CN102167590A - Precursor conversion preparation method of nitride ceramic material - Google Patents
Precursor conversion preparation method of nitride ceramic material Download PDFInfo
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- CN102167590A CN102167590A CN2011100078765A CN201110007876A CN102167590A CN 102167590 A CN102167590 A CN 102167590A CN 2011100078765 A CN2011100078765 A CN 2011100078765A CN 201110007876 A CN201110007876 A CN 201110007876A CN 102167590 A CN102167590 A CN 102167590A
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Abstract
The invention relates to a precursor conversion preparation method of a nitride ceramic material, which comprises the following steps: (1) placing elemento-organic polymer containing basic chemical bond structures of nitride ceramic in a closed pressure vessel, and preserving the temperature at 50-200 DEG C for 2-80 hours in an inert atmosphere of 0.2-10 MPa to carry out crosslinking and curing; and (2) placing the crosslinking and curing product obtained in the step (1) in a pyrolyzer, and preserving the temperature at 600-1100 DEG C for 0.5-2 hours to carry out pyrolysis, thus obtaining the required nitride ceramic. The invention has the advantages of simple operation steps, low preparation temperature and low requirement for equipment; and the prepared nitride ceramic material has adjustable molecular composition and high purity, can be easily molded, and is applicable to the preparation of components with complicated shapes.
Description
Technical field
The present invention relates to a kind of preparation method of nitride ceramics, more particularly, relate to a kind of precusor conversion preparation method of nitride ceramics.
Background technology
Along with the high speed development of science and technology, numerous high-tech areas such as Aeronautics and Astronautics, the energy have all proposed more and more urgent demand to high performance material.Since pottery have excellent high temperature resistant, anti-ly ablate, characteristic such as wear-resistant, high rigidity, and has higher modulus of elasticity and lower density, some ceramic matric composite also has many good function such as solar heat protection, heat insulation, saturating ripple concurrently, therefore, each developed country of the world all regards stupalith to the hi tech and new material of material impact being arranged and give primary study human future as.
For stupalith, its most traditional preparation technology is a sintering process, as hot pressed sintering, reaction sintering etc.But traditional sintering process exists fatal defective.Because most stupaliths have very high fusing point, therefore, required sintering temperature is very high, on the one hand, equipment has been proposed harsh requirement; On the other hand, in the agglomerating process, generally need to add sintering aid, this can have a negative impact to high-temperature behavior and other performances of material.In addition, conventional sintering technology is difficult to realize the moulding of complex shaped components.Therefore, people are conceived to the ceramic material technology of development of new.
The precursor cracking technology is a kind of new ceramic material preparation technology of development in recent years, can be used for preparing ceramic powder, porous ceramics, ceramic fiber, ceramic coating and ceramic matric composite etc.The precursor cracking technology has plurality of advantages, and for example: (1) can be designed the precursor molecule, thereby the composition of split product is controlled; (2) cracking temperature of precursor is lower, can reduce the requirement to equipment, reduces the technology cost; (3) do not need to add sintering aid in the cracking process, thereby can prepare more purified material; (4) easily realize near-net-shape, can prepare the member of complicated shape.
But existing precursor cracking conversion process prepares nitride ceramics, and product often produces defectives such as foaming and cracking.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the above-mentioned defective that prior art exists, and a kind of new nitride ceramics precursor cracking conversion preparation method is provided, and uses this method to prepare nitride ceramics, and product can not produce defectives such as foaming and cracking.
The objective of the invention is to be achieved through the following technical solutions: it may further comprise the steps:
(1) elemento-organic polymer that will contain the basic chemical bonding structure of nitride ceramics places the seal-off pressure container, under preferred 0.3～8.0MPa) inert atmosphere of 0.2～10MPa(and 50～200 ℃ of (preferred 80～120 ℃) temperature, be incubated 2～80 hours (preferred 3～72 hours), until crosslinking curing takes place;
(2) step (1) gained crosslinking curing product is placed pyrolyzer, under 600～1100 ℃ of (preferred 700～1000 ℃) temperature, be incubated 0.5 ~ 2 hour, cracking promptly obtains required nitride ceramics.
The described elemento-organic polymer that contains the basic chemical bonding structure of nitride ceramics can be polysilazane, poly-boron azane or poly-borosilicate azane etc.
