CN104211025A - Preparation method of cubic phase aluminum nitride fiber - Google Patents
Preparation method of cubic phase aluminum nitride fiber Download PDFInfo
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- CN104211025A CN104211025A CN201410436264.1A CN201410436264A CN104211025A CN 104211025 A CN104211025 A CN 104211025A CN 201410436264 A CN201410436264 A CN 201410436264A CN 104211025 A CN104211025 A CN 104211025A
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- aluminum nitride
- aluminium nitride
- emission
- cubic phase
- nitride fiber
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000835 fiber Substances 0.000 title abstract description 14
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 150000001540 azides Chemical class 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 29
- 229910017083 AlN Inorganic materials 0.000 claims description 28
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000004411 aluminium Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 229940055858 aluminum chloride anhydrous Drugs 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- TVACALAUIQMRDF-UHFFFAOYSA-N dodecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(O)=O TVACALAUIQMRDF-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- -1 polyoxyethylene Polymers 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000005416 organic matter Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- GMRIOAVKKGNMMV-UHFFFAOYSA-N tetrabutylazanium;azide Chemical compound [N-]=[N+]=[N-].CCCC[N+](CCCC)(CCCC)CCCC GMRIOAVKKGNMMV-UHFFFAOYSA-N 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000018199 S phase Effects 0.000 description 4
- 238000010041 electrostatic spinning Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002538 Polyethylene Glycol 20000 Polymers 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Inorganic Fibers (AREA)
- Cold Cathode And The Manufacture (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a preparation method of a cubic phase aluminum nitride fiber. The method comprises the following steps: preparing a mixed solution of anhydrous aluminum chloride, tetrabutylammonium azide and a template agent; carrying out solvothermal reaction; washing, centrifuging and drying, so as to obtain a reaction product; burning in vacuum or inert atmosphere, so that the attached template agent cracks; and burning in air atmosphere to remove organic matters, so as to obtain the cubic phase aluminum nitride fiber. The cubic phase aluminum nitride fiber is directly prepared by taking azide and an inorganic salt of aluminum as raw materials and an organic matter surfactant as a template by a solvothermal method, so that the technological process is simple and feasible, and the morphology of the cubic phase aluminum nitride fiber can be regulated and controlled by controlling the temperature and time of the solvothermal reaction and adding different template agents.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium nitride fibres, particularly relate to a kind of preparation method of Emission in Cubic aluminium nitride fibres, belong to materials science field.
Background technology
Aluminium nitride has high thermal conductivity, and the thermal expansivity having good electrical insulating property, low specific inductivity and dielectric loss simultaneously, match with silicon, is considered to baseplate material ideal now and electron device package material.Aluminium nitride fibres, with the good characteristic of aluminium nitride material and filamentary material, all has broad application prospects at electronics, metallurgy and space industry.
Aluminium nitride has two kinds of crystalline phases, and one is stablize six side's phases and the steady Emission in Cubic that is situated between.For six side's aluminium nitride fibres of stable phase, its technology of preparing comparative maturity, there is a large amount of reports, having with aluminium powder is the vapour deposition process of raw material, as (P.G. Zhang such as Zhang, K.Y. Wang, S.M. Guo, Large-scale synthesis of AlN nanofibers by direct nitridation of aluminum, Ceramics International 36 (2010) 2209-2213) be raw material with aluminium powder, diameter 50-500 nm has been synthesized in 1300 DEG C under 320-480 MPa nitrogen atmosphere, length-to-diameter ratio is the aluminum nitride nanometer fiber of about 400.(the Yongbing Tang such as Tang, Hongtao Cong, Zuoming Wang, Hui-Ming Cheng, Synthesis of rectangular cross-section AlN nanofibers by chemical vapor deposition, Chemical Physics Letters 416 (2005) 171-175) with aluminium powder and F
2o
3particle is raw material, at NH
3synthesized in 800 DEG C the aluminium nitride fibres that diameter is 10-200 nm under/Ar (2:1) atmosphere.Chen etc. (Hong Chen, Yongge Cao, Xianwei Xiang, Formation of AlNnano-fibers, Journal of Crystal Growth 224 (2001) 187-189) are raw material, NH with aluminium powder
4f and NH
4cl is auxiliary agent, has synthesized diameter and be 70-500 nm, reach the aluminium nitride fibres of 2 mm most under 15 normal atmosphere.Also having with sapphire whisker is template, and then carbothermic method prepares the method for aluminium nitride fibres.As (Y. Sun such as Sun, J.Y. Li, Y. Tan, L. Zhang, Fabrication of aluminum nitride (AlN) hollow fibers by arbothermal reduction and nitridation of electrospun precursor fibers, Journal of Alloys and Compounds 471 (2009) 400-403) be main raw material with aluminum nitrate, nano-alumina fiber is obtained by electrostatic spinning, then be reductive agent with carbon dust, nitrogen is nitrogenous source, nanometer aluminum nitride fiber is obtained by carbothermic method at 1600 DEG C.(the Wang Hongzhi such as Wang Hongzhi, Ding Qiu, Li Yaogang, Zhang Qinghong, electrostatic spinning prepares the method for six side's phase aluminum nitride nanometer fibers in conjunction with ammonia nitrogenize, CN 102584244) disclose a kind of electrostatic spinning prepares six side's phase aluminum nitride nanometer fibers method in conjunction with ammonia nitrogenize, take aluminum nitrate as main raw material, obtain nano-alumina fiber by electrostatic spinning, finally under ammonia atmosphere, obtain nanometer aluminum nitride fiber in 1200-1400 DEG C of insulation 4-9 h.
