CN109023279A - 一种Cu-CrBN纳米复合涂层及其制备方法 - Google Patents

一种Cu-CrBN纳米复合涂层及其制备方法 Download PDF

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CN109023279A
CN109023279A CN201811080532.5A CN201811080532A CN109023279A CN 109023279 A CN109023279 A CN 109023279A CN 201811080532 A CN201811080532 A CN 201811080532A CN 109023279 A CN109023279 A CN 109023279A
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王谦之
周飞
孔继周
孙欣宇
林云根
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Nanjing University of Aeronautics and Astronautics
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    • 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
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Abstract

本发明公开了一种Cu‑CrBN纳米复合涂层及其制备方法，属于表面改性领域，解决了CrBN硬质涂层韧性低，易碎裂的缺点。本发明包括金属Cu掺杂在CrBN涂层中，所述金属Cu以自由态形式存在；利用磁控溅射技术，在Ar和N2混合气氛中，共溅射CrB2靶（直流磁控）和Cu靶（射频磁控）；或在Ar和N2混合气氛中，共溅射Cr靶（直流磁控）、Cu靶（直流磁控）和B靶（射频磁控），在钢基材上制备硬韧兼俱的Cu‑CrBN纳米复合涂层。本发明中Cu‑CrBN涂层的B元素可来源于化合物CrB2靶或单质B靶，对靶位配置数不同的磁控溅射***均适用。

