CN102173829A - Preparation method of zirconium boride-silicon carbide/graphite layered superhigh temperature ceramic - Google Patents
Preparation method of zirconium boride-silicon carbide/graphite layered superhigh temperature ceramic Download PDFInfo
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Abstract
The invention provides a preparation method of zirconium boride-silicon carbide/graphite layered superhigh temperature ceramic. The preparation method is characterized by comprising the following steps: 1) separately preparing a zirconium boride casting sheet and a zirconium oxide casting sheet by using a casting method, namely, adding a binder and a plasticizer in a solvent and evenly mixing, separately adding a zirconium boride ceramic powder material and a graphite ceramic powder material, and evenly mixing to form a casting material, then carrying out casting forming, and drying at room temperature and demoulding to respectively obtain the zirconium boride casting sheet with the thickness of 200-1000 mu m and the graphite casting sheet with the thickness of 20-100 mu m; 2) respectively slicing the zirconium boride casting sheet and the graphite casting sheet according to the size of a mould; 3) putting the zirconium boride sheet and the graphite sheet in a graphite mould in an alternatively overlapping way for vacuum derosination; and 4) hot pressed sintering in an argon atmosphere to prepare the layered superhigh temperature ceramic. According to the invention, preparation process is simple, cost is low, the machinability of the material is strong, compositions are controllable, and the toughness of the material is up to 11.3MPa.m<1/2>.
Description
Technical field
The invention provides the preparation method of a kind of zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery, belong to the preparing technical field of porous ceramics.
Background technology
Zirconium boride ceramic has superior high temperature resistant and corrosion resistance nature and relatively low theoretical density, therefore is considered in ultrahigh-temperature pottery (UHTCs) family one of material of application prospect is arranged most always.At present, zirconium boride ceramic has been widely used as various thermal structures and functional materials, as: the turbine blade in the aircraft industry, magnetohydrodynamic generator electrode etc.But the zirconium boride ceramic fracture toughness property is lower, and tough value only is 4～5MPam
1/2, limited its application under harsh operating environment, as supersonic aircraft nose cone and forward position, scramjet engine hot-end component etc.Therefore, in order to guarantee reliability and the security in the use, must improve the fragility problem of zirconium boride ceramic, thereby improve its thermal shock resistance.Existing at present report about preparation ultrahigh-temperature zirconium boride ceramic, as: the patent No. is that " zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material and preparation method thereof " intensity of CN101602597A is 132.03～695.54MPa, and fracture toughness property is 2.01～6.57MPam
1/2The patent No. is that CN101250061B's " preparation method of Zirconia toughened boride ultra-temperature ceramic-based composite material " fracture toughness property reaches 6.0～6.8MPam
1/2, but fracture toughness property still remains further to be improved.
Summary of the invention
The objective of the invention is in order to solve the problem of existing zirconium boride 99.5004323A8ure ultrahigh-temperature ceramics toughness difference, and the preparation method of a kind of zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery is provided.Its technical scheme is:
The preparation method of a kind of zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery is characterized in that adopting following steps:
1) adopt casting method to prepare zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet respectively: will to stir in binding agent and the softening agent adding solvent earlier, add zirconium boride ceramic powder and graphite ceramic powder more respectively, stir, form the curtain coating material, flow casting molding obtains thick zirconium boride 99.5004323A8ure cast sheet of 200～1000 μ m and the thick graphite cast sheet of 20～100 μ m respectively after the drying at room temperature demoulding then;
2) zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet are cut into slices respectively according to the mould size;
3) with zirconium boride 99.5004323A8ure sheet and graphite flake alternately stack put into graphite grinding tool, vacuum degreasing, during degreasing, heat-up rate is 2～3 ℃/min, is warming up to 600～700 ℃, insulation 0.5～1h;
4) hot pressed sintering under argon gas atmosphere, sintering temperature is 1900～2000 ℃, insulation 0.5～2h, pressure is 20～40MPa, promptly gets stratiform ultrahigh-temperature pottery.
The preparation method of described zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery, in the step 1), the zirconium boride ceramic powder is by zirconium boride 99.5004323A8ure powder and silicon carbide powder per-cent 70～90% by volume: 10～30% mix, the particle diameter of zirconium boride 99.5004323A8ure powder is 1～5 μ m, and the particle diameter of silicon carbide powder is 0.5～2 μ m.
