CN114507858A - 一种长寿命超纳米金刚石周期性多层涂层刀具的制备方法 - Google Patents

一种长寿命超纳米金刚石周期性多层涂层刀具的制备方法 Download PDF

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CN114507858A
CN114507858A CN202210094826.3A CN202210094826A CN114507858A CN 114507858 A CN114507858 A CN 114507858A CN 202210094826 A CN202210094826 A CN 202210094826A CN 114507858 A CN114507858 A CN 114507858A
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nano diamond
nitrogen
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刘金龙
屠菊萍
李成明
赵云
郑宇亭
魏俊俊
陈良贤
张建军
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University of Science and Technology Beijing USTB
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Abstract

一种长寿命超纳米金刚石周期性多层涂层刀具的制备方法，属于涂层刀具的制造技术领域。该多层化刀具涂层主要包括基体、过渡层及周期性低掺氮和高掺氮超纳米金刚石多层膜。基体的材质主要是硬质合金类，过渡层厚度为100nm‑800nm，多层膜的单层厚度均小于10nm。制备方法主要包括：基体表面预处理，选择合适的喷砂速度和喷砂粒径，对基体表面进行喷砂处理，经稀硫酸溶液清洗后，获得具有合适粗糙度的基体；然后在刀具表面镀Ti/Mo复合过渡层，提高界面结合力，降低界面内应力；之后在纳米级粉体悬浊液中超声以增加形核密度；最后通过周期性调整掺氮浓度制备含氮量不同的超纳米金刚石多层涂层。本发明刀具具有硬度高、韧性好、表面光滑、精度高、寿命长等优点。

Description

一种长寿命超纳米金刚石周期性多层涂层刀具的制备方法
本案是申请号201910667303.1、申请日20190723、发明名称《一种长寿命超纳米金刚石周期性多层涂层刀具的制备方法》的分案申请。
技术领域
本发明属于涂层刀具的制造技术领域，具体地涉及一种基于加工刀具的超纳米金刚石周期性多层涂层刀具，特别是提供了一种具有高硬度和高强韧性的长寿命超纳米金刚石周期性多层涂层及其制备方法，特点是在保证单层刀具高硬度同时，通过多层化提高超纳米金刚石涂层刀具的韧性。
背景技术
金刚石是已知最硬的天然材料，具有极高的硬度，广泛应用于机械、生物医药、电子和光子等领域。随着技术的发展，对工业刀具的要求越来越高，如加工碳纤维和高硅铝材料，需要刀具具有极高的耐磨性(许立,马宁,李丙文.一种金刚石复合涂层刀具及其制备方法[P].中国专利:CN 108149219 A,2018,06,12.)，加工硬度较高的材料需要刀具具有较好的韧性。由于金刚石高的脆性，导致金刚石刀具容易崩刃，显著降低其寿命。而且现有的金刚石涂层刀具中金刚石涂层和硬质合金的结合力较弱，在使用过程中金刚石涂层容易发生脱落(R·M·佩尼奇,P·L·赫格德,A·因斯佩克托.纳米涂层刀具及其制造方法[P].中国专利:CN 1643183A,2005,07,20.)。这些问题都严重影响金刚石涂层刀具的使用寿命。
超纳米金刚石(UNCD)晶粒尺寸小于10nm，表面光滑平整，具有良好的表面质量。超纳米金刚石涂层是以SP3杂化的碳原子占绝大多数的、具有某种网状结构的膜层中晶粒尺寸小于40nm的碳薄膜(姚勇.一种基于加工刀具的复合涂层制备工艺[P].中国专利:CNIO8315716A,2018.07.24.)。UNCD涂层不仅具有良好的膜 -基附着强度，而且能够有效降低金刚石涂层的表面粗糙度，可提高刀具的切削性能。由于UNCD晶粒小、晶界比例高，在量子尺寸效应，小尺寸效应，表面效应，界面效应等更加明显，在力学，声学，光学，电学等方面的一些性能更加优越，使之越来越接近和满足工业生产和实际应用要求(吕琳,汪建华,翁俊,等. 超纳米金刚石薄膜的性能和制备及应用[J].真空与低温,2014,20(3):125-131.)。但单层涂层刀具由于在高温下沉积，会造成涂层与基体间存在应力，容易导致脱膜现象，从而严重影响刀具的使用寿命。
