CN108456845B - 一种软硬复合纳米多层涂层刀具及其制备方法 - Google Patents

一种软硬复合纳米多层涂层刀具及其制备方法 Download PDF

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CN108456845B
CN108456845B CN201810218285.4A CN201810218285A CN108456845B CN 108456845 B CN108456845 B CN 108456845B CN 201810218285 A CN201810218285 A CN 201810218285A CN 108456845 B CN108456845 B CN 108456845B
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连云崧
穆晨亮
姚斌
卓勇
肖望强
陈汇丰
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Xiamen University
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Abstract

本发明提供了一种软硬复合纳米多层涂层刀具及其制备方法。该刀具基体材料为硬质合金，涂层由下至上依次为Zr过渡层、(ZrN‑CrCN)x周期复合多层纳米硬涂层、WS2软涂层。制备该涂层仅采用N2作为反应气体，其余涂层元素均为固态靶材，有效防止了在沉积不同层的涂层时出现污染。WS2软涂层具有极低的剪切强度和摩擦系数，(ZrN‑CrCN)x周期复合多层纳米硬涂层具有极高的耐磨性，Zr作为过渡层是为了减少涂层与基体间的残余热应力，从而提高涂层与基体的结合力。极大的提高了刀具的耐磨性并且降低了刀具在切削时的切削力和切削温度，从而使得刀具更能适应干切削中恶劣的切削环境。