Described inert atmosphere is a nitrogen etc.
Step (2), described cracking is preferably carried out in ammonia atmosphere or nitrogen atmosphere, also can be to carry out in continuing vacuum environment.
Compare with the preparation method of existing nitride ceramics, technology of the present invention is simple, and preparation temperature is low, to equipment require low; The nitride ceramics molecular composition of preparing can be regulated, and purity height, and easy-formation are applicable to preparation complex configuration member.
The performance of nitride ceramics of the present invention is as shown in table 1 below.
Description of drawings
Fig. 1 is the XRD figure spectrum that the precursor of the embodiment of the invention 2 preparations transforms boron nitride ceramic material;
Fig. 2 is the XRD figure spectrum that the precursor of the embodiment of the invention 1 preparation transforms silicon nitride ceramic material;
Fig. 3 is the stereoscan photograph of the silicon boron nitrogen stupalith of the embodiment of the invention 3 preparations;
Fig. 4 is the stereoscan photograph of the boron nitride ceramic material of the embodiment of the invention 2 preparations.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) (molecular structure is [SiH with the perhydro polysilazane
2NH]
n ) place the seal-off pressure container, under the inert atmosphere protection of 0.3MPa, be heated to 120 ℃, be incubated 3 hours, until crosslinking curing takes place, obtain white solid;
(2) step (1) gained crosslinking curing product is placed pyrolyzer, be heated to 1000 ℃ in ammonia atmosphere, be incubated 1 hour, cracking obtains required silicon nitride ceramics.
Prepared silicon nitride ceramics does not have defectives such as foaming and cracking.
Embodiment 2
(1) borazine (borazine is the six-ring of B:N=1:1) is placed the seal-off pressure container, under the inert atmosphere protection of 5MPa, be heated to 80 ℃, be incubated 72 hours,, obtain white solid until crosslinking curing takes place.
(2) step (1) gained crosslinking curing product is placed pyrolyzer, be heated to 800 ℃ in nitrogen atmosphere, be incubated 1.5 hours, cracking obtains required boron nitride ceramics.
Prepared boron nitride ceramics does not have defectives such as foaming and cracking.
Embodiment 3
1) (molecular structure is will to gather the borosilicate azane
Place the seal-off pressure container, under the inert atmosphere protection of 8MPa, be heated to 100 ℃, be incubated 12 hours,, obtain white solid until crosslinking curing takes place.
(2) step (1) gained crosslinking curing product is placed pyrolyzer, be heated to 700 ℃ in continuing vacuum environment, be incubated 1.2 hours, cracking obtains required silicon boron nitrogen pottery.
Prepared silicon boron nitrogen pottery does not have defectives such as foaming and cracking.
The performance such as the following table of the nitride ceramics of embodiment 1, embodiment 2, embodiment 3 preparations:
The performance of the nitride ceramics of table 2 embodiment 1,2,3 preparations
Claims (10)
1. the precusor conversion preparation method of a nitride ceramics is characterized in that, may further comprise the steps:
(1) elemento-organic polymer that will contain the basic chemical bonding structure of nitride ceramics places the seal-off pressure container, at 0.2～10MPa inert atmosphere, is incubated 2～80 hours under 50～200 ℃ of temperature, to crosslinking curing takes place;
(2) step (1) gained crosslinking curing product is placed pyrolyzer, under 600～1100 ℃ of temperature, be incubated 0.5 ~ 2 hour, cracking promptly obtains required nitride ceramics.
2. the precusor conversion preparation method of nitride ceramics according to claim 1 is characterized in that, step (1), and inert atmosphere pressure is 0.3～8.0MPa, and the crosslinking curing temperature is 80～120 ℃, and soaking time is 3～72 hours.
3. the precusor conversion preparation method of nitride ceramics as claimed in claim 1 or 2 is characterized in that, step (1), and the described elemento-organic polymer that contains the basic chemical bonding structure of nitride ceramics is polysilazane, poly-boron azane or poly-borosilicate azane.
4. the precusor conversion preparation method of nitride ceramics as claimed in claim 1 or 2 is characterized in that, step (1), and described inert atmosphere is a nitrogen.
