CN108265291A - 一种软质基体表面的碳基涂层及其制备方法 - Google Patents

一种软质基体表面的碳基涂层及其制备方法 Download PDF

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CN108265291A
CN108265291A CN201810089810.7A CN201810089810A CN108265291A CN 108265291 A CN108265291 A CN 108265291A CN 201810089810 A CN201810089810 A CN 201810089810A CN 108265291 A CN108265291 A CN 108265291A
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transition zone
transition
carbon
matrix
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王永欣
孙尚琪
李金龙
鲁侠
曾志翔
王立平
薛群基
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

本发明公开一种软质基体表面的碳基涂层，自基体(1)表面向上依次为过渡层(2)与耐磨层(3)；过渡层(2)由第一过渡层(21)、第二过渡层(22)与第三过渡层(23)组成，并且第一过渡层(21)是位于基体(1)表面的Cr层，第二过渡层(22)是位于第一过渡层(21)表面的CrC层，第三过渡层(23)是位于第二过渡层(22)表面的CrSiC层，耐磨层(3)是位于第三过渡层(23)表面的掺杂Cr元素的非晶碳薄膜层。该碳基涂层在保证硬度及耐磨性的前提下，能够在软质基体上具有优异的摩擦学承载能力，使膜基结合力提升1～3倍，对软质基体起到有效防护作用。

Description

一种软质基体表面的碳基涂层及其制备方法
技术领域
本发明涉及基体表面处理技术领域，尤其涉及一种软质基体表面的碳基涂层及其制备方法。
背景技术
一些常用软质基体，例如软质金属及其合金材质的机械零部件，由于其低硬度等特点，很容易在摩擦等过程中变形、开裂和失效，严重影响设备使用寿命，提高成本。现阶段尽管非晶碳基涂层材料具有优异的减摩抗磨作用，但是非晶碳基涂层与软质基体的硬度、弹性模量、热膨胀系数等匹配性较差，极易因结合不牢而导致剥落失效，从而丧失对工件的保护。
发明内容
本发明提供了一种软质基体表面的碳基涂层，如图1所示，自基体1表面向上依次为过渡层2和耐磨层3。即，过渡层2位于基体1的表面，过渡层由第一过渡层21、第二过渡层22与第三过渡层23组成，其中第一过渡层21位于基体1的表面，第二过渡层22位于第一过渡层21表面，第三过渡层23位于第二过渡层22表面，耐磨层3位于第三过渡层23的表面；
软质基体不限，包括易熔且具有低硬度、低耐磨性和韧性的金属、合金及其化合物，例如铝基材料、铜基材料和不锈钢等材料。
其中，第一过渡层21为铬(Cr)层，以Cr层为第一过渡层的目的在于：Cr为高硬度金属，能够与碳生成稳定结构。使用Cr做过渡，能够与基体进行良好化学键结合，充分缓解非晶碳薄膜与基体间因热膨胀因数不匹配而引起的内应力，提高膜基结合力。
