CN103787684A - Preparation method of high-temperature resistant nitride based ceramic wave-transmitting composite material - Google Patents
Preparation method of high-temperature resistant nitride based ceramic wave-transmitting composite material Download PDFInfo
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- CN103787684A CN103787684A CN201410031273.2A CN201410031273A CN103787684A CN 103787684 A CN103787684 A CN 103787684A CN 201410031273 A CN201410031273 A CN 201410031273A CN 103787684 A CN103787684 A CN 103787684A
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Abstract
The invention discloses a preparation method of a high-temperature resistant nitride based ceramic wave-transmitting composite material. The method comprises the following steps: soaking a quartz fiber woven body in a BN (boron nitride) precursor solution and a polyborosilazane precursor solution successively for multiple times to enable the precursor solutions to effectively soak into the woven body, performing high-temperature heat treatment cross-linking and solidifying and high-temperature pyrolyzing to form a rough blank, and machining the rough blank to obtain the high-temperature nitride based ceramic wave-transmitting composite material. The prepared high-temperature nitride based ceramic wave-transmitting composite material can meet the usage requirement of high temperature of 1800 DEG C and can be applied to an antenna housing for an intermediate-and-long-range ground-to-ground missile. The prepared quartz fiber reinforced nitride based ceramic wave-transmitting composite material has good mechanical property and high temperature resistance, can meet the usage requirement of high temperature more than 1800 DEG C and has a good application prospect on the antenna housing for the intermediate-and-long-range ground-to-ground missile.
Description
Technical field
The present invention relates to missile weapon system refractory ceramics base wave-penetrating composite material preparing technical field, refer to particularly a kind of preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing, can be used for medium-long range ground tactics and strategy high temperature resistant radome electromagnetic wave transparent material for guided missile.
Background technology
Along with the development of aeronautical and space technology, the flight Mach number of missile weapon system improves constantly, the reentry velocity of ground intermediate range missile has reached 10～12Ma, and the speed that is written into of long-range missile of new generation can be up to 15～18Ma, this power, thermal environment that missile-borne radome is faced is more and more harsher.Particularly can suffer serious high temperature, high pressure, noise, vibrations, impact and overload when medium-long range ground ground ballistic missile reentry atmospheric layer, now the temperature at position, radome stationary point can be up to more than 1800 ℃.Current compound quartz-ceramics of being used widely cannot use for a long time under this high temperature, has been difficult to meet the service requirements of New Generation Missile radome.And novel nitride based ceramic penetrating wave matrix material resistance to elevated temperatures is good, can meet 1800 ℃ of applied at elevated temperature requirements, and its wave penetrate capability is good, be a kind of high temperature resistant radome wave-penetrating composite material for long-and medium-range missiles with applications well prospect.
Summary of the invention
Technical problem to be solved by this invention is just to provide a kind of preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing, the method adopts silica fibrage body successively to flood BN precursor solution and poly-boron nitrogen silane precursor liquid solution, through repeatedly flooding, make precursor solution effectively infiltrate through knitted body inside, then after high-temperature heat treatment crosslinking curing, Pintsch process, form crude green body, then be desired product after machined.The high temperature resistant nitride based ceramic penetrating wave matrix material of preparation can meet the applied at elevated temperature requirement of 1800 ℃, can be applied to medium-long range radome, antenna windows etc. for ground-to-ground missile.。
For solving the problems of the technologies described above, the preparation method of a kind of high temperature resistant nitride based ceramic penetrating wave composite material forming thing provided by the invention, comprises the following steps:
1), according to predefined shaped object shape and size, knit out satisfactory silica fibrage body;
2) silica fibrage body is put into boiling water poach 25～45h, after oven dry, under 300～500 ℃ of conditions, lead to oxygen roasting 1～3h, then it is carried out to cleanup acid treatment, after pickling, silica fibrage body is washed, remove its surperficial acid solution, again dry;
3), under vacuum condition, the silica fibrage body of again drying is placed in to BN precursor solution and floods 1～3h;
4) after dipping, silica fibrage body is carried out to vacuum-drying, remove the solvent in silica fibrage body;
5) repeating step 3) to the operation of step 4) 2～4 times;
6) will gather boron nitrogen silane and pulverize, then with dimethylbenzene according to mass ratio 5～6: 10 ratio is mixed, fully stirring and dissolving, preparation obtains gathering boron nitrogen silane precursor liquid solution;
7) under vacuum state, the poly-boron nitrogen silane precursor liquid solution of step 6) preparation will be placed in through the silica fibrage body of step 5) processing, dipping time is 1～3h, then starts to vibrate poly-boron nitrogen silane precursor liquid solution 30～60min, then silica fibrage body is taken out to Air drying;
8) repeating step 7) operation 2～3 times;
9) by being placed in thermal treatment 1～2h under 500～700 ℃ of conditions through the silica fibrage body of step 8) processing, make two kinds of presoma crosslinking curings, realize preliminary cracking;
10) be thermal treatment 1～2h under 750～950 ℃ of conditions by being placed in temperature through the silica fibrage body of step 9) processing again, make two kinds of further crosslinking curings of presoma, realize degree of depth Pintsch process, make its half ceramic form crude green body;
11) gained crude green body is machined into desired product size, obtains high temperature resistant nitride based ceramic penetrating wave composite material forming thing.
