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CN110528003B - 一种涂层的复合制备方法 - Google Patents

一种涂层的复合制备方法 Download PDF

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CN110528003B
CN110528003B CN201810511782.3A CN201810511782A CN110528003B CN 110528003 B CN110528003 B CN 110528003B CN 201810511782 A CN201810511782 A CN 201810511782A CN 110528003 B CN110528003 B CN 110528003B
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李刘合
苗虎
旷小聪
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Beihang University
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/48—Ion implantation
    • 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
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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
    • C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
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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
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    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D

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Abstract

本发明属真空镀膜技术领域，提供一种涂层的复合制备方法。所述复合制备方法涉及化学气相沉积(CVD)、等离子体浸没离子注入沉积(PIII&D)和原子层沉积(ALD)三部分。具体步骤包括：基底表面预处理后装炉，在真空和一定温度条件下，通入气体，在所述基底表面进行PIII&D涂层过程；调整真空和加热温度，依次通入前驱体、冲洗气体、第二前驱体、冲洗气体进行ALD涂层过程；调整加热温度打开偏压，通入两种前驱体的混合气体进行CVD涂层过程；重复所述CVD、PIII&D和ALD过程，依次制备三种技术交替沉积的多层结构。该复合制备方法可克服CVD涂层不够致密易发生扩散失效和ALD涂层沉积效率低的缺陷，获得不同领域内能长时间服役且具有高性能的复合涂层。

Description

一种涂层的复合制备方法
技术领域
本发明属于真空镀膜技术领域，具体涉及一种涂层的复合制备方法。
背景技术
涂层是一种涂敷在物体表面对其起到一定防护作用的薄膜，真空涂层以其超薄、厚度均匀和较高的防护性能等被广泛应用在各个领域。真空涂层的制作方法一般包括化学气相沉积(CVD)、原子层沉积(ALD)和物理气相沉积(PVD)。CVD是涂层制备最常用的方法之一，其沉积速率较快，厚度均匀可控；ALD是一种基于有序、表面自饱和反应的沉积涂层的方法，它可以实现将物质以单原子膜形式一层一层地镀在基底表面。所沉积的涂层致密、连续、均匀且无孔洞，厚度可精确控制，是一种制备高性能涂层的有效方法；PVD用于涂层的制备，所沉积的涂层均匀致密。但是这些方法也存在着比较大的缺陷，CVD技术制备的涂层以柱状晶方式生长，不够致密，在某些比较恶劣环境下出现孔洞，容易发生渗透导致失效；ALD和PVD技术所制备的涂层虽然比较均匀致密，但是其沉积效率低下。
随着我国各类事业的不断进步和人类不断探索与发展，各种部件的功能不断更新，动力需求日益增大，因此对部件的防护涂层提出了更高的要求，使用传统单一的CVD、ALD和PVD涂层制备方法已不能满足新的要求。
发明内容
等离子体浸没离子注入沉积(PIII&D)技术作为PVD技术的一种，可以在被作用表面注入同种或异种元素，不仅能够改变表面能，提高涂层之间的结合力，还可以打断CVD涂层的柱状晶生长模式，起到防止涂层之间相互渗透作用。
本发明针对以上CVD法制备涂层所存在的涂层以柱状晶方式生长不够致密、某些恶劣条件下易形成孔洞而失效以及ALD方法制备涂层沉积效率太低的缺陷，提出了一种涂层的复合制备方法，该复合制备方法结合了CVD、ALD技术各自的优点，同时加入了PIII&D技术，通过三种方法交替沉积来克服单一方法制备涂层所存在的缺陷，制备服役于不同领域具有优良性能且高效的涂层，增加其使用寿命。
本发明提供的一种涂层的复合制备方法，包括如下组成部分：
PIII&D涂层、ALD涂层、n×多层复合涂层(CVD涂层+PIII&D涂层+ALD涂层)。
所述的PIII&D层位于基体-涂层和涂层-涂层之间。
所述的ALD涂层第一层应用于与基体材料结合，以后的每一层都是与其他涂层进行连接。
所述的CVD涂层上面沉积所述的ALD涂层时必须在中间加入PIII&D涂层。
本发明的一种涂层的复合制备方法，相对现有技术具有如下优点和积极效果：
(1)本发明的复合制备方法结合了CVD、ALD和PIII&D技术各自的优点，通过交替沉积工艺可克服单一方法制备涂层的不足之处，可获得沉积效率高、膜基结合力强、相对致密的涂层，从而可提高其性能和使用寿命。
(2)本发明利用CVD、PIII&D和ALD复合制备技术制备涂层的温度和真空度范围重叠，可统一设定一个参数进行不同方法交替沉积，制备操作过程简便，效率高。
附图说明
图1为本发明实施例中一种涂层的复合制备方法结构图。
图中：
1.基体材料；2.CVD涂层；3.PIII&D涂层；4.ALD涂层；5.多层复合涂层
具体实施方式
下面将结合附图和实施例对本发明作进一步的详细说明。
本发明的目的在于获得一种特殊环境条件下性能更高、服役时间更久的涂层。
本发明提供的一种涂层的复合制备方法，如图1所示，包括：基体材料1；CVD涂层2；PIII&D涂层3；ALD涂层4；多层涂层5(CVD涂层+PIII&D涂层+ALD涂层)
基体材料1通过PIII&D技术的作用在其表面或内部形成PIII&D涂层3；然后使用ALD技术在其上面制备一层ALD涂层4；接下来依次使用CVD、PIII&D和ALD技术制备相应涂层形成多层复合涂层5，重复该多层复合涂层5的制备过程直到达到目标厚度为止。
采用本发明的涂层的复合制备方法的工作过程如下：
对基底进行表面预处理后装炉，在真空和一定温度条件下，向真空室通入反应气体，经等离子体发生器生成等离子体后在高偏压作用下进行(PIII&D)涂层过程，在基底表面进行离子注入与沉积；PIII&D沉积完成后关闭反应气体和偏压，调整真空室的真空度和加热温度，经脉冲控制方式依次通入第一前驱体AB、冲洗气体、第二前驱体C、冲洗气体进行(ALD)涂层过程，在所述PIII&D涂层基础上进行原子层沉积。然后调整加热温度打开偏压，通入AB和C的混合气体进行(CVD)涂层过程。最后重复所述CVD、PIII&D和ALD涂层过程，制备CVD、PIII&D和ALD技术交替沉积的多层结构，直到达到目标厚度。