发明内容
本发明的目的在于设计一种长寿命超纳米金刚石多层刀具涂层及其制备方法。增加过渡层提高膜基结合力，降低应力，具有多层化的涂层刀具在使用过程中会使刀具的韧性大幅度提升，提高UNCD多层涂层刀具的使用寿命。周期性掺氮生长的多层涂层刀具，多层的存在会使切削力沿着层与层之间分散，从而使超纳米金刚石周期性多层涂层刀具的韧性提高，不易断裂。
该多层化刀具涂层主要包括刀具基体、Ti/Mo复合过渡层，之后是少掺氮超纳米金刚石层和多掺氮超纳米金刚石层交替生长形成UNCD多层膜交替生长的涂层材料。所述衬底的材质主要是硬质合金类，所述Ti/Mo复合过渡层的厚度为 100nm-600nm，所述少掺氮超纳米金刚石层的厚度小于10nm，所述多掺氮超纳米金刚石层的厚度小于10nm，直至达到所要求的涂层厚度。首先对刀具表面进行预处理，随后在基体表面采用磁控溅射镀一层Ti/Mo复合以降低内应力，再放入纳米金刚石悬浊液中超声震荡，干燥后依次通入甲烷、氮气、氧气、氩气等两种或多种混合气体。在生长过程中，通过编程自动化控制生长参数，实现层与层不同的生长工艺参数，从而得到超纳米金刚石周期性多层涂层。每层超纳米金刚石的厚度小于10nm，层与层之间的区别在于气体通入量不同。最后超声清洗干净即得到超纳米金刚石周期性多层涂层材料。
一种长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于刀具基体表面周期性生长超纳米金刚石多层涂层，显著提高刀具寿命，具体包括以下步骤：
步骤1：基体表面预处理：
1.1首先对基体表面进行喷砂处理，以去除表面油污、氧化层与底材金属；
1.2喷砂后的基体经稀硫酸溶液清洗，提高涂层与基体之间的结合强度，减小应力；
1.3依次使用丙酮、无水乙醇、去离子水对预处理的基体进行超声清洗，去除表面杂质及残留的酸溶液；
步骤2：在刀具表面镀Ti/Mo复合过渡层：
采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空，分别溅射纯钛靶和钼靶，沉积结束后，等待腔室温度冷却到室温时，取出刀具；
步骤3：在纳米级粉体悬浊液中进行超声震荡以增加形核密度：
将上述镀有Ti/Mo复合过渡层的刀具置于纳米金刚石悬浊液中进行超声震荡，后在烘箱中干燥；
步骤4：超纳米金刚石周期性多层涂层刀具的制备：
将处理好的刀具基体置于微波真空腔室中，通过周期性调整氮含量进行多层沉积，根据设计涂层的厚度，沉积不同的时间和周期。
进一步地，所述基体表面预处理的具体流程为：对基体表面进行喷砂处理，喷砂粒径为0.125-0.35μm，喷砂压力为0.2-1.0MPa，样品与喷嘴的距离为3-6cm，以去除表面油污、氧化层与底材金属并能提高涂层与基体之间的结合强度。
进一步地，所述在刀具表面镀Ti/Mo复合过渡层：采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空；用氩等离子体清洗基体10-40min；随后控制氩气流量为10-80sccm，分别溅射纯钛靶和钼靶，靶材与基片的距离为8-20cm，制得厚度为100-800nm的Ti/Mo复合膜，沉积时间为10-60min，温度120-180℃。
进一步地，所述将镀完过渡层的刀具在纳米级粉体悬浊液中进行超声震荡：纳米金刚石颗粒的粒径范围为1-100nm，超声震荡的时间为20-120min，超声功率50-200瓦，最后在烘箱中干燥5-40min；经超声分散后，纳米金刚石粉变成粒径更小的纳米金刚石颗粒，吸附在刀具基体表面，从而增加形核密度。