The preparation method of described zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery in the step 1), is a basic calculation with zirconium boride ceramic powder weight, takes by weighing binding agent 5～15%, softening agent 5～15% and solvent 100～200% by weight percentage.
The preparation method of described zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery, in the step 1), the graphite ceramic powder is by powdered graphite and zirconium boride 99.5004323A8ure powder per-cent 80～100% by volume: 0～20% mixes.
The preparation method of described zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery is a basic calculation with graphite ceramic powder weight, takes by weighing binding agent 10～20%, softening agent 10～20% and solvent 500～1000% by weight percentage.
The preparation method of described zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery, binding agent adopts polyvinyl butyral acetal; The mixing of one or both in softening agent employing polyoxyethylene glycol and the polyvinyl alcohol; Solvent adopts ethanol.
The present invention compared with prior art has following advantage:
1, in the stratiform ultrahigh-temperature pottery that the present invention makes, the zirconium boride-carborundum layer is a hard formation, graphite linings is a soft formation, like this when the ultrahigh-temperature pottery when being subjected to external force, crack propagation to soft formation, just turn to parallel synusia direction expansion, and by soft formation continuation transmitted load, when treating that load increases, crackle just turns to vertical synusia direction expansion again and passes down one deck, like this, crackle just deflects after passing hard formation, has increased the extensions path of crackle, thereby improved the fracture toughness property of material, fracture toughness property is up to 11.3MPam
1/2
2, can control the thickness of zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet by the amount of control solvent, by the bed thickness ratio of adjusting hard formation and soft formation, but the mechanical property of regulating course shape ultrahigh-temperature pottery;
3, zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet is quality controllable, can reach the accurate control to stratiform ultrahigh-temperature pottery moiety by regulating the mass ratio of zirconium boride 99.5004323A8ure, silicon carbide and graphite;
4, the stratiform ultrahigh-temperature ceramic layer of present method acquisition is thin, and the zirconium boride 99.5004323A8ure bed thickness can reach 50 μ m, and graphite linings can reach 10 μ m;
5,, help the line cutting processing, make that the stratiform ultrahigh-temperature pottery workability of preparing is strong because but graphite has electroconductibility;
6, powdered graphite has preferred orientation in hot pressing, and lamella helps crack deflection perpendicular to the hot pressing direction in pressurized process.
7, adopt hot-pressing sintering technique, the stratiform ultrahigh-temperature ceramic dense height of preparation.
Description of drawings
Fig. 1 is the SEM photo of the embodiment of the invention 2 gained stratiform ultrahigh-temperature potteries;
Fig. 2 is the SEM photo after the test of the embodiment of the invention 2 gained stratiform ultrahigh-temperature ceramic fracture toughnesses.
Embodiment
Embodiment 1
1, preparation zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet: the preparation of (1) zirconium boride 99.5004323A8ure curtain coating material, elder generation's weighing 2.61 gram polyvinyl butyral acetals, 2.61 gram polyoxyethylene glycol, 52.23 gram ethanol, stir, add the zirconium boride 99.5004323A8ure powder of 42.63 grams, 1 μ m and the silicon carbide powder of 9.60 grams, 0.5 μ m again, stir, form zirconium boride 99.5004323A8ure curtain coating material, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 70%: 30% volume percent; (2) preparation of graphite curtain coating material, elder generation's weighing 3.06 gram polyvinyl butyral acetals, 3.06 gram polyoxyethylene glycol, 152.9 ethanol, stir, add 18.40 gram powdered graphites and 12.18 gram zirconium boride 99.5004323A8ure powder again, stir, form graphite curtain coating material, wherein powdered graphite and zirconium boride 99.5004323A8ure powder are to take by weighing according to 80%: 20% volume percent; (3) flow casting molding prolongs zirconium boride 99.5004323A8ure curtain coating material and the materials flow of graphite curtain coating respectively, obtains thick zirconium boride 99.5004323A8ure cast sheet of 1000 μ m and the thick graphite cast sheet of 100 μ m after the drying at room temperature demoulding;
2, zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet are cut into slices respectively according to the mould size;
3, with zirconium boride 99.5004323A8ure sheet and graphite flake alternately stack put into graphite grinding tool, vacuum degreasing, during degreasing, heat-up rate is 2 ℃/min, is warming up to 700 ℃, insulation 0.5h;
4, adopt the argon gas atmosphere hot pressed sintering then, sintering temperature is 1900 ℃, insulation 2h, and pressure is 20MPa, promptly makes stratiform ultrahigh-temperature pottery.
