CN103958738B - 用于在加工操作中增强耐磨性的适应形态的铝钛氮化物涂层和其方法 - Google Patents

用于在加工操作中增强耐磨性的适应形态的铝钛氮化物涂层和其方法 Download PDF

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CN103958738B
CN103958738B CN201280057376.5A CN201280057376A CN103958738B CN 103958738 B CN103958738 B CN 103958738B CN 201280057376 A CN201280057376 A CN 201280057376A CN 103958738 B CN103958738 B CN 103958738B
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D.库拉波夫
S.克拉斯尼策尔
M.阿恩特
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Abstract

本发明涉及(Al,Ti)N涂层，其显示具有至少两个不同涂层部分A和B，具有纳米数量级的颗粒大小，其特征在于所述涂层部分A显示具有比所述涂层部分B更大的颗粒大小和更高的弹性模量。本发明还涉及一种用于用上述涂层涂布基底的方法，从而借助于PVD技术沉积所述(Al,Ti)N涂层的至少所述涂层部分A和/或所述涂层部分B。

Description

用于在加工操作中增强耐磨性的适应形态的铝钛氮化物涂层 和其方法
本发明涉及一种铝钛氮化物((Al,Ti)N)涂层***和一种在基底表面上沉积其的方法。更具体地讲，本发明涉及一种具有调整的形态并且在加工操作中展现增强的切削性能的铝钛氮化物涂层。
包含铝钛氮化物的薄涂层常常用于在加工操作中获得切削工具的高性能。众所周知这种涂层的研发始于1980年。随后已完成通过切削操作改善铝钛氮化物涂层的性能的更多尝试。在许多情况下，据报道，通过在单层涂层***(如(Al,Ti,Si)N)中添加其他元素或通过在多层涂层***(如(Al,Ti)N/Al2O3)中与其他涂层材料组合，有可能显著改善AlTiN基涂层的温度稳定性、抗氧化性和耐磨性。通过研发AlTiN基涂层而广泛研究的其他重要方面是涂层结晶度、颗粒大小、元素组成、结构等的影响。
例如，WO2011041063的作者报道，当这些涂层具有约0至15重量%的六方相和(Alx,Ti1-x)N的元素组成，其中x在约0.53至约0.58摩尔范围内时，铝钛氮化物涂层可展现对用于端铣的烧结碳化钨切削工具意外良好的加工性质。它们还表明，这些涂层优选具有在约10至约40纳米范围内的平均颗粒大小，展现具有由X射线衍射表征的晶体学织构的立体相并且具有在约4.5至约10范围内的(200)与(111)峰强度比。
JP2644710的作者报道，具有元素组成(AlxTi1-x)N并且0.56≤x≤0.70的氮化铝涂层同时展现高硬度耐磨性和优良高温氧化性。
WO2011034492的作者报道AlTiN涂层切削工具的改善的切削性能或更长工具寿命，其中通过在反应性PVD电弧沉积期间在氮气气氛中从Ti0.33Al0.67和Ti0.30和Al0.70靶标顺序地改变基底偏压来沉积铝钛氮化物涂层。根据WO2011034492的沉积方法包含在涂布沉积期间改变基底偏压的至少一个次序(维持积极靶标)，其中改变基底偏压的次序包含子次序Si。如下调整或改变子次序Si期间的基底偏压：a)调整第一基底偏压Bi并维持10秒至60分钟的沉积时间Ti，b)在10秒至40分钟的斜坡时间Ri期间，逐渐将基底偏压改变至第二基底偏压Bi+1，其中|Bi-Bi+1|≥10 V。重复子次序Si，直至i = n，其中I = 0、1、2 ...n，其中n≥2，并且其中各新子次序在结束先前子次序时所用相同基底偏压下开始。
