CN105296960A - Preparation method of homogenized boron nitride coating - Google Patents
Preparation method of homogenized boron nitride coating Download PDFInfo
- Publication number
- CN105296960A CN105296960A CN201510711019.1A CN201510711019A CN105296960A CN 105296960 A CN105296960 A CN 105296960A CN 201510711019 A CN201510711019 A CN 201510711019A CN 105296960 A CN105296960 A CN 105296960A
- Authority
- CN
- China
- Prior art keywords
- boron nitride
- gas
- nitride coating
- boron
- coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to a preparation method of a homogenized boron nitride coating. According to the method, boron trichloride (BCl<3>) and ammonia gas (NH<3>) serve as reaction gases and are fed into a reactor, firstly the reaction gases are evenly mixed in a mixing region and then generate surface deposition in a deposition reaction region, finally an obtained sample is subjected to high-temperature heat treatment, and through a scanning tunneling microscope (SEM), Fourier transform infraRed (FT-IR) and X-ray diffraction (XRD) detection, the boron nitride coating which is even in thickness, singular in ingredient and high in degree of crystallinity is obtained. The method can be used for preparing a boron nitride interface in composite and for preparing boron nitride coatings on the surfaces of other samples and can be further used for researching the boron nitride vapor deposition process and mechanism. The method mainly solves the problem that gases are not evenly mixed in the two-component chemical gas phase sedimentary boron nitride process, so that the uniformity of the boron nitride coating is improved, and the coating thickness is better controlled.
Description
Technical field
The present invention relates to a kind of method that chemical vapour deposition technique prepares homogenizing boron nitride coating, particularly relate to the preparation at boron nitride interface in a kind of fiber, fiber braid and matrix material.
Background technology
Boron nitride interface can by generating at matrix material preparation process situ, also first interface can be prepared at fiber surface, again the fiber with boron nitride interface is applied in matrix material as fortifying fibre, adopt which kind of method to produce, this depends on the control of manufacturing condition and the limitation of production unit.At present, the method preparing BN interface has a variety of, mainly comprises liquid phase method (also referred to as dipping-cladding process), chemical Vapor deposition process and carbothermic method.In numerous preparation method, especially more excellent with the interface performance obtained by CVD and stable.The requirement of CVD to equipment is high, and the processing parameter affecting interface performance is more, but the quality of the coating of gained is often higher, is the first-selection of preparation high quality interface material.
Adopt CVD to prepare in boron nitride coating, mainly adopt BX
3+ NH
3double elements system, wherein applying maximum is BCl
3+ NH
3system, but, compared with single component system, under depositing system is in high-temperature low-pressure state, source gas reaction is violent, and gas and vapor permeation is uneven, cause different positions gas concentration different, sedimentation rate is different, then causes the coat-thickness on deposition substrate surface, coated grains size and coating degree of crystallinity different, is unfavorable for that substrate surface generates the boron nitride coating that thickness is even, composition is single, degree of crystallinity is higher.Point out in pertinent literature and patent, chemical gas-phase method is prepared in boron nitride coating process, all adopt directly in the method for flat-temperature zone deposition, double elements gas meets in sedimentary province concurrent biochemical reaction, then in substrate surface cvd nitride boron coating, gained coating is characterized, finds deposition uneven phenomenon.Pointing out in this patent, by first mixing the method deposited again, can effectively address this problem, obtain relatively stable, uniform boron nitride coating.
summary of the invention:
The object of this invention is to provide a kind of method that double elements aerochemistry vapour deposition process prepares boron nitride coating, for addressing the deficiencies of the prior art and deficiency, providing a kind of method preparing uniform coating, especially a kind of employing BX
3+ NH
3system chemical Vapor deposition process prepares the method for boron nitride coating.
Present method is optimized conventional chemical Vapor deposition process, by first mixing the method deposited again, solving the problem that boron nitride coating is uneven, obtaining relatively uniform, that composition is single, crystal property is good boron nitride coating.The present invention's technical scheme used mainly comprises: gas and vapor permeation, chemical vapour deposition and high-temperature heat treatment.
