CN106756785A - 一种多元复合纳米硬质涂层及其制备方法 - Google Patents
一种多元复合纳米硬质涂层及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于切削刀具表面用多元复合纳米硬质涂层,所述涂层包括至少两层CrN和CrTiBN,其中CrN层的Cr与N的原子百分比为60:40至70:30,CrTiBN层中各原子的百分比为Cr 10‑25%、Ti 8‑30%、B 14‑29%、N 30‑60%。根据本发明的所述涂层中B元素具有细化晶粒的作用,大幅提高了涂层硬度,并且对涂层抗高温氧化性和抗化学反应性的提高也有一定作用,可以有效延长工具的使用寿命。
Description
技术领域
本发明属于金属表面涂层技术领域,具体涉及采用一种物理气相沉积(PVD)技术对多元复合结构的纳米硬质涂层的制备。
背景技术
气相沉积技术主要包括CVD(化学气相沉积)和PVD(物理气相沉积),是当代真空技术和材料科学中最活跃的研究领域,也是目前刀具表面涂层技术的主流方向,它不仅可以用来制备各种特殊性能的薄膜涂层,而且还可以用来制备各种功能薄膜材料和装饰薄膜涂层以及沉积各种各样的化合物、非金属、半导体、陶瓷、塑料膜等。PVD技术与CVD技术相比,其沉积温度高;沉积速率快;沉积的涂层具有细微结构、抗裂纹扩展能力强;涂层表面光滑、摩擦系数低;涂层制备是在真空条件下,复合绿色制造的理念。目前PVD涂层已经扩展到了航空航天、机械加工、电子通讯、医疗器械、家电等行业,涂层类型也从最初的TiN、TiC单层涂层发展到了多层涂层、多元复合涂层、梯度涂层以及纳米涂层等。
单层涂层在气相沉积技术发展的前十几年中一直被采用,典型的代表有TiC、TiN、Al2O3、CrN,其余的还有NbC、HfC、ZrC、ZrN、BN等。其中CrN涂层目前应用最为广泛,是被誉为最能替代TiN涂层的材料之一,并且由于其耐磨性优良,其主要用于塑料膜、冷镦冲头等模具,又根据其良好的抗粘结性和化学稳定性切削软材料如钛合金,钛、铜、铝等。
多层涂层与单层涂层相比能够有效的抑制粗大晶粒组织的生长,改善涂层组织状况,发挥出各层不同涂层材料的优点,有效的提高产品性能。最常用的多层涂层是2种涂层组合或者层数在3~7层之间的多层复合涂层。
多元复合涂层是在单层涂层、多层涂层中加入如Cr、Zr、V、B、Hf等元素,能够提高抗氧化性和抗磨损性,并大大改善涂层与基材之间的结合力。目前,最常用的是TiCN和TiAlN,其余还有TiSiN、TiBN、TiAlSi、TiAlCN等。
因此梯度涂层是对基材表面进行梯度化处理,使涂层基体表面一定深度区域形成碳化物和碳氮化物的韧性区,此区域的粘结剂含量一般高于涂层基体的名义粘结剂含量,当裂纹扩展到此区域时,由于此韧性区韧性优异,将有效的吸收裂纹扩展的能量,提高刀具的使用寿命。
纳米涂层以高硬度、高耐热性、相对较高的韧性以及在低成本和绿色加工的前提下有高的使用寿命等特点一经面世就引起了研究者的广泛关注。其主要分为纳米多层结构和纳米复合结构涂层两类。
发明内容
本发明目的是提供一种用于切削刀具表面用多元复合纳米硬质涂层,所述涂层包括至少两层CrN和CrTiBN,其中CrN层的Cr与N的原子百分比为60:40至70:30,优选为67:33,CrTiBN层中各原子的百分比为Cr 10-25%、Ti 8-30%、B 14-29%、N 30-60%,优选为Cr20%、Ti19%、B19%和N42%。
优选地,所述涂层包括多层CrN和CrTiBN,优选为2-200层,优选为4-50层,更优选为2至4层,所述CrN层和CrTiBN层交替排列,优选最内层为CrN层,最外层为CrTiBN层。
优选地,所述涂层中CrN层厚度为0.3~0.35μm和CrTiBN层厚度为2.5~3μm,进一步优选地,所述CrN层厚度为0.33μm和CrTiBN层厚度为2.8μm。
优选地,包括所述CrN层和CrTiBN层的涂层的总厚度约为3~8μm。
根据本发明的包括所述CrN层和CrTiBN层的涂层的制备方法没有特别限制,可以利用本领域常规的PVD沉积方法制备所述各层。优选地,可以按照以下方法制备:
本发明另一个目的是提供一种所述多元复合纳米硬质涂层的制备方法,所述制备方法包括以下步骤:
