CN106835071A - 一种cvd碳化硅材料的制备方法 - Google Patents

一种cvd碳化硅材料的制备方法 Download PDF

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CN106835071A
CN106835071A CN201710049992.0A CN201710049992A CN106835071A CN 106835071 A CN106835071 A CN 106835071A CN 201710049992 A CN201710049992 A CN 201710049992A CN 106835071 A CN106835071 A CN 106835071A
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涂溶
徐青芳
章嵩
张联盟
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Wuhan University of Technology WUT
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C16/22—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
    • C23C16/325—Silicon carbide
    • C—CHEMISTRY; METALLURGY
    • 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
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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
    • C23C16/44—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
    • C23C16/48—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 by irradiation, e.g. photolysis, radiolysis, particle radiation
    • C23C16/481—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 by irradiation, e.g. photolysis, radiolysis, particle radiation by radiant heating of the substrate
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C16/48—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 by irradiation, e.g. photolysis, radiolysis, particle radiation
    • C23C16/483—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 by irradiation, e.g. photolysis, radiolysis, particle radiation using coherent light, UV to IR, e.g. lasers

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Abstract

本发明涉及一种CVD碳化硅材料的制备方法，包含如下步骤：将基板置于冷壁式化学气相沉积腔体中的加热台上，将真空度调至10Pa以下，预热基板，保温。以稀释气Ar将前驱体HMDS带入反应腔体，调节反应腔体压强(Pdep)至400～800Pa；打开激光，照射基板，激光波长为808nm；调节激光功率，使基板温度升(Tdep)至1100～1200℃，沉积薄膜，保温；停止通入HMDS和Ar，关闭激光，抽真空至10Pa以下，并自然冷却至室温。本发明的有益效果是：沉积碳化硅材料的同时，抑制了杂质碳的生成，提高材料的电阻率、击穿电场强度和抗腐蚀等理化性能；电阻率可高于含有杂质碳的碳化硅材料2个数量级。