Further, described step 2) in, pickling acid solution used is according to concentrated hydrochloric acid: volume ratio=1～3 of concentrated nitric acid: 1 preparation.
Again further, in described step 3), vacuum tightness is-60～-70KPa; BN precursor solution temperature is 40～60 ℃.
Again further, in described step 4), vacuum tightness is-30～-50KPa, and drying temperature is 200～300 ℃, and be 3h～5h time of drying.
Again further, in described step 7), vacuum tightness is-60～-70KPa; Poly-boron nitrogen silane precursor solution temperature is 40～60 ℃.
Again further, in described step 7), be 4～6h time of drying.
Beneficial effect of the present invention is:
1) this moulding technique adopts and repeatedly floods recombination process, makes BN precursor solution and poly-boron nitrogen silane precursor liquid solution can fully infiltrate through fibrage body inside.
2) this moulding technique adopts twice thermal treatment, and proceed step by step crosslinking curing, Pintsch process make presoma can fully carry out crosslinking curing and cracking, can improve the density of material simultaneously.
3) the Silica Fibers Reinforced Nitride ceramic penetrating wave matrix material that prepared by the present invention, there is good mechanical property and resistance to elevated temperatures, can meet 1800 ℃ of above applied at elevated temperature requirements, on medium-long range ground-to-ground missile radome, have a good application prospect.
Embodiment
In order to explain better the present invention, further illustrate main contents of the present invention below in conjunction with specific embodiment, but content of the present invention is not only confined to following examples.
Embodiment 1
The high temperature resistant nitride based ceramic penetrating wave composite material and preparation method thereof of certain intermediate range missile high temperature resistant wave-permeable radome cover body, comprises the following steps:
1), according to radome cover body dimensional requirement, knit out satisfactory radome cover body silica fibrage body;
2) silica fibrage body is put into boiling water poach 35h, after oven dry, under 400 ℃ of conditions, lead to oxygen roasting 2h, then it is carried out to cleanup acid treatment, after pickling, silica fibrage body is washed, remove its surperficial acid solution, again dry, pickling acid solution used is according to concentrated hydrochloric acid: volume ratio=3 of concentrated nitric acid: 1 preparation;
3) in vacuum tightness be-vacuum condition of 65KPa under, it is that the BN precursor solution of 50 ℃ floods 2h that the silica fibrage body of again drying is placed in to temperature;
4) after dipping, to silica fibrage body in vacuum tightness be-40KPa, temperature carry out vacuum-drying 4h under the condition of 250 ℃, remove the solvent in silica fibrage body;
5) repeating step 3) to the operation of step 4) 3 times;
6) will gather boron nitrogen silane and pulverize, then mix according to the ratio of mass ratio 11 ︰ 20 with dimethylbenzene, fully stirring and dissolving, preparation obtains poly-boron nitrogen silane precursor liquid solution;
7) in vacuum tightness be-vacuum state of 70KPa under, be 50 ℃ ± 5 ℃ poly-boron nitrogen silane precursor liquid solutions by the temperature that is placed in step 6) preparation through the silica fibrage body of step 5) processing, dipping time is 3h, then start to vibrate poly-boron nitrogen silane precursor liquid solution 50min, then silica fibrage body is taken out to Air drying 5h;
8) repeating step 7) operation 2～3 times;
9) by being placed in thermal treatment 1～2h under 600 ℃ of conditions through the silica fibrage body of step 8) processing, make two kinds of presoma crosslinking curings, realize preliminary cracking;
10) be thermal treatment 2h under 950 ℃ of conditions by being placed in temperature through the silica fibrage body of step 9) processing again, make two kinds of further crosslinking curings of presoma, realize degree of depth Pintsch process, make its half ceramic form crude green body;
11) gained crude green body is machined into desired product size, obtains high temperature resistant nitride based ceramic penetrating wave composite antenna housing cover body.
