CN111635246A - Porous silicon carbide ceramic and preparation method thereof - Google Patents
Porous silicon carbide ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of ceramic materials, and discloses a porous silicon carbide ceramic, wherein the raw materials of the porous silicon carbide ceramic comprise a main material, a dispersing agent, a binder and deionized water; the main material comprises, by weight, 80-90 parts of silicon carbide, 1-10 parts of sintering aid, 2-10 parts of pore-forming agent and 2-10 parts of additive; the sintering aid is calcium oxide and yttrium oxide; the pore-forming agent is a mixture of ammonium perchlorate and basic bismuth carbonate; the additive is calcite powder and/or pyroxene powder. The porous silicon carbide ceramic provided by the invention has low sintering temperature, low thermal expansion coefficient and high thermal shock resistance, so that the preparation of the porous silicon carbide ceramic with excellent performance is realized, and the purpose of saving energy consumption is achieved.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to porous silicon carbide ceramic and a preparation method thereof.
Background
The porous silicon carbide ceramic is a ceramic material which is sintered at high temperature and has a large number of interconnected ceramic bodies. The porous silicon carbide ceramic has the characteristics of high-temperature strength, corrosion resistance, oxidation resistance, high thermal conductivity, microwave absorption and the like, so that the porous silicon carbide ceramic is widely applied to the fields of aerospace, automobiles, machinery, electronics, chemical industry, energy, environmental protection and the like.
At present, the reported method for preparing the porous silicon carbide ceramic generally needs sintering under a high-temperature condition, the energy consumption of the preparation process is large, the cost is high, and the prepared porous silicon carbide ceramic has high thermal expansion coefficient and poor thermal shock resistance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides porous silicon carbide ceramic and a preparation method thereof.
In order to achieve the above object, a first aspect of the present invention provides a porous silicon carbide ceramic whose raw materials include a main material, a dispersant, a binder, and deionized water;
the main material comprises, by weight, 80-90 parts of silicon carbide, 1-10 parts of sintering aid, 2-10 parts of pore-forming agent and 2-10 parts of additive.
Preferably, the sintering aid is calcium oxide and yttrium oxide.
Preferably, the pore-forming agent is a mixture of ammonium perchlorate and bismuth subcarbonate.
Preferably, the additive is calcite powder and/or pyroxene powder.
Preferably, the dispersant is polyethylene glycol, and the dosage of the polyethylene glycol is 4-6% of the total weight of the main material.
Preferably, the binder is dextrin, and the dosage of the dextrin is 3-5% of the total weight of the main materials.
Preferably, the dosage of the deionized water is 45-55% of the total weight of the main materials.
Preferably, the mass ratio of the calcium oxide to the yttrium oxide is 2-5: 1.
preferably, the mass ratio of the ammonium perchlorate to the bismuth subcarbonate is 1: 4-10.
Preferably, the calcite powder and the pyroxene powder are obtained by ball milling and sieving with a 100-200 mesh sieve.
The second aspect of the present invention provides a method for preparing the porous silicon carbide ceramic, wherein the method comprises the following steps:
(1) ball-milling and mixing silicon carbide, sintering aid, additive, dispersant, binder and deionized water to obtain silicon carbide slurry;
(2) stirring and mixing the silicon carbide slurry and a pore-forming agent, spraying and granulating, and then carrying out dry pressing molding under 80-150MPa to obtain a silicon carbide biscuit;
(3) and sintering the silicon carbide biscuit in an argon atmosphere to obtain the porous silicon carbide ceramic.
Preferably, in the step (1), the ball milling time is 1-2 h.
Preferably, in the step (2), the conditions for spray granulation are as follows: the feeding speed is 2-3kg/h, the air inlet temperature is 200-250 ℃, and the air outlet temperature is 100-110 ℃.
Preferably, in the step (3), the sintering conditions are: introducing argon into the furnace at the speed of 30-40ml/min in a tubular furnace, raising the temperature to 600-minus charge 800 ℃ at the speed of 2-5 ℃/min under the protection of the argon, preserving the heat for 0.5-1h, raising the temperature to 1050-minus charge 1100 ℃ at the speed of 5-7 ℃/min, preserving the heat for 1-3h, and naturally cooling to the room temperature to obtain the porous silicon carbide ceramic.
According to the invention, the ammonium perchlorate and the bismuth subcarbonate are used in a matched manner as a pore forming agent, the calcium oxide and the yttrium oxide are used as sintering aids, at least one of the mollite powder and the pyroxene powder is used as an additive, the preparation of the porous silicon carbide ceramic at a lower temperature (1050 plus 1100 ℃) is realized, the energy is saved, the cost is reduced, and the prepared porous silicon carbide ceramic not only has a lower thermal expansion coefficient, but also has a better thermal shock resistance.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a porous silicon carbide ceramic, which comprises the following raw materials of a main material, a dispersing agent, a binder and deionized water.