步骤1)基材前处理:将基材放入清洗线超声槽依次进行除油、除锈等工序,进行粗洗;然后粗洗后对基材进行喷砂处理;最后将基材放入清洗线进行超声精洗,并烘干30min。
步骤2)将基材固定在转架上,以3维方式转动,等炉腔真空度达到8.0×10-3Pa,温度达到400℃时,开始运行PVD涂层处理。
步骤3)通入氩气辉光40min后打开Cr靶进行Cr轰击;30min后通入氮气进行CrN层沉积,涂层时间10至20min,预计厚度0.3~0.35μm。
步骤4)打开Ti靶5min后再开B靶并保持Cr靶开启状态,沉积CrTiBN层40至60min,预计厚度2.5~3μm。
优选地,所述步骤3)和步骤4)可以交替进行多次,以交替形成多层CrN层和CrTiBN层。
所述步骤3)工艺参数为:真空度1.5Pa,氩气输入量20~25,氮气输入量240~250,偏压150V,温度380℃。
步骤4)工艺参数为:真空度1.6Pa,氩气输入量7~10,氮气输入量260~270,偏压110V,温度380℃。
有益效果
(1)涂层中B元素具有细化晶粒的作用,大幅提高了涂层硬度,并且对涂层抗高温氧化性和抗化学反应性的提高也有一定作用。
(2)涂层中Cr、N元素的含量较多,大幅提高了涂层的抗高温氧化性。
(3)涂层表面含有Ti和B元素,有效降低了涂层表面的摩擦系数,提高了耐磨性。
(4)涂层采用CrN打底、多层分布的结构分布,减小了涂层内应力和涂层内部裂纹扩展,提高了膜基结合力,增加了涂层产品的使用寿命。
根据本发明的包括所述CrN层和CrTiBN层的涂层有效解决高速干式切削刀具和热作模具加工条件苛刻的问题,延长工具的使用寿命。
附图说明
图1为CrN/CrTiBN多元复合纳米硬质涂层4层结构示意图
图2为CrN/CrTiBN多元复合纳米硬质涂层制备过程流程图
图3为实施例1滚齿刀CrN/CrTiBN涂层产品外观
图4为实施例2铝压铸模具CrN/CrTiBN涂层产品外观
具体实施方式
根据本发明所述涂层中CrN层为过渡层,其可以提高膜基结合力;CrTiBN层内部内应力小、抗裂纹扩展能力强;并且涂层表面含有B元素,能够有效降低摩擦系数、提高涂层抗摩擦磨损性。
根据本发明的所述包括所述CrN层和CrTiBN层的涂层中,在CrTiBN层中引入了B元素,并且B元素的原子百分比控制在14-29%的范围内,优选为19%,本发明的发明人发现当在层中引入B元素并控制B元素的原子百分比在上述范围内时,可以非常显著的提高涂层的硬度和抗氧化温度。当B 元素的原子百分比在上述范围内时,则无法实现涂层硬度和抗氧化温度的提高。
以下,将详细地描述本发明。在进行描述之前,应当理解的是,在本说明书和所附的权利要求书中使用的术语不应解释为限制于一般含义和字典含义,而应当在允许发明人适当定义术语以进行最佳解释的原则的基础上,根据与本发明的技术方面相应的含义和概念进行解释。因此,这里提出的描述仅仅是出于举例说明目的的优选实例,并非意图限制本发明的范围,从而应当理解的是,在不偏离本发明的精神和范围的情况下,可以由其获得其他等价方式或改进方式。
在描述之前,应当了解在说明书和所附权利要求中使用的术语,并不应解释为局限于一般及辞典意义,而是应当基于允许发明人为最好的解释而适当定义术语的原则,基于对应于本发明技术层面的意义及概念进行解释。因此,在此的描述仅为说明目的的优选实例,而并非是意指限制本发明的范围,因而应当了解的是,在不偏离本发明的精神和范围下可以做出其他等同实施和修改。除非特别说明,以下实施例中使用的试剂和仪器均为市售可得产品。
实施例1:滚齿刀表面CrN/CrTiBN硬质涂层的制备
所述滚齿刀基材为用于加工外啮合直齿和斜齿圆柱齿轮。
步骤1)基材前处理:将滚齿刀放入清洗线超声槽依次进行除油、除锈等工序,进行粗洗;然后粗洗后对滚齿刀进行去毛刺,完成后进行喷砂处理;最后将滚齿刀放入清洗线进行超声精洗,并烘干30min。
步骤2)将滚齿刀固定在转架上,以3维方式转动,等炉腔真空度达到8.0×10-3Pa,温度达到400℃时,开始运行PVD涂层处理。
步骤3)通入氩气辉光40min后打开Cr靶进行Cr轰击;30min后通入氮气进行CrN层沉积,涂层时间15min,厚度0.33μm。
步骤4)打开Ti靶5min后再开B靶并保持Cr靶开启状态,沉积CrTiBN层45min,预计厚度2.8μm。