Embodiment 2
1, preparation zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet: the preparation of (1) zirconium boride 99.5004323A8ure curtain coating material, elder generation's weighing 5.51 gram polyvinyl butyral acetals, 5.51 gram polyoxyethylene glycol, 82.68 gram ethanol, stir, add the zirconium boride 99.5004323A8ure powder of 48.72 grams, 2 μ m and the silicon carbide powder of 6.40 grams, 1 μ m again, stir, form zirconium boride 99.5004323A8ure curtain coating material, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 80%: 20% volume percent; (2) preparation of graphite curtain coating material, elder generation's weighing 4.02 gram polyvinyl butyral acetals, 4.02 gram polyoxyethylene glycol, 187.53 gram ethanol, stir, add 20.70 gram powdered graphites and 6.09 gram zirconium boride 99.5004323A8ure powder again, stir, form graphite curtain coating material, wherein powdered graphite and zirconium boride 99.5004323A8ure powder are to take by weighing according to 90%: 10% volume percent; (3) flow casting molding prolongs zirconium boride 99.5004323A8ure curtain coating material and the materials flow of graphite curtain coating respectively, obtains thick zirconium boride 99.5004323A8ure cast sheet of 800 μ m and the thick graphite cast sheet of 50 μ m after the drying at room temperature demoulding;
2, zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet are cut into slices respectively according to the mould size;
3, with zirconium boride 99.5004323A8ure sheet and graphite flake alternately stack put into graphite grinding tool, vacuum degreasing, during degreasing, heat-up rate is 2.5 ℃/min, is warming up to 650 ℃, insulation 1h;
4, adopt the argon gas atmosphere hot pressed sintering then, sintering temperature is 1950 ℃, insulation 1h, and pressure is 30MPa, promptly makes stratiform ultrahigh-temperature pottery.
Embodiment 3
1, preparation zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet: the preparation of (1) zirconium boride 99.5004323A8ure curtain coating material, elder generation's weighing 8.70 gram polyvinyl butyral acetals, 8.70 gram polyvinyl alcohol, 116.02 gram ethanol, stir, add the zirconium boride 99.5004323A8ure powder of 54.81 grams, 5 μ m and the silicon carbide powder of 3.20 grams, 2 μ m again, stir, form zirconium boride 99.5004323A8ure curtain coating material, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 90%: 10% volume percent; (2) preparation of graphite curtain coating material, first weighing 4.6 gram polyvinyl butyral acetals, 4.6 gram polyvinyl alcohol, 230 gram ethanol stir, and add 23 gram powdered graphites again, stir, and form graphite curtain coating material; (3) flow casting molding prolongs zirconium boride 99.5004323A8ure curtain coating material and the materials flow of graphite curtain coating respectively, obtains thick zirconium boride 99.5004323A8ure cast sheet of 200 μ m and the thick graphite cast sheet of 20 μ m after the drying at room temperature demoulding;
2, zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet are cut into slices respectively according to the mould size;
3, with zirconium boride 99.5004323A8ure sheet and graphite flake alternately stack put into graphite grinding tool, vacuum degreasing, during degreasing, heat-up rate is 3 ℃/min, is warming up to 600 ℃, insulation 1h;
4, adopt the argon gas atmosphere hot pressed sintering then, sintering temperature is 2000 ℃, insulation 0.5h, and pressure is 40MPa, promptly makes stratiform ultrahigh-temperature pottery.