Description

一种软硬复合纳米多层涂层刀具及其制备方法
技术领域
本发明属于机械切削刀具制造技术领域，特别是涉及一种新型软硬复合纳米多层涂层刀具及其制备方法。
背景技术
刀具硬涂层的优点是硬度高，耐磨性好，根据涂层材料的组分，涂层刀具可分为二元涂层、三元涂层、多元涂层。发展至后来，涂层的结构形式也有所变化，梯度涂层、微米涂层、纳米涂层相继出现。涂层也由单一层发展至后来的双层、多层、纳米级多层，涂层的硬度和耐磨性不断提高。软涂层刀具具有较低的剪切强度，刀具与工件的摩擦系数较低，但软涂层刀具耐磨性较差。目前基于硬涂层和软涂层的优缺点，刀具涂层趋于多元复合化，越来越多涂层技术的出现，使得涂层刀具在保证耐磨性的前提下摩擦系数更低，使用寿命更长。
中国专利(专利号ZL 201610430338.X)报道了“ZrTiN/MoS2复合减摩耐磨涂层刀具及其制备工艺”，它是采用电弧镀与中频磁控溅射复合镀膜方法制备的ZrTiN/MoS2复合涂层刀具，刀具基体至表面依次为Ti过渡层，Ti/Zr过渡层，ZrTiN和MoS2复合层。通过调控MoS2的含量，使得复合涂层既具有较高的硬度又具有MoS2较低的摩擦系数。但该复合涂层中的MoS2在350℃时会剧烈氧化，从而失去润滑功能减磨功能，严重影响了涂层刀具的应用范围和使用寿命。
中国专利(专利号ZL 201110082001.1)报道了“Ti-Zr/ZrN纳米多层涂层刀具及其制备工艺”，它是采用电弧离子镀方法制备的Ti-Zr/ZrN纳米多层涂层刀具，刀具基体至表面依次为Ti过渡层，Zr与ZrN交替多层，ZrN涂层。该刀具在保持较高硬度的同时提高了涂层的韧性和与基体间的结合强度，从而提高了耐磨性。但该涂层中主要的硬质涂层ZrN会随着切削距离的增长而使得摩擦系数增加，影响了被加工工件的表面质量，当摩擦距离进一步增长，超过 1000m时，涂层剥落。
发明内容
本发明的目的在于克服上述现有技术的不足，提供一种软硬复合纳米多层涂层刀具及其制备方法。充分弥补了硬质涂层在切削距离增长后摩擦系数增大的情况，极大地提高了被加工工件的表面质量和刀具的寿命。
为了解决上述的技术问题，本发明提供了一种软硬复合纳米多层涂层刀具的制备方法，所述刀具包括基体和基体表面的软硬复合涂层；
所述基体的材料为硬质合金，所述软硬复合涂层材料为：Zr、ZrN、CrCN 和WS2，涂层由内至外依次为Zr过渡层、(ZrN-CrCN)x周期复合多层纳米硬涂层、 WS2软涂层；
所述软硬复合涂层通过直流反应磁控溅射+射频反应磁控溅射沉积在基体的表面，其制备方法的步骤为：
(1)前处理：将基体经镜面抛光，经过超声波清洗后再经氮气吹干后放入镀膜机真空室；该真空室抽真空至气压小于4.0×10-4Pa，将基体加热至350 ℃-500℃，并保温一段时间；
(2)辉光清洗：对真空室通入Ar对基体的表面进行辉光清洗，去除基体表面微小附着杂质；
(3)采用直流磁控溅射技术在基体表面沉积一层Zr涂层：选用高纯Zr 靶放置于直流靶源上，通入高纯Ar气，Ar气的流量为70sccm，沉积气压为 0.5Pa-0.8Pa，沉积功率200-300W，沉积厚度为0.2-0.3μm；(4)在Zr涂层上再沉积(ZrN-CrCN)x涂层：
(4.1)首先沉积ZrN，采用直流反应磁控溅射技术，选用高纯Zr靶，通入N2与Ar的混合气体，气体总流量80-100sccm，沉积气压0.8-1.2Pa，溅射功率200-300W，沉积厚度50-60nm，关闭Zr靶；
(4.2)再沉积CrCN，采用射频磁控溅射技术，射频电源频率为13.56MHz，选用高纯Cr3C2靶放置于射频靶位，通入通入N2与Ar的混合气体，气体总流量 80-100sccm，沉积气压0.8-1.2Pa，溅射功率200-300W，基片偏压-150--200V，沉积厚度50-60nm，关闭Cr3C2靶；
(4.3)重复步骤4.1和4.2，得到(ZrN-CrCN)x周期复合多层纳米硬涂层，厚度1.4-1.6μm；
(5)在(ZrN-CrCN)x涂层上沉积WS2涂层：关闭Zr靶和Cr3C2靶，关闭氮气，通入Ar气，沉积气压1.0-1.2Pa，打开射频靶位的高纯WS2靶，采用射频磁控溅射技术，射频电源频率为13.56MHz，基片偏压-100--200V，溅射功率50-150W，沉积厚度0.5-0.7μm；
(6)后处理：关闭WS2靶，关闭电源及气体源，涂层结束。
在一较佳实施例中：在步骤1中，对基体进行超声波清洗具体是指：先将基体放入丙酮溶液超声清洗后，再将基体放入酒精溶液超声清洗。
在一较佳实施例中：在步骤2中，Ar气的工作气压1.5Pa，辉光放电清洗的时间为20分钟。
在一较佳实施例中：在步骤4.1中，N2与Ar的气体占比为1:4。
在一较佳实施例中：在步骤4.2中，N2与Ar的气体占比为1:3。
本发明还提供了一种软硬复合纳米多层涂层刀具，所述刀具包括基体和基体表面的软硬复合涂层；
所述基体的材料为硬质合金，所述软硬复合涂层材料为：Zr、ZrN、CrCN 和WS2，涂层由内至外依次为Zr过渡层、(ZrN-CrCN)x周期复合多层纳米硬涂层、 WS2软涂层。
相较于现有技术，本发明的技术方案具备以下有益效果：