进一步地，所述超纳米金刚石周期性多层涂层材料的制备：基体预处理之后置于微波真空腔室中，抽本底真空小于0.1Pa后，通入超纯氢气(纯度99.9999％以上)50-500sccm，后升微波功率和腔压使温度达到生长温度600-800℃，再依次通入1-100sccm的甲烷，0.1-20sccm的氧气，0.1-30sccm的氮气，功率范围在 1000-3000W，腔压6.0-12.0KPa，使样品温度保持在600-800℃；通过周期掺入少量与多量氮气，实现多层超纳米金刚石膜生长，每层生长厚度小于10nm，两层为一个周期，根据设计涂层的厚度，沉积不同的时间和周期。一般刀具涂层 4-10μm，故沉积200-500个周期即可。
进一步地，所述掺入氮气的含量：少掺氮生长层的氮含量在0.1-7sccm范围内，多掺氮生长层的氮含量在7-30sccm范围内，通过高低掺氮量的调控，可以形成多层界面与界面应力场，造成界面和应力场阻碍位错运动，从而实现增强增韧。
进一步地，该生长超纳米金刚石的温度必须在600-800℃，温度过高易生成多晶金刚石，温度太低会降低生成超纳米金刚石的质量，影响其切削性能。
至此实现了超纳米金刚石的生长，制备了超纳米金刚石周期性多层涂层材料。该涂层材料不但硬度和弹性模量高，还具有极好的平滑度和较小的摩擦系数，而且抗磨损、导热性好、内应力小、黏附性极好，与硬质合金基体附着力强，特别适合用来作为刀具、钻头、流体动力轴承等机械设备的耐磨层。
本发明实施过程的关键在于：
1.基体表面预处理，为了增加基体与涂层的结合力，以及增加形核密度，首先选择合适的喷砂速度和喷砂粒径，对基体表面进行喷砂处理，去除表面油污、氧化层与底材金属。喷砂后的基体经稀硫酸溶液清洗，可得到具有合适粗糙度的基体，提高涂层与基体之间的结合强度。最后欲将基体与涂层结合的牢固，需要保证基体表面的清洁，依次使用丙酮、无水乙醇、去离子水对预处理的基体进行超声清洗，去除表面杂质及残留的酸溶液，超声波功率为30-200瓦，每次清洗 10-30min，至吹干后无水痕。
2.为了降低涂层的内应力，选择镀一层Ti/Mo复合过渡层作为过渡层，采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空；后通入氩气，用氩等离子体清洗基体10-40min；随后控制氩气流量为10-80sccm，分别溅射纯钛靶和钼靶，靶材与基片的距离为8-20cm，制得厚度为100-800nm的Ti/Mo复合膜，沉积时间为10-60min，温度120-180℃；沉积结束后，等待腔室温度冷却到室温时，取出刀具，过渡层的存在，不仅能够提高基体与涂层的结合强度，而且能够降低基体与涂层之间的内应力。
3.将上述镀有Ti/Mo复合过渡层的刀具置于纳米金刚石悬浊液中进行超声震荡，其中，纳米金刚石颗粒的粒径范围为1-100nm，超声震荡的时间为20-120min，超声功率50-200瓦，最后在烘箱中干燥5-40min。经超声分散后，纳米金刚石粉变成粒径更小的纳米金刚石颗粒，会吸附在刀具基体表面，从而增加形核密度。
4.传统的生长超纳米金刚石是在富氩无氢或富氩少氢的气氛中再通入甲烷气体，而本发明是在富氢无氩气氛下，再通入氧气、氮气和甲烷气体环境中进行 UNCD的沉积。
5.该生长超纳米金刚石的温度在600-800℃，温度过高易生成多晶金刚石，温度太低生成的超纳米金刚石质量不好。
6.多层生长：通过实验得到多掺氮和少掺氮的生长速率，采用编程控制周期性多层的生长工艺参数，使每层厚度小于10nm，通过设置循环次数实现总生长厚度。
7.多层中周期性掺氮的氮含量在一定的范围内，通过高低掺氮量的调控，可以形成多层界面与界面应力场，会造成界面和应力场阻碍位错运动，从而实现增强增韧。
8.周期性生长多层涂层的过程中，少量氧气的通入有利于超纳米金刚石颗粒的质量和表面光滑度，降低刀具表面粗糙度，提高其使用寿命。
9.制备超纳米金刚石周期性多层涂层材料的方法广泛，比如，微波等离子体化学气相沉积法(MPCVD)、气体循环直流旋转电弧等离子体法(DC Arc Plasma Jet)、射频等离子体气相沉积法(RFPCVD)等。
本发明的优点是：
1.该超纳米金刚石周期性多层涂层刀具，具有400-1000层的涂层，且每层厚度小于10nm，切削时会使切削力沿着层与层扩散，具有一定的弹性，刀具使用过程中不易发生脆性断裂，故韧性得到了提高，从而显著提高了刀具的寿命。
2.由于超纳米金刚石多层交替生长，保证硬度和韧性的同时，表面为超纳米金刚石膜，平整光滑，表面质量较高，不易引起应力集中。光滑的表面会减小刀具与工件材料接触时产生的磨损和切削力，从而延长涂层刀具的工作寿命。