Relative to the aluminium nitride fibres of six side's phases, Emission in Cubic aluminium nitride fibres because do not have the electric field polarization in (001) direction, and carries out doping vario-property than being easier to, and thus has more wide and more accurate application.But, yet there are no the report prepared about Emission in Cubic aluminium nitride fibres.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Emission in Cubic aluminium nitride fibres.
The preparation method of Emission in Cubic aluminium nitride fibres of the present invention, comprises the following steps:
1) in vacuum glove box, be that 1:9 takes Aluminum chloride anhydrous and azide TBuA by aluminium and nitrogen mol ratio, be dissolved in dimethylbenzene, be stirred to and dissolve completely, the total mass mark of solute in solution is made to be 40% ~ 60%, add the template that molar weight is 2 ~ 5 times of aluminium again, be stirred to and dissolve completely, obtain mixing solutions;
(2) mixing solutions of step (1) is transferred in pyroreaction still, after 240 DEG C ~ 280 DEG C insulation 12 h ~ 24 h, naturally cools to room temperature, take out material in reactor and repeatedly with dimethylbenzene washing and centrifugal, oven dry at 80 DEG C ~ 100 DEG C afterwards;
(3) product after step (2) being dried is 800 DEG C ~ 1000 DEG C calcining 1 h ~ 4 h under vacuum atmosphere or inert gas atmosphere, then take out 500 DEG C in air atmosphere ~ 700 DEG C calcining 1 h ~ 4 h, obtain Emission in Cubic aluminium nitride fibres.
Template described in the present invention is polyoxyethylene glycol, cetyl trimethylammonium bromide, sodium lauryl sulphate, polyether nonionic surfactant or dodecylphosphoric acid monoesters diformazan salt.
Beneficial effect of the present invention is: the present invention is using the inorganic salt of trinitride and aluminium as raw material, using organism tensio-active agent as template, Emission in Cubic aluminium nitride fibres has directly been prepared by solvent-thermal method, technological process simple possible, and by controlling the temperature of solvent thermal reaction, the time template different with interpolation, the pattern of Emission in Cubic aluminium nitride fibres can be regulated and controled.
Accompanying drawing explanation
The XRD figure spectrum of Fig. 1 Emission in Cubic aluminium nitride fibres;
The SEM photo of Fig. 2 Emission in Cubic aluminium nitride fibres.
Embodiment
Below in conjunction with example, the invention will be further described.
Embodiment 1
In vacuum glove box, take 0.01 mol Aluminum chloride anhydrous and 0.09 mol azide TBuA is dissolved in 40g dimethylbenzene, forming solute total mass mark is the solution of 40%, then adds the PEG 20000 of 0.02 mol, be stirred to and dissolve completely, obtain mixing solutions.Be transferred to by mixing solutions in pyroreaction still, 240 DEG C of insulation 24 h, naturally cool to room temperature in an oven.Take out product dimethylbenzene washing in reactor, centrifugal, repeats 3 times, collecting precipitation thing, oven dry at 80 DEG C.By product 800 DEG C of calcining 4 h under vacuum atmosphere of drying, then take out 500 DEG C of calcining 4 h in air atmosphere, obtain Emission in Cubic aluminium nitride fibres.
XRD test result shows, this product is the Emission in Cubic aluminium nitride (see figure 1) of pure phase, and SEM electromicroscopic photograph shows, this product is fibrous material (see figure 2).
Embodiment 2
In vacuum glove box, take 0.01 mol Aluminum chloride anhydrous and 0.09 mol azide TBuA is dissolved in 18g dimethylbenzene, forming solute total mass mark is the solution of 60%, then adds the cetyl trimethylammonium bromide of 0.05 mol, be stirred to and dissolve completely, obtain mixing solutions.Be transferred to by mixing solutions in pyroreaction still, 280 DEG C of insulation 12 h, naturally cool to room temperature in an oven.Take out product dimethylbenzene washing in reactor, centrifugal, repeats 5 times, collecting precipitation thing, oven dry at 100 DEG C.By product 1000 DEG C of calcining 1 h under nitrogen protection of drying, then take out 700 DEG C of calcining 1 h in air atmosphere, obtain Emission in Cubic aluminium nitride fibres.