本发明提供的软硬复合纳米多层涂层刀具，基体材料为硬质合金，涂层材料为：Zr、ZrN、CrCN和WS2，涂层由内至外依次为Zr过渡层、(ZrN-CrCN)x周期复合多层纳米硬涂层、WS2软涂层。Zr作为过渡层连接硬质合金刀具基体和(ZrN-CrCN)x周期纳米多层涂层，减小了刀具涂层的残余热应力，增强了涂层与基体的结合力。(ZrN-CrCN)x周期纳米多层涂层相较ZrN和CrCN单层，涂层硬度提升。WS2相较MoS2更易形成转移膜，摩擦系数更低，充分弥补了硬质涂层在切削距离增长后摩擦系数增大的情况，极大地提高了被加工工件的表面质量和刀具的寿命。
附图说明
图1为本发明的软硬复合纳米多层涂层刀具的涂层结构示意图。
图中：1为刀具基体，2为Zr过渡层，3为(ZrN-CrCN)x周期复合多层纳米硬涂层，4为WS2软涂层。
具体实施方式
下面给出本发明的两个最佳实施例：
一种软硬复合纳米多层涂层刀具，参考图1，所述刀具包括基,1和基体表面的软硬复合涂层；
所述基体的材料为硬质合金，所述软硬复合涂层材料为：Zr、ZrN、CrCN 和WS2，涂层由内至外依次为Zr过渡层2、(ZrN-CrCN)x周期复合多层纳米硬涂层3、WS2软涂层4。Zr作为过渡层连接硬质合金刀具基体和(ZrN-CrCN)x周期纳米多层涂层3，减小了刀具涂层的残余热应力，增强了涂层与基体的结合力。 (ZrN-CrCN)x周期纳米多层涂层3相较ZrN和CrCN单层，涂层硬度提升。WS2相较MoS2更易形成转移膜，摩擦系数更低，充分弥补了硬质涂层在切削距离增长后摩擦系数增大的情况，极大地提高了被加工工件的表面质量和刀具的寿命。
为了制备上述的刀具，本实施例给出了两种制备方法：
实施例一的制备方法的步骤如下：
(1)前处理：将硬质合金基底经镜面抛光，放入丙酮溶液超声清洗15分钟，再放入酒精溶液超声清洗15分钟，经氮气吹干后放入镀膜机真空室，该过程禁止触碰基体表面，真空室抽真空至3.0×10-4Pa，加热至350℃，保温 30分钟。
(2)辉光清洗：通入Ar气，工作气压1.5Pa，进行辉光放电清洗20分钟，去除基体表面微小附着杂质。
(3)沉积Zr：采用直流磁控溅射技术，选用纯Zr靶放置于直流靶源上，通入高纯Ar气，Ar流量70sccm，沉积气压0.5Pa，沉积功率200W，沉积厚度 0.2μm。
(4)沉积(ZrN-CrCN)x：首先沉积ZrN，采用直流反应磁控溅射技术，选用高纯Zr靶，通入N2/Ar，气体体积占比1:4，气体总流量80sccm，沉积气压 0.8Pa，溅射功率200W，沉积厚度50nm，关闭Zr靶；再沉积CrCN，采用射频磁控溅射技术，射频电源频率为13.56MHz，选用高纯Cr3C2靶，放置于射频靶位，通入N2/Ar，气体体积占比1:3，气体总流量80sccm，沉积气压0.8Pa，溅射功率200W，基片偏压-150V，沉积厚度50nm，关闭Cr3C2靶；如此依次重复，得到(ZrN-CrCN)x周期复合多层纳米硬涂层，厚度为1.5μm。
(5)沉积WS2：关闭Zr靶和Cr3C2靶，关闭氮气，通入Ar气，沉积气压 1Pa，打开射频靶位的高纯WS2靶，采用射频磁控溅射技术，射频电源频率为 13.56MHz，基片偏压-150V，溅射功率50W，沉积厚度0.4μm；
(6)后处理：关闭WS2靶，关闭电源及气体源，涂层结束。
实施例二的制备方法的步骤如下：
(1)前处理：将硬质合金基底经镜面抛光，放入丙酮溶液超声清洗15分钟，再放入酒精溶液超声清洗15分钟，经氮气吹干后放入镀膜机真空室，该过程禁止触碰基体表面，真空室抽真空至3.0×10-4Pa，加热至350℃，保温 30分钟。
(2)辉光清洗：通入Ar气，工作气压1.5Pa，进行辉光放电清洗20分钟，去除基体表面微小附着杂质。
(3)沉积Zr：采用直流磁控溅射技术，选用纯Zr靶放置于直流靶源上，通入高纯Ar气，Ar流量70sccm，沉积气压0.5Pa，沉积功率200W，沉积厚度 0.2μm。
(4)沉积(ZrN-CrCN)x：首先沉积ZrN，采用直流反应磁控溅射技术，选用高纯Zr靶，通入N2/Ar(气体占比1:4)，气体总流量80sccm，沉积气压0.8Pa，溅射功率200W，沉积厚度50nm，关闭Zr靶；再沉积CrCN，采用射频磁控溅射技术，射频电源频率为13.56MHz，选用高纯Cr3C2靶，放置于射频靶位，通入 N2/Ar(气体占比1:3)，气体总流量80sccm，沉积气压0.8Pa，溅射功率200W，基片偏压-150V，沉积厚度50nm，关闭Cr3C2靶；如此依次重复，得到(ZrN-CrCN)x周期复合多层纳米硬涂层，厚度1.0μm。
(5)沉积WS2：关闭Zr靶和Cr3C2靶，关闭氮气，通入Ar气，沉积气压 1Pa，打开射频靶位的高纯WS2靶，采用射频磁控溅射技术，射频电源频率为 13.56MHz，基片偏压-150V，溅射功率50W，沉积厚度0.9μm；
(6)后处理：关闭WS2靶，关闭电源及气体源，涂层结束。
以上所述，仅为本发明较佳实施例而已，故不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。