The high temperature resistant nitride based ceramic penetrating wave composite antenna housing cover body preparing stands to simulate actual working environment examination and without destruction: 1700～1800 ℃ of position, stationary point temperature, 1200～1400 ℃ of big area temperature.Product is as follows with stove sample performance:
Embodiment 2
The high temperature resistant nitride based ceramic penetrating wave composite material and preparation method thereof of certain intermediate range missile high temperature resistant wave-permeable radome cover body, comprises the following steps:
1), according to the requirement of radome cover body, knit out satisfactory radome cover body silica fibrage body;
2) silica fibrage body is put into boiling water poach 30h, after oven dry, under 400 ℃ of conditions, lead to oxygen roasting 2h, then it is carried out to cleanup acid treatment, after pickling, silica fibrage body is washed, remove its surperficial acid solution, again dry, pickling acid solution used is according to concentrated hydrochloric acid: volume ratio=2 of concentrated nitric acid: 1 preparation;
3) in vacuum tightness be-vacuum condition of 70KPa under, it is that the BN precursor solution of 60 ℃ floods 2h that the silica fibrage body of again drying is placed in to temperature;
4) after dipping, to silica fibrage body in vacuum tightness be-50KPa, temperature carry out vacuum-drying 3h under the condition of 300 ℃, remove the solvent in silica fibrage body;
5) repeating step 3) to the operation of step 4) 2 times;
6) will gather boron nitrogen silane and pulverize, then mix according to the ratio of mass ratio 1 ︰ 2 with dimethylbenzene, fully stirring and dissolving, preparation obtains poly-boron nitrogen silane precursor liquid solution;
7) in vacuum tightness be-vacuum state of 60KPa under, be 50 ℃ ± 5 ℃ poly-boron nitrogen silane precursor liquid solutions by the temperature that is placed in step 6) preparation through the silica fibrage body of step 5) processing, dipping time is 2h, then start to vibrate poly-boron nitrogen silane precursor liquid solution 50min, then silica fibrage body is taken out to Air drying 5h;
8) repeating step 7) operation 3 times;
9) by being placed in thermal treatment 1h under 700 ℃ of conditions through the silica fibrage body of step 8) processing, make two kinds of presoma crosslinking curings, realize preliminary cracking;
10) be thermal treatment 1h under 800 ℃ of conditions by being placed in temperature through the silica fibrage body of step 9) processing again, make two kinds of further crosslinking curings of presoma, realize degree of depth Pintsch process, make its half ceramic form crude green body;
11) gained crude green body is machined into desired product size, obtains high temperature resistant nitride based ceramic penetrating wave composite antenna housing cover body.
The high temperature resistant nitride based ceramic penetrating wave composite antenna housing cover body preparing stands to simulate actual working environment examination and without destruction: 1700～1800 ℃ of position, stationary point temperature, 1200～1400 ℃ of big area temperature.Product is as follows with stove sample performance:
Embodiment 3
The high temperature resistant nitride based ceramic penetrating wave composite material and preparation method thereof of certain intermediate range missile high temperature resistant wave-permeable radome cover body, comprises the following steps:
1), according to radome cover body dimensional requirement, knit out satisfactory radome cover body silica fibrage body;
2) silica fibrage body is put into boiling water poach 45h, after oven dry, under 500 ℃ of conditions, lead to oxygen roasting 1h, then it is carried out to cleanup acid treatment, after pickling, silica fibrage body is washed, remove its surperficial acid solution, again dry, pickling acid solution used is according to concentrated hydrochloric acid: volume ratio=1 of concentrated nitric acid: 1 preparation;
3) in vacuum tightness be-vacuum condition of 60KPa under, it is that the BN precursor solution of 40 ℃ floods 2h that the silica fibrage body of again drying is placed in to temperature;
4) after dipping, to silica fibrage body in vacuum tightness be-40KPa, temperature carry out vacuum-drying 3h under the condition of 200 ℃, remove the solvent in silica fibrage body;
5) repeating step 3) to the operation of step 4) 2 times;
6) will gather boron nitrogen silane and pulverize, then mix according to the ratio of mass ratio 3 ︰ 5 with dimethylbenzene, fully stirring and dissolving, preparation obtains poly-boron nitrogen silane precursor liquid solution;
7) in vacuum tightness be-vacuum state of 65KPa under, be 40 ℃ of poly-boron nitrogen silane precursor liquid solutions by the temperature that is placed in step 6) preparation through the silica fibrage body of step 5) processing, dipping time is 1h, then start to vibrate poly-boron nitrogen silane precursor liquid solution 30min, then silica fibrage body is taken out to Air drying 4h;
8) repeating step 7) operation 2 times;
9) by being placed in thermal treatment 2h under 500 ℃ of conditions through the silica fibrage body of step 8) processing, make two kinds of presoma crosslinking curings, realize preliminary cracking;
10) be thermal treatment 1h under 750 ℃ of conditions by being placed in temperature through the silica fibrage body of step 9) processing again, make two kinds of further crosslinking curings of presoma, realize degree of depth Pintsch process, make its half ceramic form crude green body;
11) gained crude green body is machined into desired product size, obtains high temperature resistant nitride based ceramic penetrating wave composite antenna housing cover body.
