CN108456883A - 一种基体表面碳基减摩耐磨薄膜的制备方法 - Google Patents

一种基体表面碳基减摩耐磨薄膜的制备方法 Download PDF

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CN108456883A
CN108456883A CN201710089968.XA CN201710089968A CN108456883A CN 108456883 A CN108456883 A CN 108456883A CN 201710089968 A CN201710089968 A CN 201710089968A CN 108456883 A CN108456883 A CN 108456883A
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王永欣
关晓艳
刘正兵
李金龙
鲁侠
***
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

本发明提供了一种基体表面碳基减摩耐磨薄膜的制备方法。该方法采用磁控溅射和离子束相结合的技术，首先采用磁控溅射技术在清洗后的基体表面依次沉积Cr过渡层和WC支撑层，然后采用阳极离子束沉积类金刚石非晶碳基薄膜层，最后进行退火处理，制得的多层结构薄膜在力学性能和减磨耐磨等方面均获得提升，其硬度为20GPa～25GPa，划痕结合强度大于35N，液压油环境中的摩擦系数小于0.1，液压油环境中的磨损率小于10‑7mm3N‑1m‑1数量级，因此可显著提高轴承与传动件等液压油环境下的液压元件的稳定性和使用寿命，在当代机械工业中具有良好的应用前景。