3.该制备超纳米金刚石周期性多层涂层刀具的工艺，只需周期性调整气体中的氮含量，且可编程控制调整量与气体通入与抽出时间，对设备与工艺要求简单，便于实现与工业化应用。
附图说明
图1为一种长寿命超纳米金刚石周期性多层涂层刀具结构示意图；其中1 为刀具基体，2为Ti/Mo过渡层，3为少掺氮超纳米金刚石层，4为多掺氮超纳米金刚石层；
图2为本发明方法中超纳米金刚石周期性多层涂层材料的制备流程图；
图3(a)为超纳米金刚石周期性多层涂层表面形貌图；
图3(b)为超纳米金刚石周期性多层涂层拉曼光谱图。
具体实施方式
下面结合具体实施例对本发明的技术方案做进一步说明。
经表面预处理后的基体放入真空腔室中，采用磁控溅射在刀具表面镀一层过渡层，随后在超声波悬浮液中震荡，干燥后放入真空腔室中，在生长温度下通入生长所需要的各种原料气体，通过编程控制每层的工艺参数和时间，使少掺氮层与多掺氮层交替生长，从而进行周期性多层生长，其具体流程见图2。
实施例1
将所选用的厚度2mm，尺寸3cm×3cm硬质合金基体进行表面预处理，具体流程为：首先选择合适的喷砂速度和喷砂粒径，对基体表面进行喷砂处理，去除表面油污、氧化层与底材金属。喷砂后的基体经稀硫酸溶液清洗，可得到粗糙度为19.7nm的基体，提高涂层与基体之间的结合强度。最后依次使用丙酮、无水乙醇、去离子水对预处理的基体进行超声清洗，去除表面杂质及残留的酸溶液，超声波功率为80瓦，每次清洗10min，至吹干后无水痕。采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空；后通入氩气，用氩等离子体清洗基体30min；随后控制氩气流量为20sccm，分别溅射纯钛靶和钼靶，靶材与基片的距离为10cm，制得厚度为500nm的Ti/Mo 复合膜，沉积时间为40min，温度150℃；沉积结束后，等待腔室温度冷却到室温时，取出刀具。将上述镀有Ti/Mo复合过渡层的刀具置于纳米金刚石悬浊液中进行超声震荡，悬浊液中纳米金刚石颗粒的粒径范围为30/50nm，超声震荡的时间为30min，超声功率80瓦，最后在烘箱中干燥20-30min。之后将刀具置于微波真空腔室中，开机械泵抽本底真空小于0.1Pa后，通入超纯氢气(纯度99.9999％以上)300sccm，升功率至2300W，腔室压力达到9.5kPa，使刻蚀温度达到750℃，后设置第一层少掺氮层生长工艺参数：功率2290W，腔压至7.4kPa，甲烷15sccm，氧气0.5sccm，氮气1sccm，样品温度750℃，时间1min。第二层多掺氮层工艺参数：功率2180W，腔压至7.9kPa，甲烷15sccm，氧气0.5sccm，氮气8sccm，样品温度750℃，时间55S。设定循环周期次数200次。循环结束之后即可在硬质合金基体上得到200个周期共400层少掺氮与多掺氮交替生长4μm厚的多层涂层刀具。其表面形貌与表面拉曼图谱示于图3。由图3(a)可见生长的多层涂层表面非常光滑和平整。从图3(b)拉曼图谱看见，除去金刚石1332cm-1处强的本征峰，在1190cm-1和1490cm-1存在峰位，证明成功生成了超纳米金刚石涂层材料。
实施例2
将所选用的厚度0.8mm，尺寸4mm×4mm多晶金刚石衬底进行预处理，具体流程为：首先选择合适的喷砂速度和喷砂粒径，对基体表面进行喷砂处理，去除表面油污、氧化层与底材金属。喷砂后的基体经稀硫酸溶液清洗，可得到粗糙度为19.9nm的基体，提高涂层与基体之间的结合强度。最后依次使用丙酮、无水乙醇、去离子水对预处理的基体进行超声清洗，去除表面杂质及残留的酸溶液，超声波功率为80瓦，每次清洗10min，至吹干后无水痕。采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空；后通入氩气，用氩等离子体清洗基体20min；随后控制氩气流量为20sccm，分别溅射纯钛靶和钼靶，靶材与基片的距离为10cm，制得厚度为300nm的Ti/Mo 复合膜，沉积时间为25min，温度150℃；沉积结束后，等待腔室温度冷却到室温时，取出刀具。将上述镀有Ti/Mo复合过渡层的刀具置于纳米金刚石悬浊液中进行超声震荡，悬浊液中纳米金刚石颗粒的粒径范围为30/50nm，超声震荡的时间为30min，超声功率80瓦，最后在烘箱中干燥20-30min。