CN102173810B - Preparation method of layered zirconium boride superhigh temperature ceramic with heat insulation function - Google Patents
Preparation method of layered zirconium boride superhigh temperature ceramic with heat insulation function Download PDFInfo
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- CN102173810B CN102173810B CN 201010622383 CN201010622383A CN102173810B CN 102173810 B CN102173810 B CN 102173810B CN 201010622383 CN201010622383 CN 201010622383 CN 201010622383 A CN201010622383 A CN 201010622383A CN 102173810 B CN102173810 B CN 102173810B
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Abstract
The invention provides a preparation method of layered zirconium boride superhigh temperature ceramic with a heat insulation function. The preparation method is characterized by comprising the following steps: 1) preparing a casting sheet, namely, evenly mixing a binder, a plasticizer and a solvent, adding zirconium boride ceramic powder material to form a casting material, then carrying out casting forming, and drying at room temperature and demoulding to obtain a casting sheet with the thickness of 200-1000 mu m; 2) coating zirconium oxide slurry on the surface of the casting sheet by using a coating method, and controlling the thickness of the coating through coating times; 3) slicing the casting sheet according to the size of a mould; 4) putting the sliced casting sheets in the mould in an overlapping way for vacuum derosination; and 5) carrying out hot pressed sintering in an argon atmosphere so as to obtain the layered zirconium boride superhigh temperature ceramic with heat insulation function, wherein the fracture toughness of the ceramic is up to 9.1MPa.m<1/2>, and the heat conduction of the ceramic vertical to a layer direction is 8w/m.k at room temperature. The fracture mode of the layered zirconium boride ceramic is non-brittle fracture which refers to a gradual fracture having a certain tolerance capability to flaw damage. The layered zirconium boride superhigh temperature ceramic has the advantages of heat insulation function and excellent property.
Description
Technical field
The invention provides a kind of preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function, belong to the preparing technical field of superhigh temperature ceramics.
Background technology
Zirconium boride ceramic has superior high temperature resistant and corrosion resistance nature and relatively low theoretical density, therefore is considered in superhigh temperature ceramics (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, such 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 procedure, must improve the fragility problem of zirconium boride ceramic, thereby improve its thermal shock resistance.Method 1 is to improve fracture toughness property, and method 2 is that to make fracture mode be non-brittle fracture.Existing about preparing the report of ultrahigh-temperature zirconium boride ceramic at present, 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.And fracture mode improvement problem is not reported.
Material is in actual Service Environment simultaneously, and the other end and other device contacts require to have certain heat-proof quality, could prolong like this service life of integral unit, and the zirconium boride 99.5004323A8ure thermal conductivity is 57.9w/mk, and good heat conductivity does not have heat insulating function.The patent No. be CN101391895A's " gradient heat prevention/insulation ceramic base and preparation method thereof " adopt laminating, have 5 layers, have heat insulating function, but each layer is thicker, and during lamination, each layer mixes easily, layer structure is inhomogeneous, and fracture toughness property is 6.0～6.8MPam
1/2, lower.
Summary of the invention
To the objective of the invention is to have zirconium boride ultrahigh-temperature ceramic toughness and the poor problem of heat-proof quality now in order solving, and a kind of preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function to be provided, its technical scheme is:
A kind of preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function is characterized in that adopting following steps:
1) the preparation cast sheet is even with binding agent, softening agent and stirring solvent first, adds the zirconium boride ceramic powder again and forms the curtain coating material, and then flow casting molding obtains the thick cast sheet of 200～1000 μ m after the drying at room temperature demoulding;
2) adopt cladding process, Zirconia Slurry is coated to the cast sheet surface, by applying number of times control coat-thickness;
3) cast sheet is cut into slices according to the mould size;
4) grinding tool is put in the stack of the cast sheet after will cutting into slices, vacuum degreasing, and during degreasing, heat-up rate is 2～3 ℃/min, is warming up to 600～700 ℃, insulation 0.5～1h;
5) hot pressed sintering under argon gas atmosphere, sintering temperature is 1800～1900 ℃, insulation 0.5～2h, pressure is 20～40MPa, namely gets the stratiform zirconium boride ultrahigh-temperature ceramic with heat insulating function.
Described preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function, step 1) in, the zirconium boride ceramic powder of preparation cast sheet is by zirconium boride 99.5004323A8ure powder and silicon carbide powder per-cent 70～90% by volume: 10～30% mix.
Described preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function, step 1) in, take the preparation cast sheet the zirconium boride ceramic powder as basic calculation, take by weighing by weight percentage binding agent 5～10%, softening agent 5～10% and solvent 100～200%.
Described preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function, step 2) in, after the preparation method of Zirconia Slurry is first weighing zirconium white powder, then take zirconium white powder weight as the basis, calculate and take by weighing by weight percentage softening agent 20～30% and deionized water 1000～2000%.
Described preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function, binding agent adopts polyvinyl butyral acetal, and solvent adopts ethanol; The mixing of one or both in softening agent employing polyoxyethylene glycol and the polyvinyl alcohol.