第二过渡层22为碳化铬(CrC)层，以CrC层为第二过渡层的目的在于：通过金属到碳化物的梯度设计，逐渐增加硬度，可以提升薄膜与基体的结合力，尽管该层的摩擦学性能低于非晶碳薄膜，但能够有效缓解界面应力，进而有效提高薄膜的结合力和承载力。作为优选，第二过渡层22中，沿着基体表面向上的方向，CrC含量逐渐升高，形成CrC梯度化过渡层，梯度化过渡层既保持了高硬度、低摩擦，又降低了脆性，而且提高了薄膜承载能力、膜基结合力及磨损抗力。
第三过渡层23为铬硅碳(CrSiC)层，以CrSiC层为第三过渡层的目的在于：CrC碳化物，其体系性能低于非晶碳薄膜，可以有效缓解界面应力，可以有效提高薄膜的承载力。硅与碳的结合能够部分取代碳基网络结构中的C，改变sp2-C/sp3-C的比例，进一步缓解复合涂层内部层间界面应力。同时Si掺杂后会促使涂层内部生成少量非晶碳结构，在表面耐磨层失效后可继续保持润滑和耐磨作用，延长机械零部件使用寿命。作为优选，第三过渡层23中，沿着基体表面向上的方向，Cr元素含量逐渐降低，Si元素含量逐渐升高，形成CrSiC梯度化过渡层。
耐磨层3为掺杂铬元素的非晶碳薄膜层，形成a-C:Cr薄膜，使用a-C:Cr薄膜作为耐磨层的目的在于：非晶碳基涂层材料可兼具自润滑、耐磨损、耐腐蚀特性，尤其是以等离子体增强化学气相沉积法制备的类金刚石薄膜具有高sp2含量，在摩擦剪切力作用下，能够快速形成石墨化转移膜，使基体在乳化液环境中迅速达到稳定低摩擦和低磨损，在少量Cr元素存在情况下可形成纳米晶镶嵌非晶结构，涂层可在保持良好减摩抗磨性能前提下表现出较低的内应力，获得较高的综合摩擦学性能。
本发明提供的基体表面的碳基涂层的有益效果为：在保证掺杂Cr元素的类金刚石薄膜具有良好的硬度和耐磨性的同时，使膜基结合力提升1～3倍，不易失效，并且在一些常用的软质金属及合金材质的零部件上，能够对基体起到有效防护作用，能搞显著提升其摩擦学承载能力，延长使用寿命，降低成本。例如，该涂层可用于铝基合金材质的发动机零部件，提升其耐磨性及摩擦学承载能力，为延长工件使用寿命和增加效益提供潜在可能。
本发明还提供了一种软质金属及合金表面的碳基涂层其制备方法，包括如下步骤：
(1)采用磁控溅射技术，在基体表面制备Cr过渡层，即，通入氩气，磁控溅射铬靶，基体施加偏压，得到过渡层21；
作为优选，通入氩气100～200sccm；
作为优选，铬靶溅射功率为3KW～5KW；
作为优选，基体偏压范围为20V～60V；
(2)采用磁控溅射技术复合等离子体增强化学气相沉积法，在Cr过渡层表面制备CrC过渡层，即，保持氩气流量不变，保持基体偏压不变，磁控溅射铬靶，并且通入乙炔，得到过渡层22；
作为优选，铬靶溅射功率逐渐升高至6KW～8KW；进一步优选，在20～40min以内，铬靶溅射功率逐渐升高至6KW～8KW；
作为优选，乙炔流量逐渐增加至40sccm～60sccm；
(3)采用磁控溅射技术复合等离子体增强化学气相沉积法，在CrC过渡层表面制备CrSiC过渡层，即，保持氩气流量不变，保持基体变压不变，保持乙炔流量不变，磁控溅射铬靶，并且开启硅靶溅射，得到过渡层23；
作为优选，铬靶溅射功率逐渐降低至3KW～5KW；进一步优选，在20～40min以内，铬靶溅射功率逐渐升高至3KW～5KW；
作为优选，硅靶溅射功率逐渐增加至2KW～4KW；
(4)采用磁控溅射技术复合等离子体增强化学气相沉积法，在CrSiC层表面制备铬掺杂非晶碳基耐磨工作层，即，保持氩气流量不变，保持基体变压不变，关闭硅靶电源停止其沉积，降低磁控溅射铬靶功率至1～2KW，增加乙炔流量至80～100sccm，沉积得到耐磨层3。
附图说明
图1是本发明软质金属及合金表面碳基复合涂层的结构示意图；
图2是本发明实施例1制得的碳基复合涂层的形貌图；