5. the precusor conversion preparation method of nitride ceramics as claimed in claim 1 or 2 is characterized in that, step (2), and cracking temperature is 700～1000 ℃.
6. as the precusor conversion preparation method of nitride ceramics as described in the claim 3, it is characterized in that, step (2), cracking temperature is 700～1000 ℃.
7. the precusor conversion preparation method of nitride ceramics as claimed in claim 1 or 2 is characterized in that, step (2), and described cracking is carried out in ammonia atmosphere or nitrogen atmosphere.
8. as the precusor conversion preparation method of nitride ceramics as described in the claim 3, it is characterized in that, step (2), described cracking is carried out in ammonia atmosphere or nitrogen atmosphere.
9. the precusor conversion preparation method of nitride ceramics as claimed in claim 1 or 2 is characterized in that, step (2), and described cracking is carried out in continuing vacuum environment.
10. as the precusor conversion preparation method of nitride ceramics as described in the claim 3, it is characterized in that, step (2), described cracking is carried out in continuing vacuum environment.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265896A (en) * | 2013-05-15 | 2013-08-28 | 天津城市建设学院 | High-temperature-resistant stainless steel connecting technique |
| CN105694049A (en) * | 2016-01-22 | 2016-06-22 | 中国人民解放军国防科学技术大学 | Preparation method of polyborosilazane |
| CN106995947A (en) * | 2017-05-02 | 2017-08-01 | 中国人民解放军国防科学技术大学 | The gradual decarbonization method of nitride fiber |
| CN107740205A (en) * | 2017-10-12 | 2018-02-27 | 中国科学院过程工程研究所 | A kind of compound organic precursor method prepares BN Si3N4The method of complex phase ceramic continuous fiber |
| CN108395256A (en) * | 2018-01-31 | 2018-08-14 | 哈尔滨工业大学 | A kind of preparation method of dense form richness carbon PRECURSOR-DERIVED CERAMICS |
| CN109650901A (en) * | 2019-01-31 | 2019-04-19 | 哈尔滨工业大学 | A kind of BN-Mg2Al4Si5O18Diphase ceramic material, preparation method and ceramic component |
| CN113061040A (en) * | 2021-03-30 | 2021-07-02 | 中国人民解放军军事科学院国防科技创新研究院 | Preparation method of porous boron nitride ceramic |
-
2011
- 2011-01-14 CN CN2011100078765A patent/CN102167590A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 李斌: "氮化物陶瓷基耐烧蚀、透波复合材料及其天线罩的制备与性能研究", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265896A (en) * | 2013-05-15 | 2013-08-28 | 天津城市建设学院 | High-temperature-resistant stainless steel connecting technique |
| CN105694049A (en) * | 2016-01-22 | 2016-06-22 | 中国人民解放军国防科学技术大学 | Preparation method of polyborosilazane |
| CN106995947A (en) * | 2017-05-02 | 2017-08-01 | 中国人民解放军国防科学技术大学 | The gradual decarbonization method of nitride fiber |
| CN106995947B (en) * | 2017-05-02 | 2019-07-12 | 中国人民解放军国防科学技术大学 | The gradual decarbonization method of nitride fiber |
| CN107740205A (en) * | 2017-10-12 | 2018-02-27 | 中国科学院过程工程研究所 | A kind of compound organic precursor method prepares BN Si3N4The method of complex phase ceramic continuous fiber |
| CN107740205B (en) * | 2017-10-12 | 2019-05-03 | 中国科学院过程工程研究所 | A kind of compound organic precursor method preparation BN-Si3N4The method of complex phase ceramic continuous fiber |
| CN108395256A (en) * | 2018-01-31 | 2018-08-14 | 哈尔滨工业大学 | A kind of preparation method of dense form richness carbon PRECURSOR-DERIVED CERAMICS |
| CN109650901A (en) * | 2019-01-31 | 2019-04-19 | 哈尔滨工业大学 | A kind of BN-Mg2Al4Si5O18Diphase ceramic material, preparation method and ceramic component |
| CN113061040A (en) * | 2021-03-30 | 2021-07-02 | 中国人民解放军军事科学院国防科技创新研究院 | Preparation method of porous boron nitride ceramic |
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Application publication date: 20110831 |