The main material comprises, by weight, 80-90 parts of silicon carbide, 1-10 parts of sintering aid, 2-10 parts of pore-forming agent and 2-10 parts of additive.
In a preferred case, the sintering aid is calcium oxide and yttrium oxide.
In a preferred case, the pore former is a mixture of ammonium perchlorate and bismuth subcarbonate.
In the temperature rise process of the invention, the bismuth subcarbonate is firstly decomposed to generate bismuth oxide and carbon dioxide. The generated carbon dioxide is used for carrying out pore-forming on the silicon carbide ceramic; the generated bismuth oxide can cooperate with calcium oxide and yttrium oxide to promote the generation of liquid phase, reduce the sintering temperature, prevent the cracking of a blank in the high-temperature sintering process and improve the thermal shock resistance of the porous silicon carbide ceramic. In addition, the generated bismuth oxide can also catalyze the decomposition of ammonium perchlorate, reduce the decomposition temperature of the ammonium perchlorate, promote the release of more heat, further reduce the sintering temperature, improve the efficiency of the preparation process of the silicon carbide ceramic and save energy.
In a preferred case, the additive is calcite powder and/or pyroxene powder. In the invention, the thermal expansion coefficients of the calcite powder and the pyroxene powder are lower than that of silicon carbide, and at least one of the calcite powder and the pyroxene powder is used as an additive in the preparation process of the porous silicon carbide ceramic, so that the prepared porous silicon carbide ceramic has a lower thermal expansion coefficient.
In a preferred case, the dispersant is polyethylene glycol, and the dosage of the polyethylene glycol is 4-6% of the total weight of the main material. In the invention, the polyethylene glycol is used as a dispersing agent to improve the dispersibility of each sintering component, thereby improving the compactness and stability of the ceramic structure.
In a preferred case, the binder is dextrin, and the dosage of the dextrin is 3-5% of the total weight of the main material. In the invention, the dextrin can promote the forming of the blank and increase the strength of the blank.
In a preferable case, the amount of the deionized water is 45-55% of the total weight of the main materials.
Preferably, the mass ratio of the calcium oxide to the yttrium oxide is 2-5: 1.
in a preferred case, the mass ratio of the ammonium perchlorate to the bismuth subcarbonate is 1: 4-10.
Preferably, the calcite powder and the pyroxene powder are ball milled and then sieved through a 100-200 mesh sieve.
The second aspect of the present invention provides a method for preparing the porous silicon carbide ceramic, wherein the method comprises the following steps:
(1) ball-milling and mixing silicon carbide, sintering aid, additive, dispersant, binder and deionized water to obtain silicon carbide slurry;
(2) stirring and mixing the silicon carbide slurry and a pore-forming agent, spraying and granulating, and then carrying out dry pressing molding under 80-150MPa to obtain a silicon carbide biscuit;
(3) and sintering the silicon carbide biscuit in an argon atmosphere to obtain the porous silicon carbide ceramic.
Preferably, in step (1), the ball milling time is 1 to 2 hours.
Preferably, in step (2), the spray granulation conditions are: the feeding speed is 2-3kg/h, the air inlet temperature is 200-250 ℃, and the air outlet temperature is 100-110 ℃.
Preferably, in step (3), the sintering conditions are: introducing argon into the furnace at the speed of 30-40ml/min in a tubular furnace, raising the temperature to 600-minus charge 800 ℃ at the speed of 2-5 ℃/min under the protection of the argon, preserving the heat for 0.5-1h, raising the temperature to 1050-minus charge 1100 ℃ at the speed of 5-7 ℃/min, preserving the heat for 1-3h, and naturally cooling to the room temperature to obtain the porous silicon carbide ceramic.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, calcium oxide and yttrium oxide are used as sintering aids and are matched with bismuth oxide generated by decomposing basic bismuth carbonate, so that the generation of a liquid phase can be well promoted, the temperature required by sintering is reduced, a blank body is prevented from cracking in the high-temperature sintering process, and the thermal shock resistance of the porous silicon carbide ceramic is improved.
(2) According to the invention, the mixture of ammonium perchlorate and bismuth subcarbonate is used as the pore-forming agent, besides pore-forming of silicon carbide ceramic, bismuth oxide generated by decomposition of bismuth subcarbonate can promote decomposition of ammonium perchlorate, reaction time is shortened, and a large amount of heat is released, so that external energy consumption is saved, and sintering temperature is further reduced.