Description

一种基体表面碳基减摩耐磨薄膜的制备方法
技术领域
本发明涉及液压油环境下要求耐磨性及低摩擦系数轴承与传动件，具体如液压泵、马达、绞车等中间的柱塞、滑靴、配油盘、曲柄连杆等关键摩擦副配件，尤其还涉及一种液压油环境碳基减摩耐磨薄膜的制备方法。
背景技术
高速、高压、频繁启停及变速切换等为轴承与传动件的典型工况特征，对于工业广泛应用的轴承与传动件主要的失效途径并非工况下的开裂、破损等破坏性失效，而是配件长期的相对运动导致的磨损失效。
润滑介质的添加能有效降低摩擦副材料的磨损，而液压油作为常见的润滑介质广泛地应用于相关领域，尤其是液压***。在实际工况的高载荷与循环载荷作用下使轴承与其他传动件等摩擦副零配件频繁启停，使得摩擦副配件瞬间过载及摩擦接触面间的摩擦系数急剧升高，磨损率也将急剧增大，尤其在液压油环境长期作用下磨损的磨粒将在高的剪切应力作用下对工作面带来严重的磨损。同时，长时间服役后的液压油的分子长链会被破坏，导致液压油的粘度降低，润滑效果显著下降。此外，液压油的氧化与添加剂的水解将会使具有轻微的腐蚀特性与摩擦过程产生交互作用并加速磨损。因此对轴承与传动件等液压元件在耐磨减摩及耐腐蚀等方面提出了更高的要求。
类金刚石非晶碳基薄膜具有优异的摩擦学特征，在润滑缺失的干摩擦、润滑不足的半干摩擦及润滑充分的边界润滑条件下均能表现出低摩擦与低磨损特性。同时，在腐蚀性介质中，类金刚石非晶碳基薄膜也体现了优异的耐腐蚀性能。
然而，传统类金刚石非晶碳基薄膜的厚度较薄(一般小于3μm)，致使其优异的减摩耐磨特性难以长时间服役，且承载能力受到严重的制约。同时，传统类金刚石非晶碳基薄膜的界面结构单一，其单层(基底直接沉积类金刚石非晶碳基薄膜)或双层(过渡层+类金刚石非晶碳基薄膜)结构的结合强度低(小于10N)，在高剪切应力作用下难以维持低磨损率，而且单层与双层结构难以有效避免薄膜内因薄膜本征应力引起的孔隙贯穿，液压油对基体的腐蚀作用仍然明显，从而使其服役寿命大大降低。
发明内容
本发明旨在提供一种基体表面碳基减摩耐磨薄膜的制备方法，该碳基减摩耐磨薄膜可在液压油中保持低的摩擦系数与磨损率，使沉积有该碳基减摩耐磨薄膜的摩擦副零配件在液压油环境下实现长时间稳定运转。
为达到上述技术目的，本发明将磁控溅射及阳极离子束技术相结合，采用磁控溅射技术沉积Cr过渡层和WC支撑层，然后采用阳极离子束沉积类金刚石非晶碳基薄膜层，形成多层结构，最后进行退火处理降低薄膜的内应力。多种处理方法的结合使得制备的薄膜在力学性能和减摩耐磨等方面均获得提升。
即，本发明的技术方案为：一种基体表面碳基减摩耐磨薄膜的制备方法，首先采用磁控溅射技术在清洗后的基体表面依次沉积Cr过渡层和WC支撑层，然后采用离子束沉积类金刚石非晶碳基薄膜层，最后进行退火处理。
所述的基体材料不限，包括金属及其合金。所述的基体包括液压元件，即，在液压油环境下要求耐磨性及低摩擦系数的轴承与传动件等，具体如液压泵、马达、绞车等中间的柱塞、滑靴、配油盘、曲柄连杆等关键摩擦副配件。
作为优选，所述的碳基减摩耐磨薄膜的厚度为5μm～10μm。
作为优选，沉积过渡层之前，先对基体表面进行渗氮前处理，能够有效提高基体的硬度并与过渡层在硬度等方面实现梯度过渡，再采用磁控溅射技术制备Cr过渡层和WC支撑层，可实现薄膜的高结合力及高承载。作为进一步优选，基体表面进行渗氮处理后利用氩离子轰击进行清洗处理，然后采用磁控溅射技术制备Cr过渡层和WC支撑层。
作为优选，所述Cr过渡层是采用直流磁控溅射技术在Ar气氛下溅射沉积得到。具体工艺参数优选为：选用金属Cr做靶材，真空腔内气体压力为0.5Pa～2.0Pa；直流磁控溅射电源的电流为1.0A～2.0A；偏压为400V～600V的脉冲偏压。
作为优选，所述WC支撑层是采用直流磁控溅射技术在Ar气氛下溅射沉积得到。具体工艺参数优选为：选用WC做靶材，真空腔内气体压力为0.5Pa～2.0Pa；直流磁控溅射电源的电流为1.0A～2.0A；偏压为400V～600V的脉冲偏压。
作为优选，采用阳极离子束沉积类金刚石工作层，具体工艺参数如下：乙炔气流量为40～100sccm；离子束的电压为800～1200V，偏压为200V～500V的脉冲偏压。
所述的退火处理过程中，退火时的加热温度优选为150℃～250℃，保温时间优选为1h～2h。
与现有技术相比，本发明采用磁控溅射技术与离子束技术相结合，制得多层薄膜结构优化了界面，并且进行退火处理降低了薄膜的内应力，从而使制得的薄膜在力学性能和减磨耐磨等方面均获得提升，其硬度为20GPa～25GPa，划痕结合强度(Lc1)大于35N，液压油环境中的摩擦系数小于0.1，液压油环境中的磨损率小于10-7mm3N-1m-1数量级，因此可显著提高轴承与传动件等液压油环境下的液压元件的稳定性和使用寿命，在当代机械工业中具有良好的应用前景。
附图说明
图1是实施例1中制得的多层碳基薄膜的截面形貌图；
图2是实施例1中制得的多层碳基薄膜在液压油环境下的摩擦系数曲线；
图3是实施例1中制得的多层碳基薄膜在摩擦测试后的磨痕形貌图。
具体实施方式
以下结合附图实施例对本发明作进一步详细描述。需要指出的是，以下所述实施例旨在便于对本发明的理解，而不对其起任何限定作用。
实施例1：
本实施例中，基体为38CrMoAl传动杆，在该38CrMoAl传动杆载荷作用面上制备碳基减摩耐磨涂层，具体实施步骤如下：
1)前处理