Embodiment 4
1, preparation zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet: the preparation of (1) zirconium boride 99.5004323A8ure curtain coating material, elder generation's weighing 8.70 gram polyvinyl butyral acetals, 5 gram polyoxyethylene glycol, 3.70 gram polyvinyl alcohol, 116.02 gram ethanol, stir, add the zirconium boride 99.5004323A8ure powder of 54.81 grams, 5 μ m and the silicon carbide powder of 3.20 grams, 2 μ m again, stir, form zirconium boride 99.5004323A8ure curtain coating material, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 90%: 10% volume percent; (2) preparation of graphite curtain coating material, first weighing 4.6 gram polyvinyl butyral acetals, 3 gram polyoxyethylene glycol, 1 gram polyvinyl alcohol, 230 gram ethanol stir, and add 23 gram powdered graphites again, stir, and form graphite curtain coating material; (3) flow casting molding prolongs zirconium boride 99.5004323A8ure curtain coating material and the materials flow of graphite curtain coating respectively, obtains thick zirconium boride 99.5004323A8ure cast sheet of 200 μ m and the thick graphite cast sheet of 20 μ m after the drying at room temperature demoulding;
2, zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet are cut into slices respectively according to the mould size;
3, with zirconium boride 99.5004323A8ure sheet and graphite flake alternately stack put into graphite grinding tool, vacuum degreasing, during degreasing, heat-up rate is 3 ℃/min, is warming up to 600 ℃, insulation 1h;
4, adopt the argon gas atmosphere hot pressed sintering then, sintering temperature is 2000 ℃, insulation 0.5h, and pressure is 40MPa, promptly makes stratiform ultrahigh-temperature pottery.
Claims (6)
1. the preparation method of zirconium boride-carborundum/graphite laminate ultrahigh-temperature pottery is characterized in that adopting following steps:
1) adopt casting method to prepare zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet respectively: will to stir in binding agent and the softening agent adding solvent earlier, add zirconium boride ceramic powder and graphite ceramic powder more respectively, stir, form the curtain coating material, flow casting molding obtains thick zirconium boride 99.5004323A8ure cast sheet of 200～1000 μ m and the thick graphite cast sheet of 20～100 μ m respectively after the drying at room temperature demoulding then;
2) zirconium boride 99.5004323A8ure cast sheet and graphite cast sheet are cut into slices respectively according to the mould size;
3) with zirconium boride 99.5004323A8ure sheet and graphite flake alternately stack put into graphite grinding tool, vacuum degreasing, during degreasing, heat-up rate is 2～3 ℃/min, is warming up to 600～700 ℃, insulation 0.5～1h;
4) hot pressed sintering under argon gas atmosphere, sintering temperature is 1900～2000 ℃, insulation 0.5～2h, pressure is 20～40MPa, promptly gets stratiform ultrahigh-temperature pottery.
2. the preparation method of zirconium boride-carborundum as claimed in claim 1/graphite laminate ultrahigh-temperature pottery, it is characterized in that: in the step 1), the zirconium boride ceramic powder is by zirconium boride 99.5004323A8ure powder and silicon carbide powder per-cent 70～90% by volume: 10～30% mix, the particle diameter of zirconium boride 99.5004323A8ure powder is 1～5 μ m, and the particle diameter of silicon carbide powder is 0.5～2 μ m.
3. the preparation method of zirconium boride-carborundum as claimed in claim 1/graphite laminate ultrahigh-temperature pottery, it is characterized in that: in the step 1), with zirconium boride ceramic powder weight is basic calculation, takes by weighing binding agent 5～15%, softening agent 5～15% and solvent 100～200% by weight percentage.
4. the preparation method of zirconium boride-carborundum as claimed in claim 1/graphite laminate ultrahigh-temperature pottery is characterized in that: in the step 1), the graphite ceramic powder is by powdered graphite and zirconium boride 99.5004323A8ure powder per-cent 80～100% by volume: 0～20% mixes.
5. the preparation method of zirconium boride-carborundum as claimed in claim 1/graphite laminate ultrahigh-temperature pottery, it is characterized in that: with graphite ceramic powder weight is basic calculation, takes by weighing binding agent 10～20%, softening agent 10～20% and solvent 500～1000% by weight percentage.
6. as the preparation method of claim 1,3 or 5 described zirconium boride-carborundums/graphite laminate ultrahigh-temperature pottery, it is characterized in that: binding agent adopts polyvinyl butyral acetal; The mixing of one or both in softening agent employing polyoxyethylene glycol and the polyvinyl alcohol; Solvent adopts ethanol.
