As preferably, described monomer is acrylamide, and softening agent is polyacrylamide, and linking agent is N, N '-methylene-bisacrylamide;
As preferably, described sintering aid powder is yttrium oxide and alumina powder, and the ratio taken is (3-6): 2;
As preferably, the alumina hollow ball of described pore-forming material to be particle diameter be 50-100um;
As preferably, described initiator is ammonium persulphate, and catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine;
As preferably, the weight ratio of described softening agent, monomer, linking agent, deionized water, alpha-silicon nitride powders, sintering aid, pore-forming material, initiator, catalyzer is (1-5): (10-25): (2-3): 100:(80-100): (3-10): (0.1-30): (0.08-0.1): (0.4-0.6);
As preferably, the sintering temperature of described microwave sintering is 1400 ~ 1700 DEG C, and soaking time is 1 ~ 3 hour, microwave frequency 2GHz, and nitrogen atmosphere is protected.
The present invention prepares porous silicon nitride ceramic by gel injection molding and forming technology, and technique is simple, and the time is short, and efficiency is high, and cost is low, can realize the forming requirements of the shaping and complicated shape goods of large size.By microwave sintering process, sintering time is short, energy consumption is low, the silicon nitride ceramic material intensity of preparation is high, corrosion resistance nature and resistance to elevated temperatures good.
Embodiment
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these embodiments are only for illustration of the present invention, its scope do not limited the present invention in any way.
Embodiment 1: a kind of gel injection, microwave sintering prepare the method for porous silicon nitride ceramic, comprise the steps:
(1) slurry preparation: by 18 parts of acrylamides, 1.5 parts of polyacrylamides, 2.5 parts of N, N '-methylene-bisacrylamide and 100 parts of deionized waters are mixed and made into premixed liquid, add the combined sintering auxiliary agent powder (ratio is 3:2) of 92 parts of alpha-silicon nitride powders, 8 parts of yttrium oxide and aluminum oxide again, adjust ph is 9, makes slurry after ball milling 8h;
(2) base: add the alumina hollow ball pore-forming material that 18 parts of particle diameters are 60um, 0.08 part of ammonium persulfate initiator and 0.4 part of N is added after vacuum stripping, N, N, N-Tetramethyl Ethylene Diamine catalyst mix is even, casting after vacuum stripping, reacts and makes slurry solidify the demoulding after 60 minutes, obtain base substrate;
(3) degreasing: drying adds thermal debinding in about 10 days in sintering oven, after being heated to 200 DEG C, is warming up to 550 DEG C with the temperature rise rate of 0.2-0.5 DEG C/min with the temperature rise rate of 1 DEG C/min, and at 550 DEG C of insulation 2h;
(4) microwave sintering: one-tenth parison is placed in sintering oven, microwave frequency 2GHz, nitrogen atmosphere is protected; temperature rise rate is 5 DEG C/min, and sintering temperature is 1600 DEG C, insulation 1.5h; after stopping heating, furnace cooling is to room temperature, and obtain porous ceramics, porosity is 53%.
Embodiment 2: a kind of gel injection, microwave sintering prepare the method for porous silicon nitride ceramic, comprise the steps:
(1) slurry preparation: by 22 parts of acrylamides, 2 parts of polyacrylamides, 2 parts of N, N '-methylene-bisacrylamide and 100 parts of deionized waters are mixed and made into premixed liquid, add the combined sintering auxiliary agent powder (ratio is 5:2) of 96 parts of alpha-silicon nitride powders, 4 parts of yttrium oxide and aluminum oxide again, adjust ph is 9, makes slurry after ball milling 8h;
(2) base: add the alumina hollow ball pore-forming material that 20 parts of particle diameters are 80um, 0.08 part of ammonium persulfate initiator and 0.5 part of N is added after vacuum stripping, N, N, N-Tetramethyl Ethylene Diamine catalyst mix is even, casting after vacuum stripping, reacts and makes slurry solidify the demoulding after 60 minutes, obtain base substrate;
(3) degreasing: drying adds thermal debinding in about 10 days in sintering oven, after being heated to 200 DEG C, is warming up to 550 DEG C with the temperature rise rate of 0.2-0.5 DEG C/min with the temperature rise rate of 1 DEG C/min, and at 550 DEG C of insulation 2h;
(4) microwave sintering: one-tenth parison is placed in sintering oven, microwave frequency 2GHz, nitrogen atmosphere is protected; temperature rise rate is 5 DEG C/min, and sintering temperature is 1630 DEG C, insulation 1.5h; after stopping heating, furnace cooling is to room temperature, and obtain porous ceramics, porosity is 45.6%.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (7)
1. gel injection, microwave sintering prepare a method for porous silicon nitride ceramic, it is characterized in that, comprise the steps:
(1) slurry preparation: monomer, softening agent, linking agent and deionized water are mixed and made into premixed liquid, then add alpha-silicon nitride powders, sintering aid powder, adjust ph is 8-12, makes slurry after ball milling;
(2) base: add pore-forming material, adds initiator after vacuum stripping and catalyst mix is even, and casting after vacuum stripping, makes slurry solidify the demoulding, obtain base substrate after reaction;
(3) degreasing: drying adds thermal debinding in about 10 days in sintering oven, after being heated to 200 DEG C, is warming up to 550 DEG C with the temperature rise rate of 0.2-0.5 DEG C/min with the temperature rise rate of 1 DEG C/min, and at 550 DEG C of insulation 2h;
(4) microwave sintering: base substrate after degreasing is placed in sintering oven and sinters, obtains porous ceramics.