之后将刀具置于微波真空腔室中，开机械泵抽本底真空小于0.1Pa后，通入超纯氢气(纯度99.9999％以上)300sccm，升功率至2300W，腔室压力达到9.5kPa，使刻蚀温度达到750℃，后设置第一层生长工艺参数：功率2290W，腔压至7.4kPa，甲烷15sccm，氧气 0.5sccm，氮气1sccm，样品温度750℃，时间1min。第二层工艺参数：功率2180W，腔压至7.9kPa，甲烷15sccm，氧气0.5sccm，氮气8sccm，样品温度750℃，时间55S。设定循环周期次数200次。循环结束之后即可在刀具基体上得到200个周期共400层少掺氮与多掺氮交替生长4μm厚的超纳米金刚石周期性多层涂层材料。
实施例3
将所选用的厚度3mm，尺寸3cm×1cm硬质合金衬底进行预处理，具体流程为：首先选择合适的喷砂速度和喷砂粒径，对基体表面进行喷砂处理，去除表面油污、氧化层与底材金属。喷砂后的基体经稀硫酸溶液清洗，可得到粗糙度为 19.5nm的基体，提高涂层与基体之间的结合强度。最后依次使用丙酮、无水乙醇、去离子水对预处理的基体进行超声清洗，去除表面杂质及残留的酸溶液，超声波功率为80瓦，每次清洗10min，至吹干后无水痕。采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空；后通入氩气，用氩等离子体清洗基体30min；随后控制氩气流量为20sccm，分别溅射纯钛靶和钼靶，靶材与基片的距离为10cm，制得厚度为500nm的Ti/Mo复合膜，沉积时间为40min，温度150℃；沉积结束后，等待腔室温度冷却到室温时，取出刀具。将上述镀有Ti/Mo复合过渡层的刀具置于纳米金刚石悬浊液中进行超声震荡，悬浊液中纳米金刚石颗粒的粒径范围为30/50nm，超声震荡的时间为30min，超声功率80瓦，最后在烘箱中干燥20-30min。之后将刀具置于微波真空腔室中，开机械泵抽本底真空小于0.1Pa后，通入超纯氢气(纯度99.9999％以上)300sccm，升功率至2300W，腔室压力达到9.5kPa，使刻蚀温度达到750℃，后设置第一层生长工艺参数：功率2290W，腔压至7.4kPa，甲烷15sccm，氧气 0.5sccm，氮气1sccm，样品温度750℃，时间1min。第二层工艺参数：功率2180W，腔压至7.9kPa，甲烷15sccm，氧气0.5sccm，氮气8sccm，样品温度750℃，时间55S。设定循环周期次数200次。循环结束之后即可在硬质合金基体上得到200 个周期共400层少掺氮与多掺氮交替生长4μm厚的超纳米金刚石周期性多层涂层材料。
实施例4
将所选用的厚度0.5mm，尺寸8mm×8mm硬质合金衬底进行预处理，具体流程为：首先选择合适的喷砂速度和喷砂粒径，对基体表面进行喷砂处理，去除表面油污、氧化层与底材金属。喷砂后的基体经稀硫酸溶液清洗，可得到粗糙度为19.3nm的基体，提高涂层与基体之间的结合强度。最后依次使用丙酮、无水乙醇、去离子水对预处理的基体进行超声清洗，去除表面杂质及残留的酸溶液，超声波功率为60瓦，每次清洗10min，至吹干后无水痕。采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空；后通入氩气，用氩等离子体清洗基体30min；随后控制氩气流量为20sccm，分别溅射纯钛靶和钼靶，靶材与基片的距离为10cm，制得厚度为500nm的Ti/Mo 复合膜，沉积时间为40min，温度150℃；沉积结束后，等待腔室温度冷却到室温时，取出刀具。将上述镀有Ti/Mo复合过渡层的刀具置于纳米金刚石悬浊液中进行超声震荡，悬浊液中纳米金刚石颗粒的粒径范围为30/50nm，超声震荡的时间为30min，超声功率60瓦，最后在烘箱中干燥20-30min。之后将刀具置于微波真空腔室中，开机械泵抽本底真空小于0.1Pa后，通入超纯氢气(纯度99.9999％以上)300sccm，升功率至2300W，腔室压力达到9.5kPa，使刻蚀温度达到750℃，后设置第一层生长工艺参数：功率2290W，腔压至7.4kPa，甲烷15sccm，氧气 0.5sccm，氮气1sccm，样品温度750℃，时间1min。第二层工艺参数：功率2180W，腔压至7.9kPa，甲烷15sccm，氧气0.5sccm，氮气8sccm，样品温度750℃，时间55S。设定循环周期次数300次。循环结束之后即可在硬质合金基体上得到300 个周期共600层少掺氮与多掺氮交替生长6μm厚的超纳米金刚石周期性多层涂层材料。