The present invention compared with prior art has following advantage:
1, in the stratiform zirconium boride ultrahigh-temperature ceramic, the zirconium boride 99.5004323A8ure layer is basic unit, zirconia layer is the strong interface layer, when being subject to external force, crackle generation deviation and bifurcated have increased the extensions path of crackle, thereby improved the fracture toughness property of material, simultaneously, zirconium white undergoes phase transition the toughness reinforcing ceramics toughness that also further improved, and splits toughness up to 9.1MPam
1/2
2, owing to have higher intensity and hardness behind the nano zircite layer sintering, do not reduce the intensity of stratiform zirconium boride 99.5004323A8ure matrix material;
3, because the zirconium white thermal conductivity is 2.3w/mk, so reduced the thermal conduction perpendicular to layer direction, make the stratiform zirconium boride ceramic have heat insulating function;
4, block ceramic is brittle rupture, and the one by one fracture of stratiform zirconium boride ceramic for Crack Damage is had certain tolerance.
Description of drawings
Fig. 1 is the SEM photo of the embodiment of the invention 2 gained stratiform superhigh temperature ceramics;
Fig. 2 is the SEM photo of the embodiment of the invention 2 gained stratiform superhigh temperature ceramics sections;
Fig. 3 is the load displacement curve of the embodiment of the invention 2 gained stratiform superhigh temperature ceramics.
Embodiment
Embodiment 1
1, zirconium boride 99.5004323A8ure cast sheet preparation: first weighing 2.61 gram polyvinyl butyral acetals, 2.61 gram polyoxyethylene glycol, 52.23 gram ethanol, make by stirring and to mix, the zirconium boride 99.5004323A8ure powder, 9.60 grams, the 0.5 μ m silicon carbide powder that add again 42.63 grams, 1 μ m, stir and form the curtain coating material, curtain coating, obtain the thick cast sheet of 1000 μ m after the drying at room temperature demoulding, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 70%: 30% volume percent;
2, apply: first weighing 2 gram polyoxyethylene glycol addings 100 gram deionized water for stirring are even, add 10 gram zirconium whites again and form slip; Then adopt cladding process, Zirconia Slurry is coated to the cast sheet upper surface, apply 1 time;
3, cast sheet is cut into slices according to the mould size;
4, grinding tool is put in the stack of the cast sheet after will cutting into slices, vacuum degreasing, and during degreasing, heat-up rate is 2 ℃/min, is warming up to 700 ℃, insulation 1h;
5, hot pressed sintering under argon gas atmosphere, sintering temperature is 1800 ℃, insulation 0.5h, pressure is 40MPa, namely gets the stratiform zirconium boride ultrahigh-temperature ceramic.
Embodiment 2
1, zirconium boride 99.5004323A8ure cast sheet preparation: first weighing 5.51 gram polyvinyl butyral acetals, 5.51 gram polyoxyethylene glycol, 82.68 gram ethanol, make by stirring and to mix, the zirconium boride 99.5004323A8ure powder, 6.40 grams, the 1 μ m silicon carbide powder that add again 48.72 grams, 2 μ m, stir and form the curtain coating material, curtain coating, obtain the thick cast sheet of 700 μ m after the drying at room temperature demoulding, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 80%: 20% volume percent;
2, apply: first weighing 3 gram polyvinyl alcohol addings 150 gram deionized water for stirring are even, add 10 gram zirconium whites again and form slip; Then adopt cladding process, Zirconia Slurry is coated to the cast sheet upper surface, apply 2 times;
3, cast sheet is cut into slices according to the mould size;
4, grinding tool is put in the stack of the cast sheet after will cutting into slices, vacuum degreasing, and during degreasing, heat-up rate is 2.5 ℃/min, is warming up to 700 ℃, insulation 1h;
5, hot pressed sintering under argon gas atmosphere, sintering temperature is 1850 ℃, insulation 1h, pressure is 30MPa, namely gets the stratiform zirconium boride ultrahigh-temperature ceramic.
Embodiment 3
1, zirconium boride 99.5004323A8ure cast sheet preparation: first weighing 4.06 gram polyvinyl butyral acetals, 4.06 gram polyvinyl alcohol, 116.02 gram ethanol, make by stirring and to mix, the zirconium boride 99.5004323A8ure powder, 3.20 grams, the 2 μ m silicon carbide powders that add again 54.81 grams, 5 μ m, stir and form the curtain coating material, curtain coating, obtain the thick cast sheet of 200 μ m after the drying at room temperature demoulding, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 90%: 10% volume percent;
2, apply: first weighing 2.5 gram polyvinyl alcohol addings 200 gram deionized water for stirring are even, add 10 gram zirconium whites again and form slip; Then adopt cladding process, Zirconia Slurry is coated to the cast sheet upper surface, apply 3 times;
3, cast sheet is cut into slices according to the mould size;
4, grinding tool is put in the stack of the cast sheet after will cutting into slices, vacuum degreasing, and during degreasing, heat-up rate is 3 ℃/min, is warming up to 700 ℃, insulation 1h;
5, hot pressed sintering under argon gas atmosphere, sintering temperature is 1900 ℃, insulation 2h, pressure is 20MPa, namely gets the stratiform zirconium boride ultrahigh-temperature ceramic.