The following technical scheme of concrete employing:
A preparation method for homogenizing boron nitride coating, is characterized in that the concrete steps of the method are:
A. sample to be coated is put into deposition mould sedimentary province; Pass into reactant gases boron trichloride, ammonia; Boron trichloride and ammonia are passed into by two inlet mouths respectively, do not come in contact before entering mould; Gas mixes in isothermal mixing zone; After mixing, gas enters sedimentary province, is 300 ~ 1800 DEG C at depositing temperature, and system pressure is under 1 ~ 300mbar, deposits, and depositing time is 0.5h ~ 20h, finally obtains uniform boron nitride coating at sample surfaces to be coated; Described boron trichloride and the gas flow ratio of ammonia are [NH
3]/[BCl
3]=1:1 ~ 30;
B. after deposition reaction terminates, carry out high-temperature heat treatment to gained boron nitride coating sample, thermal treatment temp is 1200 ~ 2000 DEG C, and the time is 0.5h ~ 5h, obtains hexagonal boron nitride coating.
Carrier gas and diluent gas is also had in above-mentioned reactant gases; Described carrier gas is at least one in nitrogen or argon gas, and this carrier gas and the same inlet mouth of boron trichloride enter mixing zone, and gas flow ratio is [carrier gas]: [BCl
3]=1:1 ~ 120; Described diluent gas is hydrogen, and gas flow ratio is [carrier gas]: [BCl
3]=1:1 ~ 100.
Described chemical Vapor deposition process prepares the method for even boron nitride coating, and wherein the mode that passes into of gas is BCl
3and NH
3two-way is divided into enter reaction mould, BCl
3pass into together with carrier gas, H
2pass into by arbitrary inlet mouth.
The method of even boron nitride coating is prepared in this chemical vapour deposition, can be used for the preparation of the surfaces nitrided boron coating of carbon fiber, ceramic fiber and braided part thereof, also can be used for the preparation at boron nitride interface in matrix material, also can be used for silicon chip, graphite and Al simultaneously
2o
3the preparation of surfaces nitrided boron coating and other double elements aerochemistry vapour deposition.
Use cvd nitride boron coating of the present invention, result shows, by first mixing the method deposited again, the boron nitride coating that thickness is even, structure is single, crystal property is good can be prepared, compared with technology of preparing in the past, have the following advantages: on the one hand, more easily control the thickness of boron nitride coating, make coated component and structure single stable; On the other hand, in course of industrialization, during to large part sample coating boron nitride coating, different positions place top coat can be made evenly; Finally, a kind of method is provided to research sedimentary dynamics.
Accompanying drawing explanation
Fig. 1 is reactor schematic diagram, is mainly divided into mixing zone and sedimentary province.
Fig. 2 and Fig. 3 is the SEM figure of silicon carbide fiber after cvd nitride boron coating in embodiment 1.
Embodiment
Embodiment 1
The first step: shove charge, is positioned over sedimentary province by silicon carbide fiber, and hybrid chamber and reaction chamber are in boiler tube flat-temperature zone simultaneously, vacuumizes check system resistance to air loss.
Second step: emptying intensification, passes into high pure nitrogen, vacuumizes, so circulation five times, residual air in removal system, heats up according to setting program.
3rd step: air inlet, be warming up to setting depositing temperature 800 DEG C, maintain system pressure 20mbar, pass into ammonia 60ml/min from inlet mouth 1, inlet mouth 2 passes into high pure nitrogen 100mlmin and boron trichloride 20ml/min.
4th step: mixed deposit, gas enters flat-temperature zone, first through hybrid chamber mixing, then enters sedimentary province at silicon carbide fiber surface deposition boron nitride 2h.
5th step: thermal treatment, by post-depositional silicon carbide fiber 1300 DEG C of thermal treatment 1h in argon atmosphere.
