CN112458399A - 一种TiB2/DLC涂层的制备方法 - Google Patents

一种TiB2/DLC涂层的制备方法 Download PDF

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CN112458399A
CN112458399A CN202011327116.8A CN202011327116A CN112458399A CN 112458399 A CN112458399 A CN 112458399A CN 202011327116 A CN202011327116 A CN 202011327116A CN 112458399 A CN112458399 A CN 112458399A
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彭长明
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Creasian Industrial Shenzhen Co ltd
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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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/067—Borides
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

本发明属于涂层材料制备技术领域，公开了一种TiB2/DLC涂层的制备方法及TiB2掺杂DLC涂层。本发明TiB2/DLC涂层的制备方法包括以下步骤：(1)将基材置于自动化清洗线完成液态清洗；(2)将基材放置于磁控溅射镀膜机内预抽真空；(3)在磁控溅射镀膜机内进行辉光清洗；(4)在磁控溅射镀膜机内进行膜层沉积；(5)冷却出炉；其中，膜层沉积过程中顶层的沉积采用PVD和离子源技术，对向放置线性离子源和TiB2靶材，可利用转架依次沉积层状非晶态DLC和晶态TiB2，形成晶态与非晶态的层状堆叠，如此以TiB2为掺杂元素制备得到的掺杂型DLC涂层内应力较低，同时保留了DLC涂层固有的优点，具有优异的力学性能。

Description

一种TiB2/DLC涂层的制备方法
技术领域
本发明涉及涂层材料制备技术领域，具体是涉及一种TiB2/DLC涂层的制备方法及TiB2掺杂DLC涂层。
背景技术
传统DLC涂层具有许多机械性能方面的优势，例如高硬度、高润滑性、耐摩擦以及抗磨损性能良好。然而，DLC自身的生长机制决定了其单纯DLC薄膜必定含有较大的内应力，很大程度上限制了DLC涂层的应用。目前，研究者采用了很多方法来缓解DLC涂层的应力问题，其中元素的掺杂是最简单易行且有效的方案，掺杂元素涉及金属及非金属(Ti、Cr、W、Si……)。
元素的掺杂确实有效的缓解了DLC涂层内应力大的问题，但是同时也带来了另一个问题，即掺杂后涂层硬度都有了一定程度的降低。这种涂层不再具备DLC涂层高硬度、高润滑性、耐摩擦以及抗磨损性能良好的优点，显然，这是在DLC涂层的应用中所不乐意见到的情况。
发明内容
本发明的目的是为了克服上述背景技术的不足，提供一种TiB2/DLC涂层的制备方法，本发明方法采用PVD和离子源技术，以TiB2为掺杂元素制备得到的掺杂型DLC涂层内应力较低，同时保留了DLC涂层固有的优点，具有优异的力学性能。
为达到本发明的目的，本发明TiB2/DLC涂层的制备方法包括以下步骤：
(1)将基材置于自动化清洗线完成液态清洗；
(2)将基材放置于磁控溅射镀膜机内预抽真空；
(3)在磁控溅射镀膜机内进行辉光清洗；
(4)在磁控溅射镀膜机内进行膜层沉积；
(5)冷却出炉；
其中，所述的膜层沉积的参数如下：
底层：时间为10分钟，真空度为0.3Pa，溅射气体为氩气，氩气的体积流量为400sccm，偏压为100V，占空比为50％，底层采用单一靶材，电流10A～20A；
顶层：时间为60分钟，真空度为0.32Pa，溅射气体为氩气，氩气的体积流量为400sccm，DLC沉积采用线性离子源，离子源气体为Ar 20sccm、C2H2 10sccm，离子源电流为7A，TiB2掺杂采用TiB2靶材，靶材电流为5～10A。
进一步地，所述底层采用的单一靶材为Cr靶或Ti靶。
进一步地，所述顶层沉积过程中线性离子源和TiB2靶材对向放置。
更进一步地，所述顶层沉积过程中依次沉积层状非晶态DLC和晶态TiB2，形成晶态与非晶态的层状堆叠。
进一步地，所述基材为不锈钢或钛合金。
另一方面，本发明还提供了一种TiB2掺杂DLC涂层，所述TiB2掺杂DLC涂层是采用前述TiB2/DLC涂层的制备方法制备得到。
与现有技术相比，本发明的优点如下：
(1)本发明TiB2/DLC涂层的制备方法主要通过PVD溅射技术结合离子源技术实现沉积，其主要特点在于掺杂元素为晶态超硬物质TiB2，炉内对向放置线性离子源和TiB2靶材，在沉积膜层过程中可利用转架依次沉积层状非晶态DLC和晶态TiB2，形成晶态与非晶态的层状堆叠，利用这种结构达到抑制内应力的作用；
(2)本发明中超硬材料TiB2的掺入不会大幅降低涂层整体硬度，所制产品表面硬度高，内应力小，在维持硬度的前提下弥补了内应力过大的不足。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。本发明的附加方面和优点将在下面的描述中部分给出，部分将从下面的描述中变得明显，或通过本发明的实践了解到。应当理解，以下描述仅仅用以解释本发明，并不用于限定本发明。
本文中所用的术语“包含”、“包括”、“具有”、“含有”或其任何其它变形，意在覆盖非排它性的包括。例如，包含所列要素的组合物、步骤、方法、制品或装置不必仅限于那些要素，而是可以包括未明确列出的其它要素或此种组合物、步骤、方法、制品或装置所固有的要素。
此外，本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1
一种TiB2掺杂DLC涂层，其制备方法包括以下步骤：
(1)将不锈钢基材置于自动化清洗线完成液态清洗；
(2)将基材放置于磁控溅射镀膜机内预抽真空；
(3)在磁控溅射镀膜机内进行辉光清洗；
(4)在磁控溅射镀膜机内进行膜层沉积；
(5)冷却出炉；
其中，所述的膜层沉积的参数如下：
底层：时间为10分钟，真空度为0.3Pa，溅射气体为氩气，氩气的体积流量为400sccm，偏压为100V，占空比为50％，底层采用单一靶材Cr靶，电流10A～20A；
顶层：时间为60分钟，真空度为0.32Pa，溅射气体为氩气，氩气的体积流量为400sccm，DLC沉积采用线性离子源，离子源气体为Ar 20sccm、C2H2 10sccm，离子源电流为7A，TiB2掺杂采用TiB2靶材，靶材电流为5～10A，顶层沉积过程中线性离子源和TiB2靶材对向放置，依次沉积层状非晶态DLC和晶态TiB2，形成晶态与非晶态的层状堆叠。这样获得的涂层硬度在3000Hv以上，内应力在0.8GPa左右，如采用单层DLC薄膜，则内应力在2.5GPa以上，这样高的内应力严重限制了涂层的应用。如采用其它材料与DLC进行堆叠，例如纯金属Ti则会引起硬度下降至1000Hv以下。
实施例2
一种TiB2掺杂DLC涂层，其制备方法包括以下步骤：
(1)将钛合金基材置于自动化清洗线完成液态清洗；
(2)将基材放置于磁控溅射镀膜机内预抽真空；
(3)在磁控溅射镀膜机内进行辉光清洗；
(4)在磁控溅射镀膜机内进行膜层沉积；
(5)冷却出炉；
其中，所述的膜层沉积的参数如下：
底层：时间为10分钟，真空度为0.3Pa，溅射气体为氩气，氩气的体积流量为400sccm，偏压为100V，占空比为50％，底层采用单一靶材Ti靶，电流10A～20A；
顶层：时间为60分钟，真空度为0.32Pa，溅射气体为氩气，氩气的体积流量为400sccm，DLC沉积采用线性离子源，离子源气体为Ar 20sccm、C2H2 10sccm，离子源电流为7A，TiB2掺杂采用TiB2靶材，靶材电流为5～10A，顶层沉积过程中线性离子源和TiB2靶材对向放置，依次沉积层状非晶态DLC和晶态TiB2，形成晶态与非晶态的层状堆叠。这样获得的涂层硬度在3000Hv以上，内应力在0.8GPa左右，如采用单层DLC薄膜，则内应力在2.5GPa以上，这样高的内应力严重限制了涂层的应用。如采用其它材料与DLC进行堆叠，例如纯金属Ti则会引起硬度下降至1000Hv以下。
本领域的技术人员容易理解，以上所述仅为本发明的实施例而已，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 (6)