Claims (7)

1.一种长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于,刀具基体表面周期性生长超纳米金刚石多层涂层，包括以下步骤：
步骤1：基体表面预处理：
1.1首先对基体表面进行喷砂处理，以去除表面油污、氧化层与底材金属；
1.2喷砂后的基体经稀硫酸溶液清洗，提高涂层与基体之间的结合强度，减小应力；
1.3依次使用丙酮、无水乙醇、去离子水对预处理的基体进行超声清洗，去除表面杂质及残留的酸溶液；
步骤2：在刀具表面镀Ti/Mo复合过渡层：
采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空，分别溅射纯钛靶和钼靶，沉积结束后，等待腔室温度冷却到室温时，取出刀具；
步骤3：在纳米级粉体悬浊液中进行超声震荡以增加形核密度：
将上述镀有Ti/Mo复合过渡层的刀具置于纳米金刚石悬浊液中进行超声震荡，后在烘箱中干燥；
步骤4：超纳米金刚石周期性多层涂层刀具的制备：
将处理好的刀具基体置于微波真空腔室中，通过周期性调整氮含量进行多层沉积，根据设计涂层的厚度，沉积不同的时间和周期。
2.根据权利要求1所述长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于，基体表面预处理的具体流程为：对基体表面进行喷砂处理，喷砂粒径为0.125-0.35μm，喷砂压力为0.2-1.0MPa，样品与喷嘴的距离为3-6cm，以去除表面油污、氧化层与底材金属并能提高涂层与基体之间的结合强度。
3.根据权利要求1所述长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于，在刀具表面镀Ti/Mo复合过渡层：采用射频直流磁控溅射系统设备，将刀具固定在衬底板上，然后把衬底板放到沉积腔室中，抽真空；用氩等离子体清洗基体10-40min；随后控制氩气流量为10-80sccm，分别溅射纯钛靶和钼靶，靶材与基片的距离为8-20cm，制得厚度为100-800nm的Ti/Mo复合膜，沉积时间为10-60min，温度120-180℃。
4.根据权利要求1所述长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于，将镀完过渡层的刀具在纳米级粉体悬浊液中进行超声震荡：纳米金刚石颗粒的粒径范围为1-100nm，超声震荡的时间为20-120min，超声功率50-200瓦，最后在烘箱中干燥5-40min。
5.根据权利要求1所述长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于，超纳米金刚石周期性多层涂层材料的制备：基体预处理之后置于微波真空腔室中，抽本底真空小于0.1Pa后，通入超纯氢气(纯度99.9999％以上)50-500sccm，后升微波功率和腔压使温度达到生长温度600-800℃，再依次通入1-100sccm的甲烷，0.1-20sccm的氧气，0.1-30sccm的氮气，功率范围在1000-3000W，腔压6.0-12.0KPa，使样品温度保持在600-800℃；通过周期掺入少量与多量氮气，实现多层超纳米金刚石膜生长，每层生长厚度小于10nm，两层为一个周期，根据设计涂层的厚度，沉积不同的时间和周期。
6.根据权利要求1或5所述长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于，掺入氮气的含量：少掺氮生长层的氮含量在0.1-7sccm范围内，多掺氮生长层的氮含量在7-30sccm范围内，通过高低掺氮量的调控，可以形成多层界面与界面应力场，造成界面和应力场阻碍位错运动，从而实现增强增韧。
7.根据权利要求1所述长寿命超纳米金刚石周期性多层涂层刀具的制备方法，其特征在于，周期性生长多层超纳米金刚石涂层的过程中，少量氧气的通入有利于超纳米金刚石颗粒的质量和表面光滑度，降低刀具表面粗糙度，提高其使用寿命。
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