Scanning tunnel microscope (SEM) test is carried out to the post-depositional silicon carbide fiber of gained in embodiment 1, find that fiber surface deposited the uniform and smooth boron nitride coating of one deck, and the silicon carbide fiber cvd nitride boron coat-thickness being placed in different positions in sedimentary province is basically identical, is about 1um.
Embodiment 2
The first step: shove charge, the graphite cake after cleaning is positioned over sedimentary province, and hybrid chamber and reaction chamber are in boiler tube flat-temperature zone simultaneously, vacuumize check system resistance to air loss.
Second step: emptying intensification, passes into high pure nitrogen, vacuumizes, so circulation five times, residual air in removal system, heats up according to setting program.
3rd step: air inlet, be warming up to setting depositing temperature 1300 DEG C, maintain system pressure 20mbar, pass into ammonia 60ml/min from inlet mouth 1, inlet mouth 2 passes into high pure nitrogen 100mlmin and boron trichloride 20ml/min.
4th step: mixed deposit, gas enters flat-temperature zone, first through hybrid chamber mixing, then enters sedimentary province at graphite cake surface deposition boron nitride 5h.
5th step: thermal treatment, by post-depositional graphite cake 1600 DEG C of thermal treatment 1h in argon atmosphere.
Embodiment 3
The first step: shove charge, is positioned over sedimentary province by needled carbon felt, and hybrid chamber and reaction chamber are in boiler tube flat-temperature zone simultaneously, vacuumizes check system resistance to air loss.
Second step: emptying intensification, passes into high pure nitrogen, vacuumizes, so circulation five times, residual air in removal system, heats up according to setting program.
3rd step: air inlet, be warming up to setting depositing temperature 750 DEG C, maintain system pressure 20mbar, pass into ammonia 60ml/min and hydrogen 100ml/min from inlet mouth 1, inlet mouth 2 passes into high pure nitrogen 100mlmin and boron trifluoride 20ml/min.
4th step: mixed deposit, gas enters flat-temperature zone, first through hybrid chamber mixing, then enters sedimentary province at needle punched blanket felt surface deposition boron nitride 0.5h.
5th step: thermal treatment, by post-depositional needled carbon felt 1400 DEG C of thermal treatment 2h in argon atmosphere.
Claims (2)
1. a preparation method for homogenizing boron nitride coating, is characterized in that the concrete steps of the method are:
A. sample to be coated is put into deposition mould sedimentary province; Pass into reactant gases boron trichloride, ammonia; Boron trichloride and ammonia are passed into by two inlet mouths respectively, do not come in contact before entering mould; Gas mixes in isothermal mixing zone; After mixing, gas enters sedimentary province, is 300 ~ 1800 DEG C at depositing temperature, and system pressure is under 1 ~ 300mbar, deposits, and depositing time is 0.5h ~ 20h, finally obtains uniform boron nitride coating at sample surfaces to be coated; Described boron trichloride and the gas flow ratio of ammonia are [NH
3]/[BCl
3]=1:1 ~ 30;
B. after deposition reaction terminates, carry out high-temperature heat treatment to gained boron nitride coating sample, thermal treatment temp is 1200 ~ 2000 DEG C, and the time is 0.5h ~ 5h, obtains hexagonal boron nitride coating.