Claims (6)

1.一种软硬复合纳米多层涂层刀具的制备方法，其特征在于：所述刀具包括基体和基体表面的软硬复合涂层；
所述基体的材料为硬质合金，所述软硬复合涂层材料为：Zr、ZrN、CrCN和WS2，涂层由内至外依次为Zr过渡层、(ZrN-CrCN)x周期复合多层纳米硬涂层、WS2软涂层；
所述软硬复合涂层通过直流反应磁控溅射+射频反应磁控溅射沉积在基体的表面，其制备方法的步骤为：
(1)前处理：将基体经镜面抛光，经过超声波清洗后再经氮气吹干后放入镀膜机真空室；该真空室抽真空至气压小于4.0×10-4Pa，将基体加热至350℃-500℃，并保温一段时间；
(2)辉光清洗：对真空室通入Ar对基体的表面进行辉光清洗，去除基体表面微小附着杂质；
(3)采用直流磁控溅射技术在基体表面沉积一层Zr涂层：选用高纯Zr靶放置于直流靶源上，通入高纯Ar气，Ar气的流量为70sccm，沉积气压为0.5Pa-0.8Pa，沉积功率200-300W，沉积厚度为0.2-0.3μm；(4)在Zr涂层上再沉积(ZrN-CrCN)x涂层：
(4.1)首先沉积ZrN，采用直流反应磁控溅射技术，选用高纯Zr靶，通入N2与Ar的混合气体，气体总流量80-100sccm，沉积气压0.8-1.2Pa，溅射功率200-300W，沉积厚度50-60nm，关闭Zr靶；
(4.2)再沉积CrCN，采用射频磁控溅射技术，射频电源频率为13.56MHz，选用高纯Cr3C2靶放置于射频靶位，通入通入N2与Ar的混合气体，气体总流量80-100sccm，沉积气压0.8-1.2Pa，溅射功率200-300W，基片偏压-150--200V，沉积厚度50-60nm，关闭Cr3C2靶；
(4.3)重复步骤4.1和4.2，得到(ZrN-CrCN)x周期复合多层纳米硬涂层，厚度1.4-1.6μm；
(5)在(ZrN-CrCN)x涂层上沉积WS2涂层：关闭Zr靶和Cr3C2靶，关闭氮气，通入Ar气，沉积气压1.0-1.2Pa，打开射频靶位的高纯WS2靶，采用射频磁控溅射技术，射频电源频率为13.56MHz，基片偏压-100--200V，溅射功率50-150W，沉积厚度0.5-0.7μm；
(6)后处理：关闭WS2靶，关闭电源及气体源，涂层结束。
2.根据权利要求1所述的一种软硬复合纳米多层涂层刀具的制备方法，其特征在于：在步骤1中，对基体进行超声波清洗具体是指：先将基体放入丙酮溶液超声清洗后，再将基体放入酒精溶液超声清洗。
3.根据权利要求1所述的一种软硬复合纳米多层涂层刀具的制备方法，其特征在于：在步骤2中，Ar气的工作气压1.5Pa，辉光放电清洗的时间为20分钟。
4.根据权利要求1所述的一种软硬复合纳米多层涂层刀具的制备方法，其特征在于：在步骤4.1中，N2与Ar的气体占比为1:4。
5.根据权利要求1所述的一种软硬复合纳米多层涂层刀具的制备方法，其特征在于：在步骤4.2中，N2与Ar的气体占比为1:3。
6.一种软硬复合纳米多层涂层刀具，其特征在于：所述刀具包括基体和基体表面的软硬复合涂层；
所述基体的材料为硬质合金，所述软硬复合涂层材料为：Zr、ZrN、CrCN和WS2，涂层由内至外依次为Zr过渡层、(ZrN-CrCN)x周期复合多层纳米硬涂层、WS2软涂层。
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