选用普通洗涤剂处理基体，除去38CrMoAl传动杆上的油污以及吸附的杂质；然后对38CrMoAl传动杆进行渗氮处理，并砂纸打磨除去表面畸变；再采用工业清洗剂超声波清洗38CrMoAl传动杆工作面；最后用去离子水漂洗38CrMoAl传动杆并用干燥的氮气吹干。在该实施例中，渗氮用氨的分解率为15％～30％，加热温度为500℃，保温时间为2h～4h。
2)等离子体清洗
将前处理完毕的38CrMoAl传动杆置于磁控溅射***真空腔内的样品架上，抽真空；待真空腔内气压抽至2.0×10-3Pa时，通入Ar气并调节气压至3.0Pa；打开偏压电源，调节偏压电压为1000V，偏压占空比为50％；Ar气在电场作用下被激发为等离子体，对前处理完毕的38CrMoAl传动杆的表面进行刻蚀，刻蚀时间为30min。
3)直流磁控溅射沉积
将Cr靶和WC靶分别安装在磁控溅射设备相应的靶位，并保持真空腔内Ar气的压力为1.0Pa。首先打开Cr靶电源，在经过等离子清洗的38CrMoAl传动杆工作面上沉积0.5μm的金属Cr薄膜。在沉积过程中，设置直流电源的电流为1.5A，在38CrMoAl传动杆上施加的脉冲偏压为400V，偏压占空比为50％。
随后在金属Cr薄膜表面沉积2μm的WC薄膜。在沉积过程中，直流电源电流为2.0A，在38CrMoAl传动杆上施加的脉冲偏压为500V，偏压占空比为50％。
4)阳极离子束沉积
在WC薄膜表面沉积4μm的DLC薄膜。在沉积过程中，离子束电压为1100V，乙炔气流量为80sccm，在38CrMoAl传动杆上施加的脉冲偏压为300V。
5)后处理
将经步骤4)制得的多层碳基薄膜在200℃下保温1h。
上述制得的多层碳基薄膜的截面形貌如图1所示，显示膜基结合良好，并且各层界面结合良好。
对上述制得的多层碳基薄膜进行纳米压痕测试，得到该薄膜的硬度高达21GPa，膜基结合强度为36N。
测试上述制得的多层碳基薄膜在液压油环境，10N载荷下的摩擦磨损性能，测试结果：该薄膜的摩擦系数低于0.1，摩擦系数曲线如图2所示；薄膜的磨损率为3×10-7mm3/Nm；在摩擦测试后的薄膜表面的磨痕形貌如图3所示，显示薄膜表面磨痕窄且较浅，呈现较低的磨损率和良好的耐磨损性能。
以上所述的实施例对本发明的技术方案进行了详细说明，应理解的是以上所述仅为本发明的具体实施例，并不用于限制本发明，凡在本发明的原则范围内所做的任何修改、补充或类似方式替代等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种基体表面碳基减摩耐磨薄膜的制备方法，其特征是：首先采用磁控溅射技术在清洗后的基体表面依次沉积Cr过渡层和WC支撑层，然后采用阳极离子束沉积类金刚石非晶碳基薄膜层，最后进行退火处理。
2.如权利要求1所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：沉积过渡层之前，先对基体表面进行渗氮前处理。
3.如权利要求1所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：基体表面进行渗氮处理后利用氩离子气体轰击进行清洗处理，然后采用磁控溅射技术制备Cr过渡层和WC支撑层。
4.如权利要求1所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：所述Cr过渡层是采用直流磁控溅射技术在Ar气氛下溅射沉积得到；
作为优选，所述Cr过渡层的沉积条件为：选用金属Cr做靶材，真空腔内气体压力为0.5Pa～2.0Pa；直流磁控溅射电源的电流为1.0A～2.0A；偏压为400V～600V的脉冲偏压。
5.如权利要求1所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：所述WC支撑层是采用直流磁控溅射技术在Ar气氛下溅射沉积得到；
作为优选，所述WC支撑层的沉积条件为：选用WC靶材，真空腔内气体压力为0.5Pa～2.0Pa；直流磁控溅射电源的电流为1.0A～2.0A；偏压为400V～600V的脉冲偏压。
6.如权利要求1所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：采用阳极离子束沉积类金刚石薄膜工作层，具体工艺参数如下：离子束的电压为800～1200V，工作气体C2H2流量为40～100sccm，基底偏压为200V～500V的脉冲偏压。
7.如权利要求1所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：所述的退火处理过程中，退火时的加热温度为150℃～250℃，保温时间为1h～2h。
8.如权利要求1至7中任一权利要求所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：所述的基体包括液压元件。
9.如权利要求1至7中任一权利要求所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：所述的碳基减摩耐磨薄膜的厚度为5μm～10μm。
10.如权利要求1至7中任一权利要求所述的基体表面碳基减摩耐磨薄膜的制备方法，其特征是：所述的碳基减摩耐磨薄膜的硬度为20GPa～25GPa，划痕结合强度(Lc1)大于35N，液压油环境中的摩擦系数小于0.1，液压油环境中的磨损率小于10-7mm3N-1m-1数量级。
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