CN101525234A - Preparation method for SiBCN ceramic material - Google Patents
Preparation method for SiBCN ceramic material Download PDFInfo
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- CN101525234A CN101525234A CN200910071768A CN200910071768A CN101525234A CN 101525234 A CN101525234 A CN 101525234A CN 200910071768 A CN200910071768 A CN 200910071768A CN 200910071768 A CN200910071768 A CN 200910071768A CN 101525234 A CN101525234 A CN 101525234A
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Abstract
The invention relates to a preparation method of a SiBCN ceramic material. The invention solves the problems of high manufacturing cost, poor safety, complex operations and low yield in manufacturing the SiBCN ceramic material by an organic precursor method. The method comprises the steps: 1. mixing and carrying out reaction on sodium borohydride, methyl vinyl dichlorosilane, a solvent and tetraethyleneglycol dimethyl ether; 2. adding a nitrogen source for mixed reaction; 3. distilling and drying; 4. ball-milling centrifuging and drying to obtain the SiBCN ceramic material; the inventive method has simple operations, high yield of the SiBCN ceramic material, low cost and good safety; the SiBCN ceramic material manufactured by the invention is excellent in high-temperature performance and good in oxidation resistance.
Description
Technical field
The present invention relates to a kind of preparation method of composite ceramic material.
Background technology
The making method of existing SiBCN stupalith mainly is the organic precursor method, though the organic precursor method is made the high-temperature behavior excellence of the SiBCN stupalith that obtains, good in oxidation resistance, but the organic precursor method also exists following problem: 1, the employed raw material of organic precursor method is poisonous, expensive borane complexes or halogen borine, this has not only increased the cost of manufacture of SiBCN stupalith, also endanger operator's health, poor stability; 2, the reaction process of organic precursor method is very strict to the requirement of experiment condition and test equipment, and reaction process need be carried out in protective atmosphere, and the aminolysis reaction process emits a large amount of heat, must carry out complicated operation under the condition of ice bath; 3, the organic precursor method is made yielding poorly of the SiBCN stupalith obtain, and this has seriously restricted the application in practice of SiBCN stupalith.
Summary of the invention
The present invention makes cost of manufacture height, poor stability, the complicated operation of SiBCN stupalith existence and the problem that yields poorly in order to solve the organic precursor legal system, and a kind of preparation method of SiBCN stupalith is provided.
The preparation method of SiBCN stupalith of the present invention carries out according to following steps: one, by ratio of weight and the number of copies the tetraethyleneglycol dimethyl ether of 20～30 parts sodium borohydride, 30～34 parts methyl ethylene dichlorosilane, 100～200 parts solvent and 20～40 parts is put into the environment of rare gas element, reacted 10～15h under 40～180 ℃ condition; Two, the reaction product of step 1 is carried out vacuum filtration, with the liquid behind the suction filtration and nitrogenous source according to 1～2: 1 volume ratio is mixed the environment of putting into rare gas element, and the conditioned response 10～15h at 40～180 ℃ is cooled to room temperature; Three, the reaction product of step 2 vacuum distilling under 60～90 ℃ condition, distillation obtains the environment that solid matter is put into rare gas element, sintering 1～2h under 1100～1200 ℃ condition; Four, the product of step 3 and deionized water carry out ball milling after mixing according to 1: 40～60 mass ratio, the ball milling time is 28～32h, 's centrifugal 5～15min under the condition of 2000～3000r/min with the liquid behind the ball milling at rotating speed, again the precipitation after centrifugal and deionized water are mixed according to 1: 40～60 mass ratio, at rotating speed centrifugal 5～10min under the condition of 9000～10000r/min, then being deposited under 90～120 ℃ the condition after centrifugal dried, promptly make obtaining the SiBCN stupalith.