2. a kind of gel injection according to claim 1, microwave sintering prepare the method for porous silicon nitride ceramic, and it is characterized in that, described monomer is acrylamide, and softening agent is polyacrylamide, and described linking agent is N, N '-methylene-bisacrylamide.
3. a kind of gel injection according to claim 1, microwave sintering prepare the method for porous silicon nitride ceramic, and it is characterized in that, sintering aid powder is yttrium oxide and alumina powder, and the ratio taken is (3-6): 2.
4. a kind of gel injection according to claim 1, microwave sintering prepare the method for porous silicon nitride ceramic, it is characterized in that, the alumina hollow ball of described pore-forming material to be particle diameter be 50-100um.
5. a kind of gel injection according to claim 1, microwave sintering prepare the method for porous silicon nitride ceramic, and it is characterized in that, described initiator is ammonium persulphate, and catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
6. a kind of gel injection according to claim 1, microwave sintering prepare the method for porous silicon nitride ceramic, it is characterized in that, the weight ratio of described softening agent, monomer, linking agent, deionized water, alpha-silicon nitride powders, sintering aid, pore-forming material, initiator, catalyzer is (1-5): (10-25): (2-3): 100:(80-100): (3-10): (0.1-30): (0.08-0.1): (0.4-0.6).
7. a kind of gel injection according to claim 1, microwave sintering prepare the method for porous silicon nitride ceramic; it is characterized in that, the sintering temperature of described microwave sintering is 1400 ~ 1700 DEG C, and soaking time is 1 ~ 3 hour; microwave frequency 2GHz, nitrogen atmosphere is protected.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108840685A (en) * | 2018-07-23 | 2018-11-20 | 董孟富 | A kind of superficial three-dimensional throws brick and its manufacturing method from water-fast antibacterial porcelain |
| CN110330344A (en) * | 2019-06-19 | 2019-10-15 | 华中科技大学 | A method of high porosity silicon nitride ceramics is prepared based on selective laser sintering |
| CN111393181A (en) * | 2020-03-20 | 2020-07-10 | 安徽金岩高岭土科技有限公司 | Preparation method of full-closed-pore porous mullite ceramic based on direct solidification injection molding |
| CN112661519A (en) * | 2021-01-28 | 2021-04-16 | 威海圆环先进陶瓷股份有限公司 | Production technology of silicon nitride ceramic pile |
| CN115385699A (en) * | 2022-08-31 | 2022-11-25 | 山东工业陶瓷研究设计院有限公司 | High-temperature wave-transparent and active cooling integrated material and preparation method thereof |
| CN115947605A (en) * | 2022-12-27 | 2023-04-11 | 衡阳凯新特种材料科技有限公司 | Silicon nitride porous ceramic material and preparation method thereof |
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| CN103496999A (en) * | 2013-09-18 | 2014-01-08 | 清华大学 | Method for preparing porous ceramics from hollow ceramic ball |
| CN103922748A (en) * | 2014-03-14 | 2014-07-16 | 河海大学 | Preparation method for porous silicon nitride ceramic |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108840685A (en) * | 2018-07-23 | 2018-11-20 | 董孟富 | A kind of superficial three-dimensional throws brick and its manufacturing method from water-fast antibacterial porcelain |
| CN108840685B (en) * | 2018-07-23 | 2020-07-17 | 山东振东环保科技有限公司 | Superficial three-dimensional self-water-resistant antibacterial polished porcelain tile and manufacturing method thereof |
| CN110330344A (en) * | 2019-06-19 | 2019-10-15 | 华中科技大学 | A method of high porosity silicon nitride ceramics is prepared based on selective laser sintering |
| CN110330344B (en) * | 2019-06-19 | 2020-12-18 | 华中科技大学 | Method for preparing high-porosity silicon nitride ceramic based on selective laser sintering |
| CN111393181A (en) * | 2020-03-20 | 2020-07-10 | 安徽金岩高岭土科技有限公司 | Preparation method of full-closed-pore porous mullite ceramic based on direct solidification injection molding |
| CN111393181B (en) * | 2020-03-20 | 2022-07-19 | 安徽金岩高岭土科技有限公司 | Preparation method of full-closed-pore porous mullite ceramic based on direct solidification injection molding |
| CN112661519A (en) * | 2021-01-28 | 2021-04-16 | 威海圆环先进陶瓷股份有限公司 | Production technology of silicon nitride ceramic pile |
| CN115385699A (en) * | 2022-08-31 | 2022-11-25 | 山东工业陶瓷研究设计院有限公司 | High-temperature wave-transparent and active cooling integrated material and preparation method thereof |
| CN115385699B (en) * | 2022-08-31 | 2023-11-24 | 山东工业陶瓷研究设计院有限公司 | High-temperature wave-transparent and active cooling integrated material and preparation method thereof |
| CN115947605A (en) * | 2022-12-27 | 2023-04-11 | 衡阳凯新特种材料科技有限公司 | Silicon nitride porous ceramic material and preparation method thereof |
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