CN100439286C - Method for preparing super high temperature complex phase ceramic ZrB2-ZrC-SiC near to zero ablation - Google Patents
Method for preparing super high temperature complex phase ceramic ZrB2-ZrC-SiC near to zero ablation Download PDFInfo
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Abstract
This invention relates to a method for preparing ZrB2-ZrC-SiC multiphase ceramic at ultrahigh temperatures with near-zero ablation. The ZrB2-ZrC-SiC multiphase ceramic is prepared from: ZrB2 50-75 wt.%, ZrC 15-40 wt.%, SiC 10-20 wt.%, and ZrO2 as the combustion aid 6-16 wt.%. The ZrB2-ZrC-SiC multiphase ceramic has synergistic effects at high temperatures, which can result in good high-temperature properties. The ZrB2-ZrC-SiC multiphase ceramic has a room-temperature bending strength of 300-400 MPa, a Rockwell hardness of 88-92, and a linear ablation of 0.0003-0.001 mm/s. The ZrB2-ZrC-SiC multiphase ceramic has better oxidation resistance, better ablation resistance and lower sintering temperature compared with single phase ceramics, and has such advantages as good applicability, even distribution, no limit to product shapes and little shape change after 2400 s oxygen-ethylene combustion at 2800-3200 deg.C.
Description
Technical field
The present invention relates to a kind of ultrahigh-temperature near to zero ablation ZrB
2The preparation method of-ZrC-SiC complex phase ceramic belongs to the special cermacis technical field.
Background technology
When the aerospace aircraft flies in the atmospheric layer high speed,, on thermally protective materials, produce serious pneumatic heating because the surface is subjected to the friction of atmospheric layer air-flow.Raising along with Mach number, the thermal protection technology of aircraft becomes more and more important, especially the material to uses such as nose cone cap, nose of wing, boattails has proposed more and more high requirement, and not ablate, have the demand of hyperthermal material of excellent abrasive resistance and heat-shock resistance more and more urgent to standing high temperature more than 2000 ℃ and not oxidation of long duration of action.
The hyperthermal material that uses mainly contains refractory metal, C/C material at present.Though refractory metal for example refractory metal such as W, Re has high melt point, its density is big, and oxidation-resistance is poor; Though the C/C material has high specific strength, highly heatproof and shockproof, low thermal coefficient of expansion, because C/C material at high temperature antioxidant property is poor, since just obvious oxidation more than 450 ℃, along with the rising of temperature, it is anti-worse and worse ablative.Therefore, these two kinds of materials are difficult to satisfy the needs of hypersonic aircraft thermal protection system.
Ultrahigh-temperature near to zero ablation pottery is meant in rigorous environment such as heavily stressed, strong oxidation and ablates (ablation rate＜0.001mm/s) and the most heat-stable advanced ceramic that still can use as usual hardly under ultrahigh-temperature state more than 2200 ℃.Mainly comprise HfB
2, ZrB
2, HfC, ZrC and SiC etc. with and various matrix material, developed first by United States Air Force before 40 years, demonstrated excellent high-temperature behavior, be the most promising material in following ultrahigh-temperature field.
Single-phase ZrB
2Have good oxidation-resistance below 1200 ℃, this is because liquid B
2O
3Good anti-oxidation protection effect has been played in the generation of glassy phase.More than 1200 ℃ the time, rapid evaporation, thus reduced it as a kind of effectiveness that spreads obstacle, ZrB
2Quick oxidation will take place.Add SiC and can significantly improve its antioxidant property, when high temperature, form the top layer that pyrex can covering material, stop that effectively oxygen spreads to material internal.The ZrC face-centred cubic structure, its fusing point is higher than ZrB
2, have excellent high-temperature behavior, but 1400 ℃ of strong oxidations of beginning in the air.Therefore, realize ZrB
2, ZrC the ultrahigh-temperature performance, must carry out modification, and to ZrB
2, to be optimized design be the optimal path of realizing this goal for ZrC, SiC component.
ZrB
2, ZrC, SiC class material be the extremely strong covalent linkage compound of bond energy, fusing point height, sintering activity are low, and traditional sintering processing is difficult to adopt the hot pressed mode of high temperature just can make its densification usually its densification, there is following problem in high temperature hot pressing: (1) production efficiency is low, and cost is high; (2) can only prepare the goods of simple shape, bad adaptability; (3) goods axially and the lateral performance existence than big-difference, the ablation rate height, heat-shock resistance is relatively poor; Deng, can not satisfy actual requirement.