(3) According to the invention, the mollisine powder and/or the pyroxene powder are/is used as the additive, so that the prepared porous silicon carbide ceramic has a lower thermal expansion coefficient.
The present invention will be described in detail below by way of examples, but the scope of the present invention is not limited thereto.
Example 1
(1) And (2) performing ball milling and mixing on 86 parts by weight of silicon carbide, 3 parts by weight of calcium oxide, 1 part by weight of yttrium oxide, 5 parts by weight of 150-mesh calcite powder and a mixed solution consisting of 6 parts by weight of polyethylene glycol, 5 parts by weight of dextrin and 45 parts by weight of deionized water for 1 hour to obtain silicon carbide slurry.
(2) And stirring and mixing the obtained silicon carbide slurry with 1 weight part of ammonium perchlorate and 4 weight parts of basic bismuth carbonate, then carrying out spray granulation in a spray granulator, wherein the feeding rate is 3kg/h, the air inlet temperature is 240 ℃, the air outlet temperature is 100 ℃, and then carrying out dry pressing under 140MPa to obtain a silicon carbide biscuit.
(3) And transferring the silicon carbide biscuit into a tubular furnace, introducing argon into the furnace at the speed of 30ml/min, heating to 800 ℃ at the speed of 5 ℃/min under the protection of the argon, preserving the temperature for 1h, heating to 1070 ℃ at the speed of 7 ℃/min, preserving the temperature for 2h, and naturally cooling to room temperature to obtain the porous silicon carbide ceramic S1.
Example 2
(1) And (2) carrying out ball milling and mixing on 84 parts by weight of silicon carbide, 4.8 parts by weight of calcium oxide, 1.2 parts by weight of yttrium oxide, 3 parts by weight of 200-mesh diabase powder and a mixed solution consisting of 5 parts by weight of polyethylene glycol, 4 parts by weight of dextrin and 50 parts by weight of deionized water, wherein the ball milling time is 1.5h, so as to obtain silicon carbide slurry.
(2) And stirring and mixing the obtained silicon carbide slurry with 1 weight part of ammonium perchlorate and 6 weight parts of basic bismuth carbonate, then carrying out spray granulation in a spray granulator, wherein the feeding rate is 2.5kg/h, the air inlet temperature is 220 ℃, the air outlet temperature is 105 ℃, and then carrying out dry pressing under 130MPa to obtain a silicon carbide biscuit.
(3) And transferring the silicon carbide biscuit into a tubular furnace, introducing argon into the furnace at the speed of 35ml/min, heating to 700 ℃ at the speed of 4 ℃/min under the protection of the argon, preserving the heat for 0.6h, heating to 1100 ℃ at the speed of 6 ℃/min, preserving the heat for 2.5h, and naturally cooling to room temperature to obtain the porous silicon carbide ceramic S2.
Example 3
(1) And carrying out ball milling and mixing on a mixed solution consisting of 82 parts by weight of silicon carbide, 2 parts by weight of calcium oxide, 1 part by weight of yttrium oxide, 4 parts by weight of 100-mesh calcite powder, 3 parts by weight of 100-mesh diabase powder, 4 parts by weight of polyethylene glycol, 3 parts by weight of dextrin and 55 parts by weight of deionized water for 2 hours to obtain silicon carbide slurry.
(2) And stirring and mixing the obtained silicon carbide slurry with 1 weight part of ammonium perchlorate and 7 weight parts of basic bismuth carbonate, then carrying out spray granulation in a spray granulator, wherein the feeding rate is 2kg/h, the air inlet temperature is 200 ℃, the air outlet temperature is 110 ℃, and then carrying out dry pressing under 100MPa to obtain a silicon carbide biscuit.
(3) And transferring the silicon carbide biscuit into a tubular furnace, introducing argon into the furnace at the speed of 40ml/min, heating to 600 ℃ at the speed of 3 ℃/min under the protection of the argon, preserving the heat for 0.5h, heating to 1050 ℃ at the speed of 5 ℃/min, preserving the heat for 3h, and naturally cooling to room temperature to obtain the porous silicon carbide ceramic S3.
Comparative example 1
The procedure of example 1 was repeated except that calcium oxide and yttrium oxide were not added, to obtain a porous silicon carbide ceramic D1.
Comparative example 2
The procedure of example 1 was repeated except that the basic bismuth carbonate was not added, to obtain a porous silicon carbide ceramic D2.
Comparative example 3
The procedure of example 1 was repeated except that ammonium perchlorate was not added, to obtain a porous silicon carbide ceramic D3.