The inventive method does not have violent thermopositive reaction in preparation SiBCN stupalith process, reaction temperature and, require low to experimental situation and experiment equipment, simple to operate, and the output of SiBCN stupalith is big, compares the inventive method making with the organic precursor method and obtains the output raising of SiBCN stupalith more than 10%; Method of the present invention is a raw material with sodium borohydride, methyl ethylene dichlorosilane and tetraethyleneglycol dimethyl ether, and nontoxic and cheap, cost of manufacture is low, does not influence operator's health, and security is good; The present invention make obtain under 1200 ℃ of conditions of SiBCN stupalith life-time service not crystallization, do not decompose the antioxidant property excellence.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment SiBCN stupalith carries out according to following steps: one, by ratio of weight and the number of copies the tetraethyleneglycol dimethyl ether of 20～30 parts sodium borohydride, 30～34 parts methyl ethylene dichlorosilane, 100～200 parts solvent and 20～40 parts is put into the environment of rare gas element, reacted 10～15h under 40～180 ℃ condition; Two, the reaction product of step 1 is carried out vacuum filtration, with the liquid behind the suction filtration and nitrogenous source according to 1～2: 1 volume ratio is mixed the environment of putting into rare gas element, and the conditioned response 10～15h at 40～180 ℃ is cooled to room temperature; Three, the reaction product of step 2 vacuum distilling under 60～90 ℃ condition, distillation obtains the environment that solid matter is put into rare gas element, sintering 1～2h under 1100～1200 ℃ condition; Four, the product of step 3 and deionized water carry out ball milling after mixing according to 1: 40～60 mass ratio, the ball milling time is 28～32h, 's centrifugal 5～15min under the condition of 2000～3000r/min with the liquid behind the ball milling at rotating speed, again the precipitation after centrifugal and deionized water are mixed according to 1: 40～60 mass ratio, at rotating speed centrifugal 5～10min under the condition of 9000～10000r/min, then being deposited under 90～120 ℃ the condition after centrifugal dried, promptly make obtaining the SiBCN stupalith.
Embodiment two: what present embodiment and embodiment one were different is that rare gas element is nitrogen or argon gas in the step 1.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is to react under 90～150 ℃ condition in the step 1.Other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment and embodiment three are different be in the step 1 reaction times be 11～14h.Other step and parameter are identical with embodiment three.
Embodiment five: present embodiment and embodiment one, two or four are different is that solvent in the step 1 is hexanaphthene, tetrahydrofuran (THF) or ether.Other step and parameter are identical with embodiment one, two or four.
Embodiment six: present embodiment and embodiment five are different is that nitrogenous source in the step 2 is quadrol, allylamine or benzene methanamine.Other step and parameter are identical with embodiment five.
Embodiment seven: what present embodiment and embodiment one, two, four or six were different is that rare gas element is nitrogen or argon gas in the step 2.Other step and parameter are identical with embodiment one, two, four or six.
Embodiment eight: what present embodiment and embodiment seven were different is in the step 4 liquid behind the suction filtration to be mixed according to 1.5: 1 volume ratio with nitrogenous source.Other step and parameter are identical with embodiment one, two, four or six.
Embodiment nine: present embodiment and concrete enforcement side one, two, four, six or eight are different be in the step 4 ball milling time be 30h.Other step and parameter are identical with embodiment one, two, four, six or eight.
Embodiment ten: what present embodiment and embodiment one were different is to dry under 100～110 ℃ condition in the step 4.Other step and parameter are identical with embodiment one.
Embodiment 11: what present embodiment and embodiment two were different is that rare gas element is an argon gas in the step 1.Other step and parameter are identical with embodiment two.
Embodiment 12: present embodiment and embodiment three are different is that temperature is to react under 100～140 ℃ the condition in the step 1.Other step and parameter are identical with embodiment three.
Embodiment 13: present embodiment and embodiment three are different is that temperature is to react under 120 ℃ the condition in the step 1.Other step and parameter are identical with embodiment three.
Embodiment 14: present embodiment and embodiment three are different is that temperature is to react under 140 ℃ the condition in the step 1.Other step and parameter are identical with embodiment three.
Embodiment 15: present embodiment and embodiment four are different be in the step 1 reaction times be 11h.Other step and parameter are identical with embodiment four.
Embodiment 16: present embodiment and embodiment four are different be in the step 1 reaction times be 13h.Other step and parameter are identical with embodiment four.
Embodiment 17: present embodiment and embodiment four are different be in the step 1 reaction times be 14h.Other step and parameter are identical with embodiment four.
Embodiment 18: present embodiment and embodiment six are different is that nitrogenous source in the step 2 is a quadrol.Other step and parameter are identical with embodiment five.
Embodiment 19: what present embodiment and embodiment nine were different is to dry under 100 ℃ condition in the step 4.Other step and parameter are identical with embodiment nine.
Embodiment 20: what present embodiment and embodiment nine were different is to dry under 110 ℃ condition in the step 4.Other step and parameter are identical with embodiment nine.