Summary of the invention
The object of the present invention is to provide a kind of ultrahigh-temperature near to zero ablation ZrB
2The preparation method of-ZrC-SiC complex phase ceramic, batching rationally conveniently implement, and cost is low, and adaptability is strong, the good product quality of acquisition.
Ultrahigh-temperature near to zero ablation ZrB of the present invention
2The preparation method of-ZrC-SiC complex phase ceramic, through batching, grinding, granulation, moulding with burn till and make, its raw material weight per distribution ratio is: ZrB
250～75%, ZrC 15～40% and SiC 10～20% add ZrO
2Sintering aid 6～16%.
Batching is used powder, ZrB
2, ZrC and SiC powder the meta particle diameter be 1～3 μ m, ZrO
2The meta particle diameter of powder is smaller or equal to 1 μ m.
Batching needs ultrasonic dispersing after ball milling, slip is uniformly dispersed, and guarantees sintering aid ZrO
2At ZrB
2, the homogeneity among the ZrC, SiC powder.General control frequency of ultrasonic is 20～25KHz.
Slip after the ball milling is crossed 300 mesh sieves, and through the granulation of centrifugal granulating drying machine, generally controlling rate of feeding is 5～10Kg/h, and drying temperature is 180～200 ℃, and granulation material particle size range is 0.5～2mm.
Isostatic cool pressing (CIP) moulding is adopted in moulding, and forming pressure is controlled to be 150～200MPa.
The product calcining system is: argon gas atmosphere protection pressureless sintering (promptly normal pressure-sintered, as to need not to exert pressure) down, 1700～1900 ℃ of sintering temperatures, high-temperature holding time 2～3h, naturally cooling.Pressureless sintering, and firing temperature is the highest 1900 ℃, lower, convenient enforcement, cost is low.
Among the present invention, ZrB
2/ ZrC/SiC system at high temperature can produce synergistic effect, has excellent high, compares with one-component ceramic, and complex phase ceramic has higher oxidation-resistance and anti-ablation property and lower sintering temperature.ZrO during high temperature
2With ZrB
2, ZrC, SiC particle surface impurity (as: B
2O
3, SiO
2Deng) form low-temperature eutectic phase (Zr-Si-B-O), can effectively promote ZrB
2The sintering densification of/ZrC/SiC system.And pass through ZrO
2The control of addition is not influencing ZrB
2Further reduced sintering temperature under the prerequisite of/ZrC/SiC system heatproof, anti-oxidant, anti-ablation property, production efficiency is improved, cost reduces greatly, and adopt not have to press and burn till, and has overcome hot pressing and has burnt till restriction to article shape, and adaptability is good.The complex phase ceramic material of preparation is even, room temperature bending strength 300～400MPa, Rockwell hardness 88～92, according to the GJB-323A-96 standard, under 2800～3000 ℃ of ablation under ultra high temperature conditions of oxy-acetylene flame, change hardly through 2400s simulation examination shape, linear ablative rate is 0.0003～0.001mm/s, near zero ablation.
Description of drawings
Fig. 1, process flow diagram of the present invention.
Fig. 2, burn till before raw material form synoptic diagram.
Fig. 3, burn till back complex phase ceramic thing phase composite synoptic diagram.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Ultrahigh-temperature near to zero ablation ZrB of the present invention
2The preparation method of-ZrC-SiC complex phase ceramic, carry out according to the following step:
Be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 60%, 25% and 15%; add 12% and take by weighing powder; the meta particle diameter of four kinds of powders is respectively: 1.5 μ m, 1.3,1.0 μ m and 0.5 μ m; with deionized water as dispersion agent; ball milling mixes, the 25KHz ultra-sonic dispersion is even, passes through the granulation of centrifugal drying tablets press behind 300 mesh sieves excessively, and rate of feeding is 8Kg/h; drying temperature is 200 ℃, and granulation material particle diameter is 0.5～2mm.In the oil resisting rubber grinding tool of evenly packing into special then, moulding in the wet method isostatic pressing machine, top pressure is 180MPa.Pack into the pressureless sintering kiln roasting of the indignant protection of argon gas of the print of forming, maximum sintering temperature is 1800 ℃, is incubated 2 hours.Naturally cooling gets final product.With the print that sinters according to the requirement of different tests to test piece, be worked into desired precision according to traditional cold working method after, carry out the test of relevant performance, performance sees Table 1.