所述步骤3)工艺参数为:工艺参数为:真空度1.5Pa,氩气输入量20~25,氮气输入量240~250,偏压150V;步骤4)工艺参数为:真空度1.6Pa,氩气输入量7~10,氮气输入量260~270,偏压110V,温度380℃。
获得涂层硬度为65.7GPa,涂层厚度3.13μm。1000℃下切削操作条件下,滚齿刀使用寿命提高4.17倍。
实施例2:铝压铸模具表面CrN/CrTiBN硬质涂层的制备
基材为铝压铸模具,模具基材H13为钢,经热处理和离子氮化,工作温度600℃。
除了将步骤3)和4)按顺序重复一次以外,按照实施例1相同的方式在基材为铝压铸模具表面上形成CrN/CrTiBN硬质涂层。
获得涂层硬度为63.1GPa,涂层厚度6.5μm。
对比实施例1
除了不形成CrTiBN层以外,按照实施例1相同的方式在滚齿刀表面仅形成CrN涂层。获得涂层硬度为35.2GPa,1000℃下切削操作条件下,滚齿刀使用寿命提高1.32倍。
对比实施例2
除了不形成CrN层以外,按照实施例1相同的方式在滚齿刀表面仅形成CrTiBN涂层。获得涂层硬度为40.2GPa,1000℃下切削操作条件下,滚齿刀使用寿命提高1.89倍。
对比实施例3
按照现有技术CN105839054A中记载的方法,在滚齿刀表面形成CrAlTiSiN涂层,所述涂层厚度为3.5μm。获得涂层硬度为40.8GPa,1000℃下切削操作条件下,滚齿刀使用寿命提高2.37倍。
从实施例1和2与对比实施例1至3的实验数据可以看出,本发明的包含CrN/CrTiBN层的涂层可以有效地提高产品硬度,并显著提高产品使用寿命。
Claims (10)
1.一种用于切削刀具表面用多元复合纳米硬质涂层,所述涂层包括至少两层CrN和CrTiBN,其中CrN层的Cr与N的原子百分比为60:40至70:30,CrTiBN层中各原子的百分比为Cr 10-25%、Ti 8-30%、B 14-29%、N 30-60%。
2.根据权利要求1所述的多元复合纳米硬质涂层,其特征在于,所述CrN层的Cr与N的原子百分比为67:36,CrTiBN层中各原子的百分比为Cr20%、Ti19%、B19%和N42%。
3.根据权利要求1所述的多元复合纳米硬质涂层,其特征在于,所述涂层包括2-200层CrN和CrTiBN层,优选为4-50层,更优选为2-4层。
4.根据权利要求1所述的多元复合纳米硬质涂层,其特征在于,所述CrN层和CrTiBN层交替排列。
5.根据权利要求1所述的多元复合纳米硬质涂层,其特征在于,最内层为CrN层,最外层为CrTiBN层。
6.根据权利要求1所述的多元复合纳米硬质涂层,其特征在于,所述涂层中CrN层厚度为0.3~0.35μm和CrTiBN层厚度为2.5~3μm。
7.根据权利要求1所述的多元复合纳米硬质涂层,其特征在于,所述CrN层厚度为0.33μm和CrTiBN层厚度为2.8μm。
8.根据权利要求1所述的多元复合纳米硬质涂层,其特征在于,包括所述CrN层和CrTiBN层的涂层的总厚度约为3~8μm。
9.一种多元复合纳米硬质涂层的制备方法,所述制备方法包括以下步骤:
步骤1)基材前处理:将基材放入清洗线超声槽依次进行除油、除锈等工序,进行粗洗;然后粗洗后对基材进行去毛刺,完成后进行喷砂处理;最后将基材放入清洗线进行超声精洗,并烘干30min;
步骤2)将基材固定在转架上,以3维方式转动,等炉腔真空度达到8.0×10-3Pa,温度达到400℃时,开始运行PVD涂层处理;
步骤3)通入氩气辉光40min后打开Cr靶进行Cr轰击;30min后通入氮气进行CrN层沉积,涂层时间10至20min,预计厚度0.3~0.35μm;
步骤4)打开Ti靶5min后再开B靶并保持Cr靶开启状态,沉积CrTiBN层40至60min,预计厚度2.5~3μm。
10.根据权利要求9所述的制备方法,其特征在于,所述步骤3)和步骤4)可以交替进行多次,以交替形成多层CrN层和CrTiBN层;
所述步骤3)工艺参数为:真空度1.5Pa,氩气输入量20~25,氮气输入量240~250,偏压150V,温度380℃;
步骤4)工艺参数为:真空度1.6Pa,氩气输入量7~10,氮气输入量260~270,偏压110V,温度380℃。
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