然而，尽管对该主题进行了大量研发工作，加工操作中改善切削性能的需要仍驱使对铝钛氮化物涂层的性质和沉积方法更广泛的研究。
本发明的目的
本发明的目的提供用于高性能切削工具的铝钛氮化物涂层***、特别是用于切削插件的宽带涂层，其允许比现有技术水平更高的生产率。此外，本发明的目的为提供一种用于制造所述高性能涂布工具的工业适用涂布方法。另外，根据本发明的涂布方法应该尽可能稳健并且不复杂。
发明描述
本发明通过提供具有调整的形态的铝钛氮化物涂层***和其涂层沉积方法实现上述目的，所述涂层***和方法均特别设计用于改善高性能切削工具的效率。
根据本发明的(Ti,Al)N涂层是显示具有两个不同的区域或涂层部分A和B的单层涂层，其主要特征在于不同的形态结构。
发明人意外地发现，当该涂层部分A显示具有基本上更明显柱状形态结构和比涂层部分B更大的颗粒大小时，(Ti,Al)N涂层的切削性能可以显著改善。
此外，通过根据本发明制备的在涂层部分A和B中的颗粒大小均为纳米数量级的(Ti,Al)N涂层，获得更好的切削性能。
在本发明的一个优选实施方案中，涂层部分A中的颗粒大小gzA为涂层部分B中的颗粒大小gzB的至少1.25倍，优选gzA≥1.5 gzB，更优选10 gzB≥gzA≥1.5 gzB，还更优选4gzB≥gzA≥1.8 gzB。在本发明的又一实施方案中，涂层部分A的涂层厚度thA小于涂层部分B的涂层厚度thB：thA＜thB。优选1.2 thA≤thB≤8 thA。更优选1.5 thA≤thB≤3 thA。
在本发明的其他实施方案中，使用粉末冶金合金TiAl-靶标作为源材料，通过阴极电弧蒸发产生(Ti,Al)N涂层。优选地，靶标中的原子元素组成为TixAl1-x，其中0.30≤x≤0.70。
在本发明的又一优选实施方案中，在涂层沉积期间改变靶标表面上的磁场构造以便影响去往阳极表面的电子轨线，并因此影响等离子体中的电子温度和涂布腔室中的反应气体的电离等级。根据本发明的这一优选实施方案，在涂层沉积期间强烈影响反应气体的电子温度和电离等级，以便在(Ti,Al)N涂层中获得不同的所需形态结构A和B。
在本发明的其他优选实施方案中，在(Al,Ti)N涂层的沉积期间，维持反应气体的电子温度和电离等级尽可能地低。
不同切削工具用根据本发明沉积的(Al,Ti)N涂层的不同变型来涂布，并且可能通过切削测试来验证用根据本发明的(Al,Ti)N涂层涂布的切削工具的切削性能的显著改善。具体地讲，获得弧坑磨损的显著减少和工具寿命的显著增加。
以下一些实验程序和结果将作为本发明的实施方式的实例来说明：
借助于电弧离子电镀沉积技术将(Al,Ti)N涂层沉积在切削插件上。将具有Al0.55Ti0.45、Al0.6Ti0.4、Al0.67Ti0.33和Al0.7T10.3的元素组成的靶标用作在反应性氮气氛中沉积(Al,Ti)N涂层的材料源。使用在序列号61/357272的美国专利文件中Krassnitzer等人推荐类型的电弧蒸发器，蒸发靶标材料。这种类型的电弧蒸发器包含阴极(靶标)、阳极和允许将磁场的流线引向紧邻阴极布置的阳极的磁装置。反应气体的电子温度和电离等级（此情况下为涂布腔室中氮气的电离等级）被影响，以便通过调整线圈电流的恰当值来产生不同涂层部分A和B。涂层部分A沉积在基底上，并且涂层部分B沉积在涂层部分A上。在一些情况下，夹层沉积在基底和涂层部分A之间。一般来讲，用于沉积涂层部分A的线圈电流和基底偏压的所用值ccA和sbvA高于用于沉积涂层部分B的对应所用值ccB和sbvB，因此ccA > ccB并且sbvA > sbvB。
在部分A和B的各自对应的沉积开始时，不使用斜坡，分别调整ccA和sbvA值以及ccB和sbvB值，并随后分别维持恒定，直至涂层部分A和B的各对应沉积时间完成。所用线圈电流在0 A至2 A之间变化。