Embodiment 2
Be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 50%, 35% and 15%, add 12% and take by weighing powder, other is with embodiment 1.Performance sees Table 1.
Embodiment 3
Be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 70%, 20% and 10%, add 12% and take by weighing powder, other is with embodiment 1.Performance sees Table 1.
Embodiment 4
Be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 60%, 25% and 15%, add 10% and take by weighing powder, other is with embodiment 1.Performance sees Table 1.
Embodiment 5
Be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 60%, 25% and 15%, add 14% and take by weighing powder, other is with embodiment 1.Performance sees Table 1.
Embodiment 6
Sintering temperature is changed into 1750 ℃, and other is with embodiment 1.Performance sees Table 1.
Embodiment 7
Sintering temperature is changed into 1850 ℃, and other is with embodiment 1.Performance sees Table 1.
Table 1, material property table
| The example example | ZrB 2∶ZrC∶SiC ZrO 2Weight (wt%) | Densification degree (%) | Luo Shi hardness (H RA) | Bending strength (Mpa) | The oxy-acetylene temperature (℃) | Linear ablative rate (* 10 -4mm/s) |
| 1 | 60∶25∶15 12 | 93.2％ | 91 | 396 | 2950 | 3.2 |
| 2 | 50∶35∶15 12 | 90.2％ | 90 | 323 | 2855 | 8.0 |
| 3 | 70∶20∶10 12 | 95.0 | 91 | 330 | 2890 | 5.5 |
| 4 | 60∶25∶15 10 | 91.3％ | 90 | 355 | 2900 | 5.0 |
| 5 | 60∶25∶15 14 | 94.1％ | 91 | 366 | 2910 | 4.1 |
| 6 | 60∶25∶15 12 | 87％ | 88 | 300 | 2900 | 7.2 |
| 7 | 60∶25∶15 12 | 96.2％ | 92 | 390 | 2900 | 3.9 |
Embodiment 8, ultrahigh-temperature near to zero ablation ZrB of the present invention
2The preparation method of-ZrC-SiC complex phase ceramic carries out according to the following step: be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 62%, 26% and 12%; add 15% and take by weighing powder; the meta particle diameter of four kinds of powders is respectively: 1.5 μ m, 1.2,1.0 μ m and 0.8 μ m; with deionized water as dispersion agent; ball milling mixes, the 20KHz ultra-sonic dispersion is even, passes through the granulation of centrifugal drying tablets press behind 300 mesh sieves excessively, and rate of feeding is 7Kg/h; drying temperature is 180 ℃, and granulation material particle size range is 0.5～2mm.In the oil resisting rubber grinding tool of evenly packing into special then, moulding in the wet method isostatic pressing machine, top pressure is 190MPa.Pack into the pressureless sintering kiln roasting of the indignant protection of argon gas of the print of forming, maximum sintering temperature is 1870 ℃, being incubated after 2.2 hours naturally, cooling gets final product.
Embodiment 9, ultrahigh-temperature near to zero ablation ZrB of the present invention
2The preparation method of-ZrC-SiC complex phase ceramic carries out according to the following step: be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 56%, 30% and 14%; add 8% and take by weighing powder; the meta particle diameter of four kinds of powders is respectively: 1.3 μ m, 1.0,1.2 μ m and 0.6 μ m; with deionized water as dispersion agent; ball milling mixes, the 23KHz ultra-sonic dispersion is even, passes through the granulation of centrifugal drying tablets press behind 300 mesh sieves excessively, and rate of feeding is 9Kg/h; drying temperature is 190 ℃, and granulation material particle size range is 0.5～1.5mm.In the oil resisting rubber grinding tool of evenly packing into special then, moulding in the wet method isostatic pressing machine, top pressure is 160MPa.Pack into the pressureless sintering kiln roasting of the indignant protection of argon gas of the print of forming, maximum sintering temperature is 1820 ℃, being incubated after 2.4 hours naturally, cooling gets final product.
