CN117888081A - 一种连续式制备碳化硅纳米线增韧碳化硅涂层的方法 - Google Patents
一种连续式制备碳化硅纳米线增韧碳化硅涂层的方法 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 43
- 238000000576 coating method Methods 0.000 title claims abstract description 33
- 239000011248 coating agent Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000151 deposition Methods 0.000 claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 230000008021 deposition Effects 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 13
- 239000002070 nanowire Substances 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- -1 iron ion Chemical class 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920003257 polycarbosilane Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- SICLLPHPVFCNTJ-UHFFFAOYSA-N 1,1,1',1'-tetramethyl-3,3'-spirobi[2h-indene]-5,5'-diol Chemical compound C12=CC(O)=CC=C2C(C)(C)CC11C2=CC(O)=CC=C2C(C)(C)C1 SICLLPHPVFCNTJ-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
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Abstract
本发明公开一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，旨在基于化学气相沉积的方法，对制备碳化硅纳米线增韧碳化硅涂层的方法进行改进，在减少工艺步骤的条件下，制备出理想的碳化硅涂层。
Description
技术领域
本发明涉及一种连续式制备碳化硅纳米线增韧碳化硅涂层的方法。
背景技术
碳基复合材料具有比模量高、强度高、耐高温、抗热震性好等特点，广泛应用于半导体、新能源、航空航天等领域，如各类高温热场部件：MOCVD石墨基座、坩埚、加热器；正负电极材料、燃料电池双极板；飞机刹车盘、制动器、火箭喷管和鼻锥等。但碳基复合材料由于其脆性大，结合力不足，热匹配性不佳，抗热震性差，这极大地限制了其在高温、腐蚀领域的应用。SiC涂层由于具有高耐磨性、优异的抗氧化性以及与碳材料良好的物理化学相容性，被广泛认为是碳基复合材料最理想的涂层之一。然而，SiC涂层在多次热冲击下，在界面处易引起应力集中，在经受高低温交变时涂层在界面处会出现开裂，甚至在恶劣的环境下脱粘，失去其保护作用。因此，十分有必要提高SiC涂层的断裂韧性。
碳化硅涂层工艺是通过化学气相沉积(CVD)的方法将碳化硅材料沉积在基材表面上。在碳化硅涂层工艺中，通常使用硅烷和甲烷等前驱体作为反应气体，在高温下分解生成碳化硅。碳化硅涂层具有高硬度、高熔点和优异的化学稳定性，能够有效保护基材表面免受腐蚀和磨损。SiC纳米线具有优良的物理、化学等性能，在能量存储和结构陶瓷等方面得到广泛应用。其制备方法多种多样，其中化学气相沉积法(CVD)制备SiC纳米线因具有工艺简单、组成可控和重复性好等优点而备受关注。通过在碳材料基底上制备SiC纳米线，而后再在已沉积的碳化硅纳米线上制备碳化硅涂层，所制备出的即为碳化硅纳米线增韧碳化硅涂层。
论文Fabrication and frictional wear property of bamboo-like SiCnanowires reinforced SiC coating采用的是将聚碳硅烷和活性炭溶解在正庚烷中形成均匀的溶液，然后在马弗炉中干燥，以获得由聚碳硅烷和活性炭组成的均匀混合粉末。然后，用硝酸铁-醇溶液均匀地涂覆石墨基体，并置于马弗炉中干燥。第三步，将得到的粉末均匀分成两份，放入两个坩埚中，然后将两个坩埚与石墨基体一起推入管式炉中，制出竹节状SiC纳米线。然后采用化学气相沉积(CVD)技术，三氯甲基硅烷(MTS)，H2，Ar被用作SiC的前驱体沉积SiC涂层，最终得到SiC纳米线增强SiC涂层。