Description

一种Cu-CrBN纳米复合涂层及其制备方法
技术领域
本发明涉及表面改性领域，尤其涉及一种Cu-CrBN纳米复合涂层的制备方法。
背景技术
众所周知，硬度(H)不仅是评价材料抵抗塑性变形能力的重要参数，也是评价材料抗磨损能力的主要力学性能，被普遍认为是决定材料耐磨性的直接指标。因此，硬质涂层(H>20GPa)就成为机械零件表面耐磨材料的首选。CrBN涂层因具有CrN、CrB2纳米晶粒(nc-CrN、nc-CrB2)分布在非晶BN基质(a-BN)中的结构，这种复合结构具有硬化效果，使得CrBN涂层被视为一种能有效增强零件表面耐磨性的硬质涂层材料。然而，CrBN涂层的相关研究表明，硬度更高的CrBN涂层反而表现出更差的耐磨性，因为CrBN涂层的韧性(抵抗裂纹的能力)随着自身硬度的增加反而减弱。在这种情况下，CrBN涂层在磨损过程中主要以裂纹形成、扩展及碎裂的形式发生材料损失。因此，CrBN硬质涂层韧性的提高是保证其良好耐磨性的关键点，而关于改善CrBN硬质涂层韧性的研究还很少。
发明内容
本发明提供了一种Cu-CrBN纳米复合涂层及其制备方法，所述Cu-CrBN纳米复合涂层硬韧兼具，所述制备方法可根据磁控溅射***靶源的配置数，有针对性地选择溅射靶材种类。
为实现以上目的，本发明采用以下技术方案，包括：
一种Cu-CrBN纳米复合涂层，包括金属Cu掺杂在CrBN涂层中，所述金属Cu以自由态形式存在。
一种Cu-CrBN纳米复合涂层的制备方法，包括以下步骤：
(1)基材预处理：将基材精抛钢进行清洗，去除基材表面残留物并活化基材沉积表面；
(2)过渡层制备：保持通入高纯Ar气，在设定的脉冲偏压下，通过直流磁控溅射化合物CrB2靶或者通过直流磁控溅射金属Cr靶，在步骤(1)预处理过的钢基材上沉积一层CrB2或金属Cr过渡层；
(3)Cu-CrBN纳米复合涂层制备：通入高纯Ar和N2气，在设定的脉冲偏压下，通过直流磁控溅射化合物CrB2靶，射频磁控溅射金属Cu靶，在CrB2过渡层上制备Cu-CrBN纳米复合涂层；或者通入高纯Ar和N2气，在设定的脉冲偏压下，通过直流磁控溅射金属Cr、Cu靶，射频磁控溅射非金属B靶，在金属Cr过渡层上制备Cu-CrBN纳米复合涂层。
以上所述步骤中，步骤(2)和步骤(3)中所述的脉冲偏压为-100V，占空比为60％；步骤(2)中所述的过渡层厚度为100～200nm。
步骤(1)基材预处理包括：依次用丙酮、酒精和去离子水对精抛钢基材进行超声清洗，随后装夹在磁控溅射设备的圆形载物台上；当腔体达到高真空后通入高纯Ar气，利用离子束枪离化Ar气，在设定的脉冲偏压下对基材进行加速轰击，去除基材表面残留物并活化基材沉积表面。
步骤(2)中当磁控溅射设备有两靶位时通过直流(DC)阴极溅射金属CrB2靶，在步骤(1)预处理后的基材上沉积CrB2过渡层；当磁控溅射设备有三靶位时通过直流(DC)阴极溅射金属Cr靶，在步骤(1)预处理后的基材上沉积Cr过渡层。
步骤(3)中当磁控溅射设备有两靶位时，通过直流(DC)阴极溅射化合物CrB2靶，射频(RF)阴极溅射金属Cu靶，在步骤(2)所述的CrB2过渡层上制备Cu-CrBN纳米复合涂层；当磁控溅射设备有三靶位时通过直流(DC)阴极溅射金属Cr、Cu靶，射频(RF)阴极溅射非金属B靶，在步骤(2)所述的金属Cr过渡层上制备Cu-CrBN纳米复合涂层。本发明的有益效果：本发明提供了一种Cu-CrBN纳米复合涂层及其制备方法，该制备方法可以根据磁控溅射设备靶源的配置数(两靶或三靶)自由选择B元素的来源，当用Cr、Cu、B三靶溅射时，可以方便地调节Cu-CrBN纳米复合涂层中Cr与B元素的比例；而且可以通过调节金属Cu靶的溅射功率来控制Cu-CrBN纳米复合涂层的化学成分，从而控制涂层的硬度和韧性。采用本发明方法制备的Cu-CrBN纳米复合涂层兼具硬度和韧性，金属Cu的延展性优异，且元素Cu很难与CrBN涂层中的元素Cr、B、N形成化合物，将金属Cu掺杂进入CrBN涂层中，金属Cu多以自由态的形式存在，从而保持其良好的韧性，因此，形成Cu-CrBN纳米复合涂层硬韧兼具。
附图说明
图1是采用实施例1的方法制备的Cu-CrBN纳米复合涂层的表面(a)和截面(b)形貌扫描电子显微镜照片；
图2是采用实施例1的方法制备的Cu-CrBN纳米复合涂层的压痕裂纹分布情况；
图3是采用实施例2的方法制备的Cu-CrBN纳米复合涂层的表面(a)和截面(b)形貌扫描电子显微镜照片；
图4是采用实施例2的方法制备的Cu-CrBN纳米复合涂层的磨痕形貌光学照片；
图5是采用实施例1的方法制备Cu-CrBN耐磨耐蚀涂层的沉积***布局示意图；
图6是采用实施例2的方法制备Cu-CrBN耐磨耐蚀涂层的沉积***布局示意图。
具体实施方式
下面结合附图和实施例对本发明的技术方案进行详细说明：
实施例1
(1)基材预处理
将粗糙度精抛至50nm的45钢(Φ30×6mm2)依次在丙酮，酒精和去离子水中进行超声清洗各10分钟，用电吹风吹干并装夹在物理气相沉积***的载物台上，距离靶材17cm；当物理气相沉积***本底真空度达到7.0×10-4Pa时，通入10sccm的高纯Ar气，设定45钢基材偏压-600V，偏压的占空比为60％，利用离子束源产生的Ar+离子加速轰击45钢表面20分钟，清除基材表面的污染物并活化沉积表面；
(2)过渡层制备
Ar+离子轰击清洗基材后，调节高纯Ar气通入量为5sccm，调节45钢基材偏压至-100V，保持偏压占空比为60％，通过直流(DC)阴极溅射金属CrB2靶10分钟，加载功率为200W，在45钢基材上沉积厚度为100～200nm的CrB2过渡层，增加Cu-CrBN涂层与45钢基材的结合力；
(3)Cu-CrBN纳米复合涂层制备
通入1sccm的N2，调节高纯Ar气通入量为7sccm，通过直流(DC)阴极溅射金属CrB2靶，加载功率为200W，射频(RF)阴极溅射金属Cu靶，加载功率为100W，保持45钢基材偏压-100V，偏压占空比为60％，在室温下运行1小时25分钟，得到Cu-CrBN纳米复合涂层；
(4)薄膜的表征
表面及截面形貌表征：通过扫描电子显微镜(SEM)观察Cu-CrBN纳米复合涂层表面及截面形貌。如图1所示，Cu-CrBN纳米复合涂层呈现柱状生长，柱状晶簇尺寸均匀，整体厚度约2.6μm。
压痕裂纹表征：利用显微硬度仪测量Cu-CrBN纳米复合涂层的压痕裂纹分布。如图2所示，Cu-CrBN纳米复合涂层压痕没有出现放射性裂纹，韧性较好，由压痕面积计算涂层显微硬度约680Hv。
实施例2
(1)基材预处理
将粗糙度精抛至50nm的45钢(Φ30×6mm2)依次在丙酮，酒精和去离子水中进行超声清洗各10分钟，用电吹风吹干并装夹在物理气相沉积***的载物台上，距离靶材17cm；当物理气相沉积***本底真空度达到7.0×10-4Pa时，通入10sccm的高纯Ar气，设定45钢基材偏压-600V，偏压的占空比为60％，利用离子束源产生的Ar+离子加速轰击45钢表面20分钟，清除基材表面的污染物并活化沉积表面；
(2)过渡层制备
Ar+离子轰击清洗基材后，调节高纯Ar气通入量为5sccm，调节45钢基材偏压至-100V，保持偏压占空比为60％，通过直流(DC)阴极溅射金属Cr靶10分钟，加载功率为200W，在45钢基材上沉积厚度为100～200nm的金属Cr过渡层，增加Cu-CrBN涂层与45钢基材的结合力；
(3)Cu-CrBN纳米复合涂层制备
通入1sccm的N2，调节高纯Ar气通入量为7sccm，通过直流(DC)阴极溅射金属Cr，加载功率为200W，金属Cu靶，加载功率为55W，射频(RF)阴极溅射非金属B靶，加载功率为100W，保持45钢基材偏压-100V，偏压占空比为60％，在室温下运行1小时30分钟，得到Cu-CrBN纳米复合涂层；
(4)薄膜的表征
表面及截面形貌表征：通过扫描电子显微镜(SEM)观察Cu-CrBN纳米复合涂层表面及截面形貌。如图3所示，Cu-CrBN纳米复合涂层呈现柱状生长，柱状晶簇尺寸均匀，整体厚度约2.5μm,。
磨痕形貌表征：利用XJZ-6型金相显微镜观察Cu-CrBN纳米复合涂层磨痕形貌。如图4所示，磨痕光滑且没有脆裂的现象，说明制备的Cu-CrBN纳米复合涂层具有良好的硬度和韧性。
本发明溅射靶材种类选择很多，以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以作出若干改进，这些改进也应视为本发明的保护范围。