图3为本发明实施例1制得的碳基复合涂层的硬度及弹性模量测试结果图；
图4是本发明实施例1与对比实施例1制得的碳基复合涂层的结合力图；
图5是本发明实施例1制得的碳基复合涂层在大气环境中的摩擦曲线；
图6是本发明实施例2与对比实施例2制得的碳基复合涂层的结合力图；
图7是本发明实施例2制得的碳基复合涂层在大气环境中的摩擦曲线。
具体实施方式
下面结合附图实施例对本发明作进一步详细描述，需要说明的是，以下所述实施例和术语旨在便于对本发明的理解，而对其不起任何限定作用。
实施例1：
本实施例中，基体1为铝基合金材质基体，该基体1表面为DLC复合涂层，结构如图1所示，自基体1表面向上依次为过渡层2、耐磨层3。即，过渡层2位于基体1的表面，过渡层2由第一过渡层21、第二过渡层22与第三过渡层23组成，其中第一过渡层21位于基体1的表面，第二过渡层22位于第一过渡层21表面，第三过渡层23位于第二过渡层22表面，耐磨层3位于第三过渡层23的表面。
其中，第一过渡层21为Cr层，第二过渡层22为CrC层，第三过渡层23为CrSiC层，磁控溅射Cr和Si靶，通入乙炔气体，形成CrSiC梯度化过渡层。
该基体表面的碳基涂层的制备方法如下：
(1)将基体进行丙酮、酒精和去离子水超声清洗后，放在磁控溅射腔体内部的样品台上，基体与磁控溅射靶的距离为100mm，对腔体抽真空，抽至4.0×10-5mbar以下；样品台旋转速度为3r/min，在通入纯Ar气0.2Pa的条件下，基体在250V负偏压下刻蚀30min。
(2)制备过渡层2
对腔体通Ar气的流量为150sccm，基体偏压为30V，沉积温度200℃以下，在基体表面进行如下沉积：
首先，溅射铬靶，铬靶功率为4KW，氩气流量150sccm，沉积时间为15min，制备Cr层；
然后，保持氩气流量150sccmb不变，在30min以内，改变Cr靶功率由4KW并逐渐上升至5KW，通入乙炔气体且逐渐增大流量至50sccm；
接着，保持氩气流量150sccm和乙炔流量50sccm不变，在30min以内，改变Cr靶功率由5KW逐渐降低至3KW，开启Si靶溅射将功率由0逐渐上升至3KW，制备CrSiC层。
(3)制备耐磨层3
保持Ar气流量为150sccm，基体偏压为30V，将Cr靶功率降低至2KW，乙炔流量增加至80sccm，在经步骤(2)处理后的过渡层表面沉积Cr掺杂的碳质涂层，沉积时间120分钟。
上述制得的基体表面的碳基涂层的形貌如图2所示，显示薄膜体系厚度约为4.2μm，由基体表面向上依次为过渡层2(21，22，23)以及工作层3。
对比实施例1：
本实施例中，基体1与实施例1中的基体完全相同。
本实施例中，基体表面是Cr掺杂的碳质涂层作为耐磨层，制备方法如下：
该基体表面的碳基涂层的制备方法如下：
(1)将基体进行丙酮、酒精和去离子水超声清洗后，放在磁控溅射腔体内部的样品台上，基体与磁控溅射靶的距离为100mm，对腔体抽真空，抽至4.0×10-5mbar以下；样品台旋转速度为3r/min，在通入纯Ar气0.2Pa的条件下，基体在250V负偏压下刻蚀30min。
(2)制备耐磨层
保持Ar气流量为150sccm，基体偏压为30V，将Cr靶功率提升至2KW，乙炔流量增加至80sccm，在经步骤(2)处理后的过渡层表面沉积Cr掺杂的碳质涂层a-C:Cr，沉积时间120分钟。
对上述实施例1与对比实施例1制得的碳基涂层进行性能测试，结果如下：
硬度及弹性模量测试结果如图3所示，显示该碳基涂层具有良好的硬度。