Embodiment 10, ultrahigh-temperature near to zero ablation ZrB of the present invention
2The preparation method of-ZrC-SiC complex phase ceramic carries out according to the following step: be ZrB by weight ratio
2, ZrC and SiC and add ZrO
2Be respectively 62%, 20% and 18%; add 13% and take by weighing powder; the meta particle diameter of four kinds of powders is respectively: 2 μ m, 1.0,1.1 μ m and 0.5 μ m; with deionized water as dispersion agent; ball milling mixes, the 25KHz ultra-sonic dispersion is even, passes through the granulation of centrifugal drying tablets press behind 300 mesh sieves excessively, and rate of feeding is 8Kg/h; drying temperature is 200 ℃, and granulation material particle size range is 0.7～1.8mm.In the oil resisting rubber grinding tool of evenly packing into special then, moulding in the wet method isostatic pressing machine, top pressure is 195MPa.Pack into the pressureless sintering kiln roasting of the indignant protection of argon gas of the print of forming, maximum sintering temperature is 1780 ℃, being incubated after 2.6 hours naturally, cooling gets final product.
Claims (6)
1, a kind of ultrahigh-temperature near to zero ablation ZrB
2The preparation method of-ZrC-SiC complex phase ceramic through batching, grinding, granulation, moulding with burn till and make, is characterized in that the raw material weight per distribution ratio is: ZrB
250～75%, ZrC 15～40% and SiC 10～20% add ZrO
2Sintering aid 6～16%.
2, ultrahigh-temperature near to zero ablation ZrB according to claim 1
2The preparation method of-ZrC-SiC complex phase ceramic is characterized in that batching is powder, ZrB
2, ZrC and SiC powder the meta particle diameter be 1～3 μ m, ZrO
2The meta particle diameter of powder is smaller or equal to 1 μ m.
3, ultrahigh-temperature near to zero ablation ZrB according to claim 2
2The preparation method of-ZrC-SiC complex phase ceramic is characterized in that batching needs ultrasonic dispersing after ball milling.
4, according to claim 1,2 or 3 described ultrahigh-temperature near to zero ablation ZrB
2The preparation method of-ZrC-SiC complex phase ceramic is characterized in that the slip after the ball milling is crossed 300 mesh sieves, and through the granulation of centrifugal granulating drying machine, rate of feeding is 5～10Kg/h, and drying temperature is 180～200 ℃, and granulation material particle size range is 0.5～2mm.
5, ultrahigh-temperature near to zero ablation ZrB according to claim 4
2The preparation method of-ZrC-SiC complex phase ceramic is characterized in that moulding employing cold isostatic compaction, and forming pressure is controlled to be 150～200MPa.
6, ultrahigh-temperature near to zero ablation ZrB according to claim 5
2The preparation method of-ZrC-SiC complex phase ceramic is characterized in that calcining system is: the argon gas atmosphere protection is normal pressure-sintered down, 1700～1900 ℃ of sintering temperatures, high-temperature holding time 2～3h, naturally cooling.
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| CN101844925B (en) * | 2010-05-21 | 2012-05-23 | 李艳 | Tape casting method for preparing multilayer ZrB2Process for preparing-SiC complex phase superhigh temperature ceramic plate material |
| CN103207128A (en) * | 2012-10-11 | 2013-07-17 | 湖北航天化学技术研究所 | Determination method for ablation residue ratio of heat-insulating material |
| CN104388881A (en) * | 2014-11-26 | 2015-03-04 | 西安工业大学 | Anti-ablation composite coating and preparation method thereof |
| CN113773090B (en) * | 2021-11-15 | 2022-02-18 | 长沙理工大学 | A kind of preparation method of ZrB2-ZrC-SiC nanocomposite ceramic material |
| CN114230348A (en) * | 2022-01-18 | 2022-03-25 | 吉林大学 | A high-pressure preparation method of high-density ZrB2-based ultra-high temperature ceramics |
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Assignee: Zibo Bo Bo Electronic Ceramics Co., Ltd. Assignor: Sinoma high and new material Limited by Share Ltd|Shandong Industrial Ceramic Research & Design Institute Contract record no.: 2010370000280 Denomination of invention: Method for preparing ultra high temperature near zero ablation ZrB*-ZrC-SiC multiphase ceramic Granted publication date: 20081203 License type: Exclusive License Open date: 20070221 Record date: 20100521 |