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| CN103360070A (en) * | 2012-03-31 | 2013-10-23 | 深圳光启创新技术有限公司 | Ceramic substrate based metamaterial and preparation method |
| CN104227823A (en) * | 2014-09-11 | 2014-12-24 | 瑞声精密制造科技(常州)有限公司 | Molding method for multilayer structure ceramic product |
| CN104892004A (en) * | 2015-05-18 | 2015-09-09 | 山东理工大学 | Preparation process of highly oriented boron nitride composite material |
| CN104891996A (en) * | 2015-05-18 | 2015-09-09 | 山东理工大学 | Preparation process for highly oriented graphite composite material |
| CN106091791A (en) * | 2016-05-30 | 2016-11-09 | 安徽普瑞普勒传热技术有限公司 | A kind of corrosion-resistant plate type heat exchanger composite surface coating and preparation method thereof |
| CN108249929A (en) * | 2018-01-22 | 2018-07-06 | 哈尔滨工业大学 | A kind of preparation method of the brick of multiple dimensioned toughening-mud structure superhigh temperature ceramic material |
| CN109824382A (en) * | 2019-04-08 | 2019-05-31 | 西安航空学院 | A kind of heat management SiC/ graphite film laminar composite and preparation method thereof |
| CN110156486A (en) * | 2019-05-23 | 2019-08-23 | 西北工业大学 | The preparation method of high tenacity stratiform bullet-resistant ceramic material and the tape casting combination hot pressing sintering method |
| CN115008574A (en) * | 2022-06-30 | 2022-09-06 | 深圳市吉迩科技有限公司 | Forming method of porous ceramic for atomizing core |
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| CN103360070A (en) * | 2012-03-31 | 2013-10-23 | 深圳光启创新技术有限公司 | Ceramic substrate based metamaterial and preparation method |
| CN103360070B (en) * | 2012-03-31 | 2015-11-18 | 深圳光启创新技术有限公司 | A kind of based on ceramic substrate metamaterial and preparation method |
| CN104227823A (en) * | 2014-09-11 | 2014-12-24 | 瑞声精密制造科技(常州)有限公司 | Molding method for multilayer structure ceramic product |
| CN104892004A (en) * | 2015-05-18 | 2015-09-09 | 山东理工大学 | Preparation process of highly oriented boron nitride composite material |
| CN104891996A (en) * | 2015-05-18 | 2015-09-09 | 山东理工大学 | Preparation process for highly oriented graphite composite material |
| CN106091791B (en) * | 2016-05-30 | 2017-11-28 | 安徽普瑞普勒传热技术有限公司 | A kind of corrosion-resistant plate type heat exchanger composite surface coating and preparation method thereof |
| CN106091791A (en) * | 2016-05-30 | 2016-11-09 | 安徽普瑞普勒传热技术有限公司 | A kind of corrosion-resistant plate type heat exchanger composite surface coating and preparation method thereof |
| CN108249929A (en) * | 2018-01-22 | 2018-07-06 | 哈尔滨工业大学 | A kind of preparation method of the brick of multiple dimensioned toughening-mud structure superhigh temperature ceramic material |
| CN108249929B (en) * | 2018-01-22 | 2020-11-27 | 哈尔滨工业大学 | Preparation method of multi-scale toughened brick-mud structure ultrahigh-temperature ceramic material |
| CN109824382A (en) * | 2019-04-08 | 2019-05-31 | 西安航空学院 | A kind of heat management SiC/ graphite film laminar composite and preparation method thereof |
| CN109824382B (en) * | 2019-04-08 | 2021-04-30 | 西安航空学院 | SiC/graphite film layered composite material for thermal management and preparation method thereof |
| CN110156486A (en) * | 2019-05-23 | 2019-08-23 | 西北工业大学 | The preparation method of high tenacity stratiform bullet-resistant ceramic material and the tape casting combination hot pressing sintering method |
| CN115008574A (en) * | 2022-06-30 | 2022-09-06 | 深圳市吉迩科技有限公司 | Forming method of porous ceramic for atomizing core |
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