2. the preparation method of homogenizing boron nitride coating according to claim 1, is characterized in that also having carrier gas and diluent gas in described reactant gases; Described carrier gas is at least one in nitrogen or argon gas, and this carrier gas and the same inlet mouth of boron trichloride enter mixing zone, and gas flow ratio is [carrier gas]: [BCl
3]=1:1 ~ 120; Described diluent gas is hydrogen, and gas flow ratio is [carrier gas]: [BCl
3]=1:1 ~ 100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510711019.1A CN105296960A (en) | 2015-10-28 | 2015-10-28 | Preparation method of homogenized boron nitride coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510711019.1A CN105296960A (en) | 2015-10-28 | 2015-10-28 | Preparation method of homogenized boron nitride coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105296960A true CN105296960A (en) | 2016-02-03 |
Family
ID=55194758
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510711019.1A Pending CN105296960A (en) | 2015-10-28 | 2015-10-28 | Preparation method of homogenized boron nitride coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105296960A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842767A (en) * | 2016-05-04 | 2016-08-10 | 上海大学 | Equipment for preparing diffractive optical element by adopting microscopic pattern electrode thermal polarization and method thereof |
| CN107058975A (en) * | 2017-01-23 | 2017-08-18 | 上海大学 | Based on parameter region control high throughput chemical gas-phase permeation technique, using and device |
| CN107460447A (en) * | 2017-09-25 | 2017-12-12 | 何军舫 | A kind of production method of the boron nitride plectane with high-flatness |
| CN107863173A (en) * | 2017-11-01 | 2018-03-30 | 中国科学院合肥物质科学研究院 | High energy particle degrader part and preparation method thereof |
| CN108545914A (en) * | 2018-05-18 | 2018-09-18 | 山东国晶新材料有限公司 | A kind of preparation method of the pyrolytic boron nitride coating layer hot bending die for the anti-aliquation solving oxidation |
| CN109234703A (en) * | 2018-11-27 | 2019-01-18 | 湖南顶立科技有限公司 | A kind of gas-phase deposition system |
| CN111363544A (en) * | 2018-12-26 | 2020-07-03 | 中国科学院物理研究所 | Phosphorus-like electron-doped hexagonal boron nitride and preparation method thereof |
| CN115968361A (en) * | 2020-08-21 | 2023-04-14 | 赛峰航空陶瓷技术公司 | Method for depositing a coating on a line in a microwave field |
| CN117089825A (en) * | 2023-06-01 | 2023-11-21 | 无锡松煜科技有限公司 | Plating chamber with uniform fluid distribution and plating method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021533A (en) * | 2010-11-22 | 2011-04-20 | 赵凤鸣 | Chemical vapor deposition technology and vapor deposition furnace for preparing pyrolytic boron nitride (PBN) products |
| CN102796995A (en) * | 2012-08-27 | 2012-11-28 | 北京博宇半导体工艺器皿技术有限公司 | Vapor deposition furnace and method for preparing pyrolytic boron nitride product |
| CN202786419U (en) * | 2012-08-27 | 2013-03-13 | 北京博宇半导体工艺器皿技术有限公司 | Gas phase depositing furnace used for preparing pyrolytic boron nitride products and provided with separated air inlets |
| CN103058697A (en) * | 2012-12-14 | 2013-04-24 | 西北工业大学 | Method for modifying boron nitride interface phase of ceramic matrix composite material |
-
2015
- 2015-10-28 CN CN201510711019.1A patent/CN105296960A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021533A (en) * | 2010-11-22 | 2011-04-20 | 赵凤鸣 | Chemical vapor deposition technology and vapor deposition furnace for preparing pyrolytic boron nitride (PBN) products |
| CN102796995A (en) * | 2012-08-27 | 2012-11-28 | 北京博宇半导体工艺器皿技术有限公司 | Vapor deposition furnace and method for preparing pyrolytic boron nitride product |
| CN202786419U (en) * | 2012-08-27 | 2013-03-13 | 北京博宇半导体工艺器皿技术有限公司 | Gas phase depositing furnace used for preparing pyrolytic boron nitride products and provided with separated air inlets |
| CN103058697A (en) * | 2012-12-14 | 2013-04-24 | 西北工业大学 | Method for modifying boron nitride interface phase of ceramic matrix composite material |
Non-Patent Citations (1)
| Title |
|---|