Description

一种CVD碳化硅材料的制备方法
技术领域
本发明涉及一种高质量CVD碳化硅材料的制备方法，属于化学气相沉积法制备无机材料领域。
背景技术
碳化硅具有高击穿电场强度、高电子迁移率和耐腐蚀等理化性能，因此特别适合应用于制备高温、高频、高压、大功率半导器件，同时还可应用于辐射环境中，是具有广阔应用前景的第三代半导体。
CVD碳化硅材料是指以化学气相沉积法制备的碳化硅块体材料，这种碳化硅材料相比传统烧结和压坯法制备的材料具有如下优点：1)可在较低温度下制备高致密度碳化硅块体材料；2)制备中仅通过前驱体反应合成材料，而不需要烧结助剂，可制成高纯度碳化硅块体材料；3)通过对工艺的控制，可制备指定晶体取向的碳化硅块体材料；4)可涂覆于其它基底材料表面，易制备曲面材料。
化学气相沉积法(CVD)生长碳化硅材料工艺中，为控制材料成分、提高沉积速率，常采用活性高的小分子为前驱体，如SiH4+CH4，或SH4+C3H8，或CH4+SiCl4等，并以H2为稀释气。然而，高活性小分子前驱体和H2均易燃易爆，生产过程安全性差。采用活性低、安全性高的大分子六甲基二硅烷((CH3)3-Si-Si-(CH3)3，HMDS)为前驱体，并以惰性气体Ar为稀释气，可安全高效沉积SiC薄膜。但前驱体HMDS中C/Si原子数量比为3，而碳化硅的C/Si比为1。前驱体中C/Si比高于所沉积材料中的C/Si比，可导致所沉积的碳化硅中含有杂质碳。碳的导电性较高，因此碳化硅材料中存在杂质碳，可显著降低碳化硅材料的击穿电场强度、电阻率、抗弯强度和抗腐蚀能力等理化性能。
发明内容
为克服上述现有技术的不足，本发明提供了一种CVD碳化硅材料的制备方法。采用激光化学气相沉积法，控制大分子前驱体HMDS的反应进程，以惰性气体Ar气为稀释气，通过调节沉积参数，安全高效沉积碳化硅材料的同时，消除材料中的杂质碳。
本发明解决上述技术问题所采用的技术方案是：一种CVD碳化硅材料的制备方法，其特征在于包括以下步骤：
(1)将基板置于冷壁式化学气相沉积腔体中的加热台上，将真空度调至10Pa以下，加热基板，并保温；
(2)以稀释气将前驱体带入反应腔体，调节反应腔体内压强(Pdep)至400～800Pa；
(3)打开激光，照射基板；
(4)调节激光功率，使基板温度(Tdep)升至1100～1200℃沉积薄膜，保温10min；
(5)停止通入稀释气和前驱体，关闭激光，抽真空至10Pa以下，材料自然冷却至室温。
按上述方案，步骤(1)中加热基板温度为600℃，保温时间30min。
按上述方案，步骤(2)采用Ar为稀释气，HMDS为前驱体。
按上述方案，步骤(3)采用的激光波长为808nm。
本发明的有益效果是：安全高效沉积碳化硅材料的同时，抑制了杂质碳的生成，从而提高材料的电阻率、击穿电场强度和抗腐蚀等理化性能。本发明制备的不含杂质碳的碳化硅材料，其电阻率可高于含有杂质碳的碳化硅材料2个数量级。
附图说明
图1为Tdep＝1250℃，其它制备参数与本发明实施例1相同时所沉积的材料，及本发明实施例1所沉积材料的XRD图谱。
图2(a)、(c)为Tdep＝1250℃，其它制备参数与实施例1相同时，所沉积碳化硅材料断面扫描电子显微镜图(SEM)和电子能谱(EDX)；图2(b)、(d)为本发明实施例1所沉积碳化硅材料的断面SEM像和EDX。
图3为Tdep＝1250℃，其它制备参数与实施例1相同时，所沉积的碳化硅材料，和本发明实施例1所制备的碳化硅材料，电阻率随材料温度变化的规律。
具体实施方式
为了更好地理解本发明，下面结合实施例进一步阐述本发明的内容，本发明不仅仅局限于下面的实施例。
实施例1
(1)将基板置于冷壁式化学气相沉积腔体中的加热台上，将腔体内真空度调至10Pa以下，加热基板至600℃，保温30min；
(2)以稀释气Ar将前驱体HMDS带入反应腔体内，调节Pdep至600Pa；
(3)打开激光，照射基板，激光波长为808nm；
(4)调节激光功率，使Tdep升至1200℃，保温10min；
(5)停止通入HMDS和Ar，关闭激光，抽真空至10Pa以下，材料自然冷却至室温。
如图1所示，Tdep＝1250℃，其它制备参数与本发明实施例1相同时所沉积的材料，其XRD图谱既含有SiC衍射峰，还含有单质碳衍射峰，表明材料为碳化硅，并且含单质碳。本发明实施例一所沉积的材料，其XRD谱图中仅出现碳化硅的衍射峰，而不含杂质碳的衍射峰，表明材料为碳化硅，并且不含单质碳。
图2(a)和(b)中，虚线为碳化硅材料与基板界面处，虚线上方为沉积的碳化硅材料。沿图2(a)和(b)中实线，作EDX分析，结果分别如图2(c)和(d)所示。图2(c)显示，沿图2(a)中实线，C原子信号峰顶，对应Si原子信号峰谷，表明材料中有杂质碳生成。图2(d)显示，沿图2(b)中实线，Si原子和C原子的比例保持为1:1，表明薄膜中不含杂质碳。EDX测试结果与XRD测试结果一致。
据报道HMDS分解并沉积为SiC的反应过程如下所示：
步骤一：(CH3)3-Si-Si-(CH3)3→(CH3)3-Si-Si-(CH3)2 ++CH3 -
步骤二：(CH3)3-Si-Si-(CH3)2 ++CH3 -→(CH3)n-Si-H4-n(n＝1～3)+CnHm
步骤三：(CH3)n-Si-H4-n(n＝1～3)→SiC(solid)+CnHm
图2(a)中碳化硅材料含有杂质碳，可能的原因是其沉积温度较高，为1250℃,HMDS反应步骤三中的Si-C键打开，导致形成过多的甲基，沉积到材料中，引起材料碳原子过多，从而形成杂质碳。而实施例1的沉积温度适中，为1200℃，可使HMDS恰好分解，按照步骤三进行，形成不含杂质碳的碳化硅材料。
因为，Tdep＝1200℃时，碳化硅材料不含杂质碳，而Tdep＝1250℃时，碳化硅材料含杂质碳，因此Tdep＝1200℃时所沉积碳化硅材料的电阻率，可高于Tdep＝1250℃时所沉积的碳化硅材料2个数量级。
实施例2
(1)将基板置于冷壁式化学气相沉积腔体中的加热台上，将腔体内真空度调至10Pa以下，加热基板至600℃，保温30min；
(2)以稀释气Ar将前躯体HMDS带入反应腔体，调节Pdep至800Pa；
(3)打开激光，照射基板，激光波长为808nm；
(4)调节激光功率，使Tdep升至1100℃，保温10min；
(5)停止通入HMDS和Ar，关闭激光，抽真空至10Pa以下，材料自然冷却至室温。
实施例3
(1)将基板置于冷壁式化学气相沉积腔体中的加热台上，将腔体内真空度调至10Pa以下，加热基板至600℃，保温30min；
(2)以稀释气Ar将前驱体HMDS带入反应腔体内，调节Pdep至400Pa；
(3)打开激光，照射基板，激光波长为808nm；
(4)调节激光功率，使Tdep升至1150℃，保温10min；
(5)停止通入HMDS和Ar，关闭激光，抽真空至10Pa以下，材料自然冷却至室温。
以上所述的具体实施例，对本发明的目的、技术方案和有益效果进行了进一步的详细说明。对于本领域的技术人员来说，本发明可以有各种修改和变化，凡在本发明的精神和原则内所做的任何修改，等同替换、改进等，均应在本发明的保护范围内。