Embodiment 3
In vacuum glove box, take 0.01 mol Aluminum chloride anhydrous and 0.09 mol azide TBuA is dissolved in 27g dimethylbenzene, forming solute total mass mark is the solution of 50%, then adds the sodium lauryl sulphate of 0.04 mol, be stirred to and dissolve completely, obtain mixing solutions.Be transferred to by mixing solutions in pyroreaction still, 260 DEG C of insulation 18 h, naturally cool to room temperature in an oven.Take out product dimethylbenzene washing in reactor, centrifugal, repeats 4 times, collecting precipitation thing, oven dry at 90 DEG C.By product 900 DEG C of calcining 2 h under vacuum atmosphere of drying, then take out 600 DEG C of calcining 2 h in air atmosphere, obtain Emission in Cubic aluminium nitride fibres.
Claims (2)
1. a preparation method for Emission in Cubic aluminium nitride fibres, is characterized in that comprising the following steps:
(1) in vacuum glove box, be that 1:9 takes Aluminum chloride anhydrous and azide TBuA by aluminium and nitrogen mol ratio, be dissolved in dimethylbenzene, be stirred to and dissolve completely, the total mass mark of solute in solution is made to be 40% ~ 60%, add the template that molar weight is 2 ~ 5 times of aluminium again, be stirred to and dissolve completely, obtain mixing solutions;
(2) mixing solutions of step (1) is transferred in pyroreaction still, after 240 DEG C ~ 280 DEG C insulation 12 h ~ 24 h, naturally cools to room temperature, take out material in reactor and repeatedly with dimethylbenzene washing and centrifugal, oven dry at 80 DEG C ~ 100 DEG C afterwards;
(3) product after step (2) being dried is 800 DEG C ~ 1000 DEG C calcining 1 h ~ 4 h under vacuum atmosphere or inert gas atmosphere, then take out 500 DEG C in air atmosphere ~ 700 DEG C calcining 1 h ~ 4 h, obtain Emission in Cubic aluminium nitride fibres.
2. the preparation method of Emission in Cubic aluminium nitride fibres according to claim 1, is characterized in that: described template is polyoxyethylene glycol, cetyl trimethylammonium bromide, sodium lauryl sulphate, polyether nonionic surfactant or dodecylphosphoric acid monoesters diformazan salt.
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| CN201410436264.1A CN104211025B (en) | 2014-08-29 | 2014-08-29 | A kind of preparation method of Emission in Cubic aluminium nitride fibres |
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| CN201410436264.1A CN104211025B (en) | 2014-08-29 | 2014-08-29 | A kind of preparation method of Emission in Cubic aluminium nitride fibres |
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| CN104211025A true CN104211025A (en) | 2014-12-17 |
| CN104211025B CN104211025B (en) | 2016-01-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112110424A (en) * | 2020-09-23 | 2020-12-22 | 航天特种材料及工艺技术研究所 | Preparation method of superfine aluminum nitride powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01100007A (en) * | 1987-10-12 | 1989-04-18 | Idemitsu Petrochem Co Ltd | Production of aluminum nitride with cubic system |
| CN102502538A (en) * | 2011-11-08 | 2012-06-20 | 中国计量学院 | Method for synthesizing ultrafine aluminum nitride powder at low temperature under assistance of calcium |
| CN103320899A (en) * | 2013-07-01 | 2013-09-25 | 中国计量学院 | Preparation method of nanometer aluminum nitride fiber |
-
2014
- 2014-08-29 CN CN201410436264.1A patent/CN104211025B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01100007A (en) * | 1987-10-12 | 1989-04-18 | Idemitsu Petrochem Co Ltd | Production of aluminum nitride with cubic system |
| CN102502538A (en) * | 2011-11-08 | 2012-06-20 | 中国计量学院 | Method for synthesizing ultrafine aluminum nitride powder at low temperature under assistance of calcium |
| CN103320899A (en) * | 2013-07-01 | 2013-09-25 | 中国计量学院 | Preparation method of nanometer aluminum nitride fiber |
Non-Patent Citations (1)
| Title |
|---|
| 吕惠民等: "低温条件下单晶氮化铝纳米线生长机理的研究", 《物理学报》, vol. 56, no. 5, 31 May 2007 (2007-05-31), pages 2808 - 2812 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112110424A (en) * | 2020-09-23 | 2020-12-22 | 航天特种材料及工艺技术研究所 | Preparation method of superfine aluminum nitride powder |
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