采用划痕测试仪测试其膜基结合力，结果如图4所示，显示实施例1中制得的Cr/CrC/CrSiC/a-C:Cr复合涂层的膜基结合力约为18N，而对比实施例制得的a-C:Cr涂层的膜基结合力4N。即，与对比实施例1制得的a-C:Cr涂层相比，实施例1中制得的梯度碳质涂层在铝合金表面呈现出了良好的膜基结合。
图5为上述实施例1制得的Cr/CrC/CrSiC/a-C:Cr涂层在大气环境中的摩擦系数测试结果图，显示其摩擦系数为0.11，具有优异的综合摩擦学性能。
实施例2：
本实施例中，基体1为铜基合金材质基体，该基体1表面为DLC复合涂层，结构如图1所示，自基体1表面向上依次为过渡层2、耐磨层3。即，过渡层2位于基体1的表面，过渡层2由第一过渡层21、第二过渡层22与第三过渡层23组成，其中第一过渡层21位于基体1的表面，第二过渡层22位于第一过渡层21表面，第三过渡层23位于第二过渡层22表面，耐磨层3位于第三过渡层23的表面。
其中，第一过渡层21为Cr层，第二过渡层22为CrC层，第三过渡层23为CrSiC层，磁控溅射Cr和Si靶，通入乙炔气体，形成CrSiC梯度化过渡层。
该基体表面的碳基涂层的制备方法如下：
(1)将基体进行丙酮、酒精和去离子水超声清洗后，放在磁控溅射腔体内部的样品台上，基体与磁控溅射靶的距离为100mm，对腔体抽真空，抽至4.0×10-5mbar以下；样品台旋转速度为3r/min，在通入纯Ar气0.2Pa的条件下，基体在250V负偏压下刻蚀30min。
(2)制备过渡层2
对腔体通Ar气的流量为160sccm，基体偏压为35V，沉积温度200℃以下，在基体表面进行如下沉积：
首先，溅射铬靶，铬靶功率为5KW，氩气流量160sccm，沉积时间为15min，制备Cr层；
然后，保持氩气流量160sccmb不变，在30min以内，改变Cr靶功率由5KW并逐渐上升至6KW，通入乙炔气体且逐渐增大流量至60sccm；
接着，保持氩气流量160sccm和乙炔流量60sccm不变，在30min以内，改变Cr靶功率由6KW逐渐降低至4KW，开启Si靶溅射将功率由0逐渐上升至4KW，制备CrSiC层。
(3)制备耐磨层3
保持Ar气流量为160sccm，基体偏压为35V，将Cr靶功率降低至3KW，乙炔流量增加至75sccm，在经步骤(2)处理后的过渡层表面沉积Cr掺杂的碳质涂层，沉积时间120分钟。
对上述制得的碳基涂层进行如下性能测试：
采用划痕测试仪测试其膜基结合力，结果如图6所示，显示其膜基结合力约为7N。
对比实施例2：
本实施例中，基体2与实施例2中的基体完全相同。
本实施例中，基体表面是Cr掺杂的碳质涂层作为耐磨层，制备方法如下：
该基体表面的碳基涂层的制备方法如下：
(1)将基体进行丙酮、酒精和去离子水超声清洗后，放在磁控溅射腔体内部的样品台上，基体与磁控溅射靶的距离为100mm，对腔体抽真空，抽至4.0×10-5mbar以下；样品台旋转速度为3r/min，在通入纯Ar气0.2Pa的条件下，基体在250V负偏压下刻蚀30min。
(2)制备耐磨层
保持Ar气流量为160sccm，基体偏压为35V，将Cr靶功率提升至3KW，乙炔流量增加至75sccm，在经步骤(2)处理后的过渡层表面沉积Cr掺杂的碳质涂层a-C:Cr，沉积时间120分钟。
对上述实施例与对比实施例制得的碳基涂层进行性能测试，结果如下：
采用划痕测试仪测试其膜基结合力，结果如图6所示，显示实施例2中制得的Cr/CrC/CrSiC/a-C:Cr复合涂层的膜基结合力约为7N，而对比实施例制得的a-C:Cr涂层的膜基结合力33N。即，与对比实施例2制得的a-C:Cr涂层相比，实施例2中制得的梯度碳质涂层在铜合金表面呈现出了良好的膜基结合。