Embodiment 4
1, zirconium boride 99.5004323A8ure cast sheet preparation: first weighing 4.06 gram polyvinyl butyral acetals, 4 gram polyoxyethylene glycol, 1 gram polyvinyl alcohol, 116.02 gram ethanol, make by stirring and to mix, the zirconium boride 99.5004323A8ure powder, 3.20 grams, the 2 μ m silicon carbide powders that add again 54.81 grams, 2 μ m, stir and form the curtain coating material, curtain coating, obtain the thick cast sheet of 200 μ m after the drying at room temperature demoulding, wherein zirconium boride 99.5004323A8ure powder and silicon carbide powder are to take by weighing according to 90%: 10% volume percent;
2, apply: it is even that first weighing 1.5 gram polyoxyethylene glycol, 1 restrain polyvinyl alcohol adding 100 gram deionized water for stirring, adds 10 gram zirconium whites again and form slip; Then adopt cladding process, Zirconia Slurry is coated to the cast sheet upper surface, apply 2 times;
3, cast sheet is cut into slices according to the mould size;
4, grinding tool is put in the stack of the cast sheet after will cutting into slices, vacuum degreasing, and during degreasing, heat-up rate is 3 ℃/min, is warming up to 700 ℃, insulation 1h;
5, hot pressed sintering under argon gas atmosphere, sintering temperature is 1900 ℃, insulation 2h, pressure is 20MPa, namely gets the stratiform zirconium boride ultrahigh-temperature ceramic.
Claims (4)
1. preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function is characterized in that adopting following steps:
1) preparation cast sheet, first that binding agent, softening agent and stirring solvent is even, add again the zirconium boride ceramic powder and form the curtain coating material, then flow casting molding, obtain the thick cast sheet of 200～1000 μ m after the drying at room temperature demoulding, the zirconium boride ceramic powder that wherein prepares cast sheet is by zirconium boride 99.5004323A8ure powder and silicon carbide powder per-cent 70～90% by volume: 10～30% mix;
2) adopt cladding process, Zirconia Slurry is coated to the cast sheet surface, by applying number of times control coat-thickness, after wherein the preparation method of Zirconia Slurry is first weighing zirconium white powder, then take zirconium white powder weight as the basis, calculate and take by weighing by weight percentage softening agent 20～30% and deionized water 1000～2000%;
3) cast sheet is cut into slices according to the mould size;
4) grinding tool is put in the stack of the cast sheet after will cutting into slices, vacuum degreasing, and during degreasing, heat-up rate is 2～3 ℃/min, is warming up to 600～700 ℃, insulation 0.5～1h;
5) hot pressed sintering under argon gas atmosphere, sintering temperature is 1800～1900 ℃, insulation 0.5～2h, pressure is 20～40MPa, namely gets the stratiform zirconium boride ultrahigh-temperature ceramic with heat insulating function.
2. the preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function as claimed in claim 1, it is characterized in that: step 1) in, take the preparation cast sheet the zirconium boride ceramic powder as basic calculation, take by weighing by weight percentage binding agent 5～10%, softening agent 5～10% and solvent 100～200%.
3. the preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function as claimed in claim 1 or 2 is characterized in that: binding agent employing polyvinyl butyral acetal, solvent employing ethanol.
4. the preparation method with stratiform zirconium boride ultrahigh-temperature ceramic of heat insulating function as claimed in claim 1 or 2 is characterized in that: the mixing of one or both in softening agent employing polyoxyethylene glycol and the polyvinyl alcohol.
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| CN111848158B (en) * | 2020-06-18 | 2022-10-04 | 日照鼎源新材料有限公司 | Method for preparing straight-through-hole zirconia ceramic with compact hole wall by wet spinning coextrusion |
| CN112898027A (en) * | 2021-02-28 | 2021-06-04 | 唐明明 | Novel heat-preservation and heat-insulation ceramic material and preparation method thereof |
| CN114804843B (en) * | 2022-05-10 | 2023-05-02 | 佛山市东鹏陶瓷有限公司 | High-strength ultrathin rock plate and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844925A (en) * | 2010-05-21 | 2010-09-29 | 李艳 | Process for preparing multilayer ZrB2-SiC complex phase ultrahigh temperature ceramic wafer material by tape casting |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844925A (en) * | 2010-05-21 | 2010-09-29 | 李艳 | Process for preparing multilayer ZrB2-SiC complex phase ultrahigh temperature ceramic wafer material by tape casting |
Non-Patent Citations (2)
| Title |
|---|
| Processing and properties of ZrB2–SiC composites obtained by aqueous tape casting and hot pressing;Zhihui Lü et al.;《ceramics international》;20100929;第37卷;第293页摘要 * |
| Zhihui Lü et al..Processing and properties of ZrB2–SiC composites obtained by aqueous tape casting and hot pressing.《ceramics international》.2010,第37卷第293页摘要. |
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