当前在化学气相沉积制备碳化硅纳米线这一工艺环节中，通常需要一道引入铁离子等作为催化位点诱导生长碳化硅纳米线的工序，并不能直接对基底进行纳米线的制备和后续的涂层沉积。
发明内容
为解决以上现有技术存在的问题，本发明提出一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，其是一种气体腐蚀携带铁离子的方式，在进行碳化硅涂层沉积之前，可以以相同的工艺条件进行碳化硅纳米线的生长，减少了一道生产环节，降低制备碳化硅纳米线增强碳化硅涂层的工艺复杂程度，能够有效地提升良品率和缩减工艺环节，降低人工成本。
本发明可通过以下技术方案予以实现：
一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，包括以下步骤：
1)将所用石墨基底超声清洗，并提前放入沉积炉中；
2)升温加热，同时通入氩气作为保护气；
3)打开沉积炉阀门一，让前驱体(MTS)经过阀门一与铁离子负载器(后进入沉积炉中；其中铁离子负载器由不锈钢材料构成，内为中空网状结构；
4)进行碳化硅纳米线的沉积，沉积后关闭阀门一；
5)打开阀门二，在高温底真空下，进行碳化硅涂层沉积。
进一步地，所述石墨基底超声清洗两次，每次5min。
进一步地，所述步骤2)升温加热为：以5℃/min升温速度，开始加热，加热至1200℃。
进一步地，所述步骤4)中沉积为：在1100℃-1500℃，4～12kPa，沉积4～10h。
进一步地，所述步骤5)中沉积为：在1100℃-1500℃，4～12kPa，沉积7～10h。
有益效果
本发明将MTS通过铁离子负载器，使得化学气相沉积的前驱体中携带铁离子，并附着在基底上，得以直接进行碳化硅纳米线的生长。原方案在配制溶液时将会导致溶液原材料的浪费，本方案能够节省这一步的损耗；原方案存在高温还原过程，需要用到高温炉，又会造成能源，与相关反应材料的浪费，本方案只有沉积碳化硅纳米线时采用高温炉，有效节省能耗。
附图说明
图1为本发明的流程示意图；
图2为本发明的装置示意图；MTS储存罐与气体连接路径均采用聚四氟乙烯材料，铁离子负载器为不锈钢材料；
图3为本方案沉积出的碳化硅纳米线示意图。
具体实施方式
以下通过特定的具体实施例说明本发明的实施方式，本领域的技术人员可由本说明书所揭示的内容轻易地了解本发明的其他优点及功效。
如图1，2所示，本发明的一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，首先，将所用石墨基底超声清洗两次，每次5min，并提前放入沉积炉中。随后以5℃每分钟升温速度，开始加热，加热至1200℃，同时通入氩气作为保护气。此时打开阀门1，让前驱体(MTS)经过阀门1与铁离子负载器(通过阀门3、4、5调整所需负载器数量)后进入沉积炉中，此时进行碳化硅纳米线的沉积(沉积炉设备包括加热装置、保护气进气装置、真空装置等未在图中表述)，在1100℃-1500℃，低真空，沉积4～10h后，关闭阀门1，打开阀门2，在1100℃-1500℃，低真空，沉积7～10h条件下进行碳化硅涂层沉积。如图3所示为本发明沉积出的碳化硅纳米线示意图。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，其特征在于，包括以下步骤：
1)将所用石墨基底超声清洗，并放入沉积炉中；
2)升温加热，同时通入氩气作为保护气；
3)打开沉积炉阀门一，让前驱体三氯甲基硅烷经过阀门一与铁离子负载器后进入沉积炉中；
4)进行碳化硅纳米线的沉积，沉积后关闭阀门一；
5)打开阀门二，在高温底真空下，进行碳化硅涂层沉积。
2.根据权利要求1所述的一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，其特征在于，所述石墨基底超声清洗两次，每次5min。
3.根据权利要求1所述的一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，其特征在于，所述步骤2)升温加热为：以5℃/min升温至1200℃。
4.根据权利要求1所述的一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，其特征在于，所述步骤4)中沉积为：在1100℃-1500℃，4～12kPa，沉积4～10h。
5.根据权利要求1所述的一种连续式制备碳化硅纳米线增强碳化硅涂层的方法，其特征在于，所述步骤5)中沉积为：在1100℃-1500℃，4～12kPa，沉积7～10h。
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