Embodiment 21: the preparation method of present embodiment SiBCN stupalith carries out according to following steps: one, by ratio of weight and the number of copies the tetraethyleneglycol dimethyl ether of 25 parts sodium borohydride, 32 parts methyl ethylene dichlorosilane, 100 parts solvent and 20 parts is put into the environment of rare gas element, reacted 13h under 70 ℃ condition; Two, the reaction product of step 1 is carried out vacuum filtration, the liquid behind the suction filtration is mixed the environment of putting into rare gas element with nitrogenous source according to 1: 1 volume ratio, the conditioned response 12h at 120 ℃ is cooled to room temperature; Three, the reaction product of step 2 vacuum distilling under 90 ℃ condition, the remaining solid matter in distillation back is put into the environment of rare gas element, is incubated 2h under 1100 ℃ condition; Four, the product of step 3 and deionized water carry out ball milling after according to 1: 50 mixed, the ball milling time is 30h, 's centrifugal 5～15min under the condition of 2500r/min with the liquid behind the ball milling at rotating speed, again with the precipitation after centrifugal and deionized water mixed according to 1: 50, at rotating speed centrifugal 5～10min under the condition of 10000r/min, then being deposited under 100 ℃ the condition after centrifugal dried, promptly make obtaining the SiBCN stupalith.
Rare gas element in the present embodiment step 1 is nitrogen or argon gas.
Solvent in the present embodiment step 1 is hexanaphthene, tetrahydrofuran (THF) or ether.
Nitrogenous source in the present embodiment step 2 is quadrol, allylamine or benzene methanamine.
Rare gas element in the present embodiment step 2 is nitrogen or argon gas.
Present embodiment make obtain under 1200 ℃ of conditions of SiBCN stupalith life-time service not crystallization, do not decompose the antioxidant property excellence.
Embodiment 22: the preparation method of present embodiment SiBCN stupalith carries out according to following steps: one, by ratio of weight and the number of copies with 29 parts sodium borohydride, 33 parts methyl ethylene dichlorosilane, 150 parts hexanaphthene.Put into the environment of rare gas element with 33 parts tetraethyleneglycol dimethyl ether, under 90 ℃ condition, react 12h; Two, the reaction product of step 1 is carried out vacuum filtration, the liquid behind the suction filtration is mixed the environment of putting into rare gas element with quadrol according to 1.5: 1 volume ratio, the conditioned response 12h at 120 ℃ is cooled to room temperature; Three, the reaction product of step 2 vacuum distilling under 90 ℃ condition, distillation obtains the environment that solid matter is put into rare gas element, dry 2h under 1100 ℃ condition; Four, the product of step 3 and deionized water carry out ball milling after mixing according to 1: 50 mass ratio, the ball milling time is 30h, 's centrifugal 10min under the condition of 2500r/min with the liquid behind the ball milling at rotating speed, again the precipitation after centrifugal and deionized water are mixed according to 1: 40～60 mass ratio, at rotating speed centrifugal 10min under the condition of 10000r/min, then being deposited under 100 ℃ the condition after centrifugal dried, promptly make obtaining the SiBCN stupalith.
Present embodiment make obtain under 1200 ℃ of conditions of SiBCN stupalith life-time service not crystallization, do not decompose the antioxidant property excellence.
Claims (9)
1, the preparation method of SiBCN stupalith, the preparation method who it is characterized in that the SiBCN stupalith carries out according to following steps: one, by ratio of weight and the number of copies the tetraethyleneglycol dimethyl ether of 20～30 parts sodium borohydride, 30～34 parts methyl ethylene dichlorosilane, 100～200 parts solvent and 20～40 parts is put into the environment of rare gas element, reacted 10～15h under 40～180 ℃ condition; Two, the reaction product of step 1 is carried out vacuum filtration, with the liquid behind the suction filtration and nitrogenous source according to 1～2: 1 volume ratio is mixed the environment of putting into rare gas element, and the conditioned response 10～15h at 40～180 ℃ is cooled to room temperature; Three, the reaction product of step 2 vacuum distilling under 60～90 ℃ condition, distillation obtains the environment that solid matter is put into rare gas element, sintering 1～2h under 1100～1200 ℃ condition; Four, the product of step 3 and deionized water carry out ball milling after mixing according to 1: 40～60 mass ratio, the ball milling time is 28～32h, 's centrifugal 5～15min under the condition of 2000～3000r/min with the liquid behind the ball milling at rotating speed, again the precipitation after centrifugal and deionized water are mixed according to 1: 40～60 mass ratio, at rotating speed centrifugal 5～10min under the condition of 9000～10000r/min, then being deposited under 90～120 ℃ the condition after centrifugal dried, promptly make obtaining the SiBCN stupalith.