The high temperature resistant nitride based ceramic penetrating wave composite antenna housing cover body preparing stands to simulate actual working environment examination and without destruction: 1700～1800 ℃ of position, stationary point temperature, 1200～1400 ℃ of big area temperature.Product is as follows with stove sample performance:
Embodiment 4
The high temperature resistant nitride based ceramic penetrating wave composite material and preparation method thereof of certain intermediate range missile high temperature resistant wave-permeable antenna windows, comprises the following steps:
1), according to antenna windows dimensional requirement, knit out satisfactory antenna windows silica fibrage body;
2) silica fibrage body is put into boiling water poach 25h, after oven dry, under 300 ℃ of conditions, lead to oxygen roasting 3h, then it is carried out to cleanup acid treatment, after pickling, silica fibrage body is washed, remove its surperficial acid solution, again dry, pickling acid solution used is according to concentrated hydrochloric acid: volume ratio=3 of concentrated nitric acid: 1 preparation;
3) in vacuum tightness be-vacuum condition of 70KPa under, it is that the BN precursor solution of 55 ℃ floods 2h that the silica fibrage body of again drying is placed in to temperature;
4) after dipping, to silica fibrage body in vacuum tightness be-45KPa, temperature carry out vacuum-drying 4h under the condition of 280 ℃, remove the solvent in silica fibrage body;
5) repeating step 3) to the operation of step 4) 4 times;
6) will gather boron nitrogen silane and pulverize, then mix according to the ratio of mass ratio 6.8 ︰ 10 with dimethylbenzene, fully stirring and dissolving, preparation obtains poly-boron nitrogen silane precursor liquid solution;
7) in vacuum tightness be-vacuum state of 60KPa under, be 60 ℃ of poly-boron nitrogen silane precursor liquid solutions by the temperature that is placed in step 6) preparation through the silica fibrage body of step 5) processing, dipping time is 2h, then start to vibrate poly-boron nitrogen silane precursor liquid solution 55min, then silica fibrage body is taken out to Air drying 5h;
8) repeating step 7) operation 3 times;
9) by being placed in thermal treatment 1h under 650 ℃ of conditions through the silica fibrage body of step 8) processing, make two kinds of presoma crosslinking curings, realize preliminary cracking;
10) be thermal treatment 2h under 850 ℃ of conditions by being placed in temperature through the silica fibrage body of step 9) processing again, make two kinds of further crosslinking curings of presoma, realize degree of depth Pintsch process, make its half ceramic form crude green body;
11) gained crude green body is machined into desired product size, obtains high temperature resistant nitride based ceramic penetrating wave matrix material.
The high temperature resistant nitride based ceramic penetrating wave matrix material antenna windows preparing stands to simulate actual working environment examination and without destruction: 1400～1600 ℃ of big area temperature.Product is as follows with stove sample performance:
Other unspecified part is prior art.Although above-described embodiment has been made detailed description to the present invention; but it is only the present invention's part embodiment; rather than whole embodiment, people can also obtain other embodiment according to the present embodiment under without creative prerequisite, and these embodiment belong to protection domain of the present invention.