Claims (7)

1.一种Cu-CrBN纳米复合涂层，其特征在于，包括金属Cu掺杂在CrBN涂层中，所述金属Cu以自由态形式存在。
2.一种Cu-CrBN纳米复合涂层的制备方法，其特征在于，包括以下步骤：
(1)基材预处理：将基材精抛钢进行清洗，去除基材表面残留物并活化基材沉积表面；
(2)过渡层制备：保持通入高纯Ar气，在设定的脉冲偏压下，通过直流磁控溅射化合物CrB2靶或者通过直流磁控溅射金属Cr靶，在步骤(1)预处理过的钢基材上沉积一层CrB2或金属Cr过渡层；
(3) Cu-CrBN纳米复合涂层制备：通入高纯Ar和N2气，在设定的脉冲偏压下，通过直流磁控溅射化合物CrB2靶，射频磁控溅射金属Cu靶，在CrB2过渡层上制备Cu-CrBN纳米复合涂层；或者通入高纯Ar和N2气，在设定的脉冲偏压下，通过直流磁控溅射金属Cr、Cu靶，射频磁控溅射非金属B靶，在金属Cr过渡层上制备Cu-CrBN纳米复合涂层。
3.根据权利要求2所述Cu-CrBN纳米复合涂层的制备方法，其特征在于，步骤(2)中当磁控溅射设备有两靶位时通过直流阴极溅射金属CrB2靶，在步骤(1)预处理后的基材上沉积CrB2过渡层；当磁控溅射设备有三靶位时通过直流阴极溅射金属Cr靶，在步骤(1)预处理后的基材上沉积Cr过渡层。
4.根据权利要求2所述Cu-CrBN纳米复合涂层的制备方法，其特征在于，步骤(3)中当磁控溅射设备有两靶位时，通过直流阴极溅射化合物CrB2靶，射频阴极溅射金属Cu靶，在步骤(2)所述的CrB2过渡层上制备Cu-CrBN纳米复合涂层；当磁控溅射设备有三靶位时通过直流阴极溅射金属Cr、Cu靶，射频阴极溅射非金属B靶，在步骤(2)所述的金属Cr过渡层上制备Cu-CrBN纳米复合涂层。
5.根据权利要求2所述Cu-CrBN纳米复合涂层的制备方法，其特征在于，步骤(2)和步骤(3)中所述的脉冲偏压为-100V，偏压占空比为60 %。
6.根据权利要求2或3所述Cu-CrBN纳米复合涂层的制备方法，其特征在于，步骤(2)中所述的过渡层厚度为100~200 nm。
7.根据权利要求2所述Cu-CrBN纳米复合涂层的制备方法，其特征在于，步骤(1)基材预处理包括：依次用丙酮、酒精和去离子水对精抛钢基材进行超声清洗，随后装夹在磁控溅射设备的圆形载物台上；当腔体达到高真空后通入高纯Ar气，利用离子束枪离化Ar气，在设定的脉冲偏压下对基材进行加速轰击，去除基材表面残留物并活化基材沉积表面。
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