2, the preparation method of SiBCN stupalith according to claim 1 is characterized in that rare gas element is nitrogen or argon gas in the step 1.
3, the preparation method of SiBCN stupalith according to claim 1 and 2 is characterized in that reacting under 90～150 ℃ condition in the step 1.
4, the preparation method of SiBCN stupalith according to claim 3 is characterized in that the reaction times is 11～14h in the step 1.
5,, it is characterized in that the solvent in the step 1 is hexanaphthene, tetrahydrofuran (THF) or ether according to the preparation method of claim 1,2 or 4 described SiBCN stupaliths.
6, the preparation method of SiBCN stupalith according to claim 5 is characterized in that the nitrogenous source in the step 2 is quadrol, allylamine or benzene methanamine.
7,, it is characterized in that rare gas element is nitrogen or argon gas in the step 2 according to the preparation method of claim 1,2,4 or 6 described SiBCN stupaliths.
8, the preparation method of SiBCN stupalith according to claim 7 is characterized in that in the step 4 liquid behind the suction filtration being mixed according to 1.5: 1 volume ratio with nitrogenous source.
9,, it is characterized in that the ball milling time is 30h in the step 4 according to the preparation method of claim 1,2,4,6 or 8 described SiBCN stupaliths.
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| CN2009100717687A CN101525234B (en) | 2009-04-13 | 2009-04-13 | Preparation method for SiBCN ceramic material |
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| CN2009100717687A CN101525234B (en) | 2009-04-13 | 2009-04-13 | Preparation method for SiBCN ceramic material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817641A (en) * | 2010-04-30 | 2010-09-01 | 北京航空航天大学 | Manufacturing method of SiC-SiBCN nucleated glass |
| CN101870586A (en) * | 2010-07-07 | 2010-10-27 | 哈尔滨工业大学 | Amorphous and nanocrystalline Si-B-C-N ceramic composite material and preparation method thereof |
| CN101693618B (en) * | 2009-10-29 | 2012-05-23 | 哈尔滨工业大学 | Preparation method of SiCN(O)ceramic material |
| CN103755348A (en) * | 2013-11-22 | 2014-04-30 | 天津大学 | Silicon boron carbon nitrogen ceramic and preparation method thereof |
| CN104591741A (en) * | 2015-02-17 | 2015-05-06 | 哈尔滨工业大学 | Method for preparing SiNCB ceramic material |
| CN105218829A (en) * | 2015-09-09 | 2016-01-06 | 西北工业大学 | A kind of can the preparation method of thermopolymerization ceramic precursor containing SiBCN |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100503514C (en) * | 2005-01-05 | 2009-06-24 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of Si-B-C-N amorphous ceramic material for high temperature sensing device |
| CN100491287C (en) * | 2007-09-13 | 2009-05-27 | 中国人民解放军国防科学技术大学 | Method for preparing pyro-ceramic fibre |
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2009
- 2009-04-13 CN CN2009100717687A patent/CN101525234B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101693618B (en) * | 2009-10-29 | 2012-05-23 | 哈尔滨工业大学 | Preparation method of SiCN(O)ceramic material |
| CN101817641A (en) * | 2010-04-30 | 2010-09-01 | 北京航空航天大学 | Manufacturing method of SiC-SiBCN nucleated glass |
| CN101870586A (en) * | 2010-07-07 | 2010-10-27 | 哈尔滨工业大学 | Amorphous and nanocrystalline Si-B-C-N ceramic composite material and preparation method thereof |
| CN103755348A (en) * | 2013-11-22 | 2014-04-30 | 天津大学 | Silicon boron carbon nitrogen ceramic and preparation method thereof |
| CN103755348B (en) * | 2013-11-22 | 2015-08-19 | 天津大学 | Si-B-C-N ceramic and preparation method thereof |
| CN104591741A (en) * | 2015-02-17 | 2015-05-06 | 哈尔滨工业大学 | Method for preparing SiNCB ceramic material |
| CN105218829A (en) * | 2015-09-09 | 2016-01-06 | 西北工业大学 | A kind of can the preparation method of thermopolymerization ceramic precursor containing SiBCN |
| CN105218829B (en) * | 2015-09-09 | 2017-10-13 | 西北工业大学 | It is a kind of containing SiBCN can thermal polymerization ceramic precursor preparation method |
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