Claims (10)

1.一种涂层的复合制备方法，其特征在于：
结合了CVD、PIII&D和ALD三种涂层制备技术，具体过程为：在真空和一定温度条件下，向真空室通入反应气体，经等离子体发生器生成等离子体后在高偏压作用下进行PIII&D涂层过程，在基底表面进行离子注入与沉积；PIII&D沉积完成后关闭反应气体和偏压，调整真空室的真空度和加热温度，经脉冲控制方式依次通入第一前驱体AB、冲洗气体、第二前驱体C、冲洗气体进行ALD涂层过程，从而在所述PIII&D涂层基础上制备所述ALD涂层；然后调整加热温度打开偏压，通入AB和C的混合气体进行CVD涂层过程；在所述CVD涂层上进行PIII&D涂层过程；再在PIII&D涂层上形成ALD涂层；最后重复CVD、PIII&D和ALD涂层过程，制备CVD、PIII&D和ALD技术交替沉积的多层结构，直到达到目标厚度。
2.根据权利要求1所述的一种涂层的复合制备方法，其特征在于：所述PIII&D涂层沉积过程气压为10-4～100Pa。
3.根据权利要求2所述的一种涂层的复合制备方法，其特征在于：所述PIII&D涂层沉积过程加热温度为23℃～1000℃,上述23℃为常温。
4.根据权利要求3所述的一种涂层的复合制备方法，其特征在于：所述PIII&D涂层沉积过程反应气体为含目标涂层的化合物，其中目标元素为A，化合物为AB，B包括单元素和多种元素。
5.根据权利要求4所述的一种涂层的复合制备方法，其特征在于：所述PIII&D涂层沉积过程偏压大小为-10kV ～-10V。
6.根据权利要求5所述的一种涂层的复合制备方法，其特征在于：所述ALD涂层过程气压为10-3～1kPa。
7.根据权利要求6所述的一种涂层的复合制备方法，其特征在于：所述ALD涂层过程加热温度为23℃～1000℃,上述23℃为常温。
8.根据权利要求7所述的一种涂层的复合制备方法，其特征在于：所述ALD涂层过程冲洗气体为惰性气体。
9.根据权利要求8所述的一种涂层的复合制备方法，其特征在于：所述CVD涂层过程加热温度为23℃～1500℃,上述23℃为常温。
10.根据权利要求9所述的一种涂层的复合制备方法，其特征在于：所述CVD涂层过程偏压为-1000～-10V。
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CN111560602B (zh) * 2020-04-13 2021-10-26 哈尔滨工业大学 一种氧化物薄膜表面复合的优化方法
CN113072063B (zh) * 2020-07-10 2024-01-23 华南理工大学 基于氢储运设备内表面的阻氢涂层及制备方法
CN112725765A (zh) * 2020-12-29 2021-04-30 兰州空间技术物理研究所 一种高致密涂层的复合制备方法

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