图7为上述实施例2制得的Cr/CrC/CrSiC/a-C:Cr涂层在大气环境中的摩擦系数测试结果图，显示其摩擦系数为0.09，具有优异的综合摩擦学性能。
以上所述仅为本发明的说明实施例，在上述说明书的描述中提到的数值及数值范围并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种软质基体表面的碳基涂层，其特征是：自基体(1)表面向上依次为过渡层(2)与耐磨层(3)；
过渡层(2)由第一过渡层(21)、第二过渡层(22)与第三过渡层(23)组成，其中第一过渡层(21)是位于基体(1)表面的Cr层，第二过渡层(22)是位于第一过渡层(21)表面的CrC层，第三过渡层(23)是位于第二过渡层(22)表面的CrSiC层，耐磨层(3)是位于第三过渡层(23)表面的掺杂Cr元素的非晶碳薄膜层。
2.如权利要求1所述的软质基体表面的碳基涂层，其特征是：沿着基体表面向上的方向，第二过渡层(22)中CrC含量逐渐升高，形成CrC梯度化过渡层。
3.如权利要求1所述的软质基体表面的碳基涂层，其特征是：沿着基体表面向上的方向，在第二过渡层(23)中，Cr元素含量逐渐降低，Si元素含量逐渐升高，形成CrSiC梯度化过渡层。
4.如权利要求1所述的软质基体表面的碳基涂层，其特征是：所述的软质基体包括铝基合金材料、铜基合金材料和不锈钢。
5.如权利要求1、2、3或4所述的软质基体表面的碳基涂层的制备方法，其特征是：包括如下步骤：
(1)采用磁控溅射技术，在基体表面制备Cr过渡层，即，通入氩气，磁控溅射铬靶，基体施加偏压，得到过渡层(21)；
(2)采用磁控溅射技术复合等离子体增强化学气相沉积法，在Cr过渡层制备CrC过渡层，即，保持氩气流量不变，保持基体变压不变，磁控溅射铬靶，并且通入乙炔，得到过渡层(22)；
(3)采用磁控溅射技术复合等离子体增强化学气相沉积法，在CrC过渡层表面制备CrSiC过渡层，即，保持氩气流量不变，保持基体变压不变，保持乙炔流量不变，磁控溅射铬靶，同时开启Si靶溅射，得到过渡层(23)；
(4)采用磁控溅射技术复合等离子体增强化学气相沉积法，在CrSiC层表面制备掺杂Cr元素的非晶碳薄膜层，即，保持氩气流量不变，保持基体变压不变，关闭Si靶电源，降低磁控溅射Cr靶功率至1KW～2KW，增加乙炔流量至80sccm～100sccm，沉积得到耐磨层(3)。
6.如权利要求5所述的软质基体表面的碳基涂层的制备方法，其特征是：所述的步骤(1)中，铬靶溅射功率为3KW～5KW；
作为优选，所述的步骤(1)中，基体偏压范围为20V～60V；
作为优选，所述的步骤(1)中，通入氩气100～200sccm。
7.如权利要求5所述的软质基体表面的碳基涂层的制备方法，其特征是：所述的步骤(2)中，铬靶溅射功率逐渐升高至6KW～8KW；
作为优选，在20～40min以内，铬靶溅射功率逐渐升高至6KW～8KW。
8.如权利要求5所述的软质基体表面的碳基涂层的制备方法，其特征是：所述的步骤(2)中，乙炔流量逐渐增加至40sccm～60sccm。
9.如权利要求5所述的软质基体表面的碳基涂层的制备方法，其特征是：所述的步骤(3)中，铬靶溅射功率逐渐降低至3KW～5KW；
作为优选，在20～40min以内，铬靶溅射功率逐渐升高至3KW～5KW。
10.如权利要求5所述的软质基体表面的碳基涂层的制备方法，其特征是：所述的步骤(4)中，硅靶溅射功率逐渐增加至2KW～4KW。
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