Claims (3)

1.一种CVD碳化硅材料的制备方法，其特征在于包括以下步骤：
(1)将基板置于冷壁式化学气相沉积腔体中的加热台上，将真空度调至10Pa以下，加热基板，并保温；
(2)以稀释气将前驱体带入反应腔体，调节反应腔体内压强(Pdep)至400～800Pa；
(3)打开激光，激光波长为808nm，照射基板；
(4)调节激光功率，使基板温度(Tdep)升至1100～1200℃沉积薄膜，保温10min；
(5)停止通入稀释气和前驱体，关闭激光，抽真空至10Pa以下，材料自然冷却至室温。
2.根据权利要求1所描述的一种CVD碳化硅材料的制备方法，其特征在于步骤(1)中加热基板温度为600℃，保温时间30min。
3.根据权利要求1所描述的一种CVD碳化硅材料的制备方法，其特征在于步骤(2)采用Ar为稀释气，HMDS为前驱体。
CN201710049992.0A 2017-01-23 2017-01-23 一种cvd碳化硅材料的制备方法 Pending CN106835071A (zh)

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CN113424298A (zh) * 2019-04-18 2021-09-21 韩国东海炭素株式会社 碳化硅材料及其制备方法
CN114150292A (zh) * 2021-12-14 2022-03-08 武汉理工大学 一种抗热震碳化硅纳米多孔涂层材料及其制备方法与应用

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Publication number Priority date Publication date Assignee Title
CN107513698A (zh) * 2017-09-08 2017-12-26 武汉理工大学 一种立方碳化硅涂层的制备方法
CN107513698B (zh) * 2017-09-08 2019-03-08 武汉理工大学 一种立方碳化硅涂层的制备方法
CN113424298A (zh) * 2019-04-18 2021-09-21 韩国东海炭素株式会社 碳化硅材料及其制备方法
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CN110218987A (zh) * 2019-07-24 2019-09-10 合肥百思新材料研究院有限公司 一种冷壁法cvd沉积设备及其工作方法
CN114150292A (zh) * 2021-12-14 2022-03-08 武汉理工大学 一种抗热震碳化硅纳米多孔涂层材料及其制备方法与应用
CN114150292B (zh) * 2021-12-14 2023-03-10 武汉理工大学 一种抗热震碳化硅纳米多孔涂层材料及其制备方法与应用

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