Claims (6)
1. a preparation method for high temperature resistant nitride based ceramic penetrating wave composite material forming thing, is characterized in that: comprise the following steps:
1), according to predefined shaped object shape and size, knit out satisfactory silica fibrage body;
2) silica fibrage body is put into boiling water poach 25～45h, after oven dry, under 300～500 ℃ of conditions, lead to oxygen roasting 1～3h, then it is carried out to cleanup acid treatment, after pickling, silica fibrage body is washed, remove its surperficial acid solution, again dry;
3), under vacuum condition, the silica fibrage body of again drying is placed in to BN precursor solution and floods 1～3h;
4) after dipping, silica fibrage body is carried out to vacuum-drying, remove the solvent in silica fibrage body;
5) repeating step 3) to the operation of step 4) 2～4 times;
6) will gather boron nitrogen silane and pulverize, then with dimethylbenzene according to mass ratio 5～6: 10 ratio is mixed, fully stirring and dissolving, preparation obtains gathering boron nitrogen silane precursor liquid solution;
7) under vacuum state, the poly-boron nitrogen silane precursor liquid solution of step 6) preparation will be placed in through the silica fibrage body of step 5) processing, dipping time is 1～3h, then starts to vibrate poly-boron nitrogen silane precursor liquid solution 30～60min, then silica fibrage body is taken out to Air drying;
8) repeating step 7) operation 2～3 times;
9) by being placed in thermal treatment 1～2h under 500～700 ℃ of conditions through the silica fibrage body of step 8) processing, make two kinds of presoma crosslinking curings, realize preliminary cracking;
10) be thermal treatment 1～2h under 750～950 ℃ of conditions by being placed in temperature through the silica fibrage body of step 9) processing again, make two kinds of further crosslinking curings of presoma, realize degree of depth Pintsch process, make its half ceramic form crude green body;
11) gained crude green body is machined into desired product size, obtains high temperature resistant nitride based ceramic penetrating wave composite material forming thing.
2. the preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing according to claim 1, is characterized in that: described step 2) in, pickling acid solution used is according to concentrated hydrochloric acid: volume ratio=1～3 of concentrated nitric acid: 1 preparation.
3. according to the preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing described in claim 1 or 2, it is characterized in that: in described step 3), vacuum tightness is-60～-70KPa; BN precursor solution temperature is 40～60 ℃.
4. according to the preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing described in claim 1 or 2, it is characterized in that: in described step 4), vacuum tightness is-30～-50KPa, and drying temperature is 200～300 ℃, and be 3h～5h time of drying.
5. according to the preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing described in claim 1 or 2, it is characterized in that: in described step 7), vacuum tightness is-60～-70KPa; Poly-boron nitrogen silane precursor solution temperature is 40～60 ℃.
6. according to the preparation method of high temperature resistant nitride based ceramic penetrating wave composite material forming thing described in claim 1 or 2, it is characterized in that: in described step 7), be 4～6h time of drying.
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Cited By (4)
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| CN104910353A (en) * | 2015-06-03 | 2015-09-16 | 东华大学 | Preparation method of high-temperature-resistant epoxy resin adopting polyborosilazane as curing agent |
| CN105198471A (en) * | 2015-11-02 | 2015-12-30 | 湖北三江航天江北机械工程有限公司 | Preparation method of graphene modified ceramic matrix composite material with stealth and wave transmission properties |
| CN104393402B (en) * | 2014-10-31 | 2017-06-27 | 湖北三江航天江北机械工程有限公司 | The manufacture method of miniature and thin-walled composite ceramic wave-transparent antenna house |
| CN110078517A (en) * | 2019-04-11 | 2019-08-02 | 山东工业陶瓷研究设计院有限公司 | A kind of shuffling fiber reinforcement nitride ceramic composites antenna house and preparation method thereof |
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| CN101831178A (en) * | 2010-05-04 | 2010-09-15 | 中国人民解放军国防科学技术大学 | Quartz fiber reinforced composite material and preparation method thereof |
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| CN101591192A (en) * | 2008-11-21 | 2009-12-02 | 中材高新材料股份有限公司 | The Enhancement Method of fibre-quartz ceramic-base composite material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104393402B (en) * | 2014-10-31 | 2017-06-27 | 湖北三江航天江北机械工程有限公司 | The manufacture method of miniature and thin-walled composite ceramic wave-transparent antenna house |
| CN104910353A (en) * | 2015-06-03 | 2015-09-16 | 东华大学 | Preparation method of high-temperature-resistant epoxy resin adopting polyborosilazane as curing agent |
| CN104910353B (en) * | 2015-06-03 | 2017-01-11 | 东华大学 | Preparation method of high-temperature-resistant epoxy resin adopting polyborosilazane as curing agent |
| CN105198471A (en) * | 2015-11-02 | 2015-12-30 | 湖北三江航天江北机械工程有限公司 | Preparation method of graphene modified ceramic matrix composite material with stealth and wave transmission properties |
| CN110078517A (en) * | 2019-04-11 | 2019-08-02 | 山东工业陶瓷研究设计院有限公司 | A kind of shuffling fiber reinforcement nitride ceramic composites antenna house and preparation method thereof |
| CN110078517B (en) * | 2019-04-11 | 2021-12-21 | 山东工业陶瓷研究设计院有限公司 | Mixed-woven fiber reinforced nitride composite material radome and preparation method thereof |
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