| YU CHENG ET.AL: "BN coatings prepared by low pressure chemical vapor dedposition using boron trichloride-ammonia-hydrogen-argon mixture gases", 《SURFACE & COATINGS TECHNOLOGY》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842767A (en) * | 2016-05-04 | 2016-08-10 | 上海大学 | Equipment for preparing diffractive optical element by adopting microscopic pattern electrode thermal polarization and method thereof |
| CN105842767B (en) * | 2016-05-04 | 2018-05-01 | 上海大学 | The device and method of diffraction optical element are prepared using micro- pattern electrode thermal poling |
| CN107058975A (en) * | 2017-01-23 | 2017-08-18 | 上海大学 | Based on parameter region control high throughput chemical gas-phase permeation technique, using and device |
| CN107460447A (en) * | 2017-09-25 | 2017-12-12 | 何军舫 | A kind of production method of the boron nitride plectane with high-flatness |
| CN107863173A (en) * | 2017-11-01 | 2018-03-30 | 中国科学院合肥物质科学研究院 | High energy particle degrader part and preparation method thereof |
| CN108545914A (en) * | 2018-05-18 | 2018-09-18 | 山东国晶新材料有限公司 | A kind of preparation method of the pyrolytic boron nitride coating layer hot bending die for the anti-aliquation solving oxidation |
| CN109234703A (en) * | 2018-11-27 | 2019-01-18 | 湖南顶立科技有限公司 | A kind of gas-phase deposition system |
| CN111363544A (en) * | 2018-12-26 | 2020-07-03 | 中国科学院物理研究所 | Phosphorus-like electron-doped hexagonal boron nitride and preparation method thereof |
| CN115968361A (en) * | 2020-08-21 | 2023-04-14 | 赛峰航空陶瓷技术公司 | Method for depositing a coating on a line in a microwave field |
| CN117089825A (en) * | 2023-06-01 | 2023-11-21 | 无锡松煜科技有限公司 | Plating chamber with uniform fluid distribution and plating method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105296960A (en) | Preparation method of homogenized boron nitride coating | |
| Li et al. | Preparation and characterization of boron nitride coatings on carbon fibers from borazine by chemical vapor deposition | |
| CN104030716A (en) | Method for in-situ synthesis of SiC nanowires modified carbon/carbon composite preform by sol-gel method | |
| CN110382735A (en) | Porous body and preparation method | |
| Liu et al. | Preparation of ZrC-SiC composite coatings by chemical vapor deposition and study of co-deposition mechanism | |
| Nyutu et al. | Experimental design in the deposition of BN interface coatings on SiC fibers by chemical vapor deposition | |
| Patibandla et al. | Chemical vapor deposition of boron nitride | |
| CN115584486A (en) | Tantalum carbide coating product and preparation method thereof | |
| CN104611916B (en) | Carbon fiber of appearance deposition SiBCN coating and preparation method thereof | |
| CN110261256B (en) | Method for measuring intrinsic deposition rate of CVD/CVI process precursor | |
| CN102502578B (en) | Chemical vapor synthesis method for growing carbon nanotubes in mode of being attached to wall of pore channel of template | |
| CN105601311B (en) | A kind of highly-textured based composite material of carbon and preparation method | |
| CN108385087A (en) | A method of it is continuous, quick to prepare SiC fiber surface BN coatings | |
| Zeng et al. | Microstructure and deposition mechanism of CVD amorphous boron carbide coatings deposited on SiC substrates at low temperature | |
| JPH05254808A (en) | Preparation of boron nitride | |
| US11932937B2 (en) | Coated product and production method | |
| EP3597621A1 (en) | Method for producing silicon-carbide-based complex | |
| CN114956836A (en) | Preparation method of SiBN/SiBCN composite interface layer on ceramic fiber surface | |
| Moss et al. | Chemical Vapor Deposition of B13C2 from BCl3‐CH4‐H2‐Argon Mixtures | |
| Ye et al. | Investigation on preparing boron nitride by nitriding pure boron at 1200–1550° C | |
| KR20040082529A (en) | Method for Manufacturing Porous Material with Large Specific Surface Area | |
| CN105503270A (en) | Method for preparing SiC coating | |
| Gulden et al. | Ceramic Fiber Coating by Gas‐Phase and Liquid‐Phase Processes | |
| Hao et al. | Cl2 corrosion resistance of SiC coatings with different morphologies | |
| Yang et al. | Preparation of BN Coating on KD-II Silicon Carbide Fiber by Dip-Coating Process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160203 |
|
| WD01 | Invention patent application deemed withdrawn after publication |