Comparative example 4
The procedure of example 1 was repeated except that ammonium perchlorate was replaced with ammonium hydrogencarbonate to obtain a porous silicon carbide ceramic D4.
Comparative example 5
The procedure of example 1 was repeated except that the calcite powder was changed to forsterite powder to obtain a porous silicon carbide ceramic D5.
Test example
The porous silicon carbide ceramics obtained in examples 1 to 3 and comparative examples 1 to 5 were tested for their properties, and the results are shown in Table 1.
TABLE 1
From the results in table 1, it is understood that both calcite powder and pyroxene powder can reduce the thermal expansion coefficient of the ceramic; the bismuth oxide obtained by decomposing the basic bismuth carbonate is matched with the calcium oxide and the yttrium oxide for use, so that the liquid phase generation can be promoted, the sintering temperature can be reduced, and the thermal shock resistance of the porous silicon carbide ceramic can be improved; in addition, the bismuth oxide can promote the decomposition of the ammonium perchlorate, improve the thermal decomposition efficiency and further reduce the sintering temperature; when bismuth subcarbonate or ammonium perchlorate is not added or other pore formers are replaced in the preparation process of the ceramic, the sintering temperature cannot be well reduced (sintering is carried out at a higher temperature, actually at 1070 ℃), so that the green body is insufficiently sintered, and the thermal shock resistance of the ceramic is further reduced. By adopting the method, the porous silicon carbide ceramic can be sintered at 1050-1100 ℃, and the prepared porous silicon carbide ceramic has lower thermal expansion coefficient and higher thermal shock resistance.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (9)
1. The porous silicon carbide ceramic is characterized in that raw materials of the porous silicon carbide ceramic comprise a main material, a dispersing agent, a binder and deionized water;
the main material comprises, by weight, 80-90 parts of silicon carbide, 1-10 parts of sintering aid, 2-10 parts of pore-forming agent and 2-10 parts of additive;
the sintering aid is calcium oxide and yttrium oxide; the pore-forming agent is a mixture of ammonium perchlorate and basic bismuth carbonate; the additive is calcite powder and/or pyroxene powder.
2. The porous silicon carbide ceramic according to claim 1, wherein the dispersant is polyethylene glycol in an amount of 4-6% by weight of the total weight of the main material; the binder is dextrin, and the dosage of the dextrin is 3-5% of the total weight of the main materials; the dosage of the deionized water is 45-55% of the total weight of the main materials.
3. The porous silicon carbide ceramic according to claim 1, wherein the mass ratio of the calcium oxide to the yttrium oxide is 2-5: 1.
4. the porous silicon carbide ceramic of claim 1, wherein the mass ratio of ammonium perchlorate to bismuth subcarbonate is 1: 4-10.
5. The porous silicon carbide ceramic of claim 1, wherein the calcite powder and the pyroxene powder are ball milled and then sieved through a 100-200 mesh sieve.
6. The method of preparing a porous silicon carbide ceramic according to any one of claims 1 to 5, comprising the steps of:
(1) ball-milling and mixing silicon carbide, sintering aid, additive, dispersant, binder and deionized water to obtain silicon carbide slurry;
(2) stirring and mixing the silicon carbide slurry and a pore-forming agent, spraying and granulating, and then carrying out dry pressing molding under 80-150MPa to obtain a silicon carbide biscuit;
(3) and sintering the silicon carbide biscuit in an argon atmosphere to obtain the porous silicon carbide ceramic.
7. The preparation method according to claim 6, wherein in the step (1), the ball milling time is 1-2 h.
8. The production method according to claim 6, wherein in the step (2), the conditions for the spray granulation are: the feeding speed is 2-3kg/h, the air inlet temperature is 200-250 ℃, and the air outlet temperature is 100-110 ℃.
9. The production method according to claim 6, wherein in the step (3), the sintering conditions are: introducing argon into the furnace at the speed of 30-40ml/min in a tubular furnace, raising the temperature to 600-minus charge 800 ℃ at the speed of 2-5 ℃/min under the protection of the argon, preserving the heat for 0.5-1h, raising the temperature to 1050-minus charge 1100 ℃ at the speed of 5-7 ℃/min, preserving the heat for 1-3h, and naturally cooling to the room temperature to obtain the porous silicon carbide ceramic.
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Cited By (2)
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|---|---|---|---|---|
| CN115959923A (en) * | 2023-01-03 | 2023-04-14 | 深圳市卓尔悦电子科技有限公司 | Porous ceramic, atomizing core, atomizing device and preparation method of porous ceramic |
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