1.一种TiB2/DLC涂层的制备方法，其特征在于，所述TiB2/DLC涂层的制备方法包括以下步骤：
(1)将基材置于自动化清洗线完成液态清洗；
(2)将基材放置于磁控溅射镀膜机内预抽真空；
(3)在磁控溅射镀膜机内进行辉光清洗；
(4)在磁控溅射镀膜机内进行膜层沉积；
(5)冷却出炉；
其中，所述的膜层沉积的参数如下：
底层：时间为10分钟，真空度为0.3Pa，溅射气体为氩气，氩气的体积流量为400sccm，偏压为100V，占空比为50％，底层采用单一靶材，电流10A～20A；
顶层：时间为60分钟，真空度为0.32Pa，溅射气体为氩气，氩气的体积流量为400sccm，DLC沉积采用线性离子源，离子源气体为Ar 20sccm、C2H2 10sccm，离子源电流为7A，TiB2掺杂采用TiB2靶材，靶材电流为5～10A。
2.根据权利要求1所述的TiB2/DLC涂层的制备方法，其特征在于，所述底层采用的单一靶材为Cr靶或Ti靶。
3.根据权利要求1所述的TiB2/DLC涂层的制备方法，其特征在于，所述顶层沉积过程中线性离子源和TiB2靶材对向放置。
4.根据权利要求1所述的TiB2/DLC涂层的制备方法，其特征在于，所述顶层沉积过程中依次沉积层状非晶态DLC和晶态TiB2，形成晶态与非晶态的层状堆叠。
5.根据权利要求1所述的TiB2/DLC涂层的制备方法，其特征在于，所述基材为不锈钢或钛合金。
6.一种TiB2掺杂DLC涂层，其特征在于，所述TiB2掺杂DLC涂层是采用权利要求1-5任一项所述的TiB2/DLC涂层的制备方法制备得到。
CN202011327116.8A 2020-11-24 2020-11-24 一种TiB2/DLC涂层的制备方法 Pending CN112458399A (zh)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106086886A (zh) * 2016-08-10 2016-11-09 广东工业大学 一种自润滑二硼化钛/类金刚石涂层及其制备方法和应用
CN107034440A (zh) * 2017-05-03 2017-08-11 马鞍山市卡迈特液压机械制造有限公司 一种复合类金刚石碳膜及其制备方法
CN111057996A (zh) * 2020-01-03 2020-04-24 创隆实业(深圳)有限公司 一种全固态绝缘透波pvd膜层及其制备方法和应用

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106086886A (zh) * 2016-08-10 2016-11-09 广东工业大学 一种自润滑二硼化钛/类金刚石涂层及其制备方法和应用
CN107034440A (zh) * 2017-05-03 2017-08-11 马鞍山市卡迈特液压机械制造有限公司 一种复合类金刚石碳膜及其制备方法
CN111057996A (zh) * 2020-01-03 2020-04-24 创隆实业(深圳)有限公司 一种全固态绝缘透波pvd膜层及其制备方法和应用

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Application publication date: 20210309