此外，使用以下分析技术之等，分析对应于上述实例的根据本发明的沉积涂层：能量分散X-射线光谱学(EDX)；扫描电子显微术(SEM)、X射线衍射(XRD)和纳米刻痕方法。
基本上，沉积涂层的部分A和B均显示具有面心立方体结晶结构和主要(200)晶体学织构。一般来讲，在涂层部分A中观察到的柱状结构比在涂层部分B中更明显。此外，与涂层部分B相比，在涂层部分A中观察到增加的颗粒大小、硬度和弹性模量。颗粒大小值为纳米数量级。特别地，在具有5 nm至50 nm的颗粒大小的涂层中观察到良好切削性能。硬度值在37 GPa至55 GPa之间变化。弹性模量值在410 GPa至450 GPa之间变化。与钛有关的铝原子百分比分数以及涂层部分A中测得的压缩应力一般略低于涂层部分B中测得那些。
使用用根据本发明沉积的(Al,Ti)N涂层涂布的切削插件进行铣削和车削测试的切削性能结果示于附图1和2。与其他4种不同的商业确立的(Al,Ti)N涂层相比，所获得的结果显示于图1-2。
此外，经验证，仅含有对应于涂层部分A或涂层部分B的结构的(Al,Ti)N涂层未显示改进的高切削性能。该结果可在图3中观察到。
附图名称：
图1：切削测试1中通过铣削操作来比较切削性能。切削测试1中的测试条件为：
材料：1.4571
工具：碳化物***物ADKT 1505
切削参数：Vc=125m/min, fz=0.15mm, ap=4mm, ae=35mm
操作：端面铣削/干燥
图2：切削测试2中通过车削操作来比较切削性能。切削测试2中的测试条件为：
材料：1.4571
工具：CNMG432
切削参数：Vc=180m/min, fz=0.25mm, ap=2mm
操作：湿法切削/外部车削
标准：Vbmax≥205 μm
图3：切削测试3中通过车削操作来比较切削性能。切削测试3中的测试条件为：
材料：1.2344 45 HRC
工具：端铣刀ϕ 10mm
切削参数：Vc=180m/min, fz=0.1mm, ap=10mm, ae=0.5mm
操作：湿法切削/精磨
标准：Vbmax≥100 μm
在本发明的背景下，名称(Ti,Al)N涂层和(Al,Ti)N涂层具有相同含义并因此无差别地被使用。
涂布方法常用的电弧蒸发器包括阴极，但不包括特定阳极，因为阳极由涂布腔室壁构成。为此，阴极处生成的更多电子必须穿越等离子体，以便达到阳极。为此，更多电子在电弧PVD涂布方法期间到达等离子体。
在本发明的情况下，如上文所提及，用于制备(Al,Ti)N涂层的电弧蒸发器具有特殊构造，其中阳极放置于阴极的周围并且磁场构造还有助于使绝大多数电子从阴极向阳极偏移，避免电子在电弧PVD方法期间到达等离子体。使得阴极处生成的较少数量的电子能到达等离子体，并因此可能在(Al.Ti)N涂层的沉积期间，尽可能低地维持等离子体中反应气体的电子温度和电离等级，如上文提及的本发明的优选实施方案之一中所述。
由于所用电弧蒸发器具有允许将电子从阴极向紧邻阴极布置的阳极偏移的构造，有可能通过调整线圈电流和基底偏压来生成用于根据本发明形成具有部分A和B的涂层所必需的加工条件。越高的线圈电流值伴有电子从阴极向阳极的越高偏移。
所施加基底偏压sbvA和sbvB在-30 V至-200 V之间变化，并且sbvA > sbvB。
根据所实现的实验，如果对于沉积(Al,Ti)N涂层的涂层部分A，所施加基底偏压不低于-150 V (sbvA不具有比-150 V更低负值)，并且对于沉积(Al,Ti)N涂层的涂层部分A，所施加基底偏压不低于-200 V (sbvB不具有比-200 V更低负值)，则根据本发明涂布的切削工具显示特别良好的切削性能。换句话讲，如果在涂层部分A的沉积期间施加于基底的偏压的绝对值低于在涂层部分B沉积期间所施加偏压的绝对值，则可以根据本发明获得极良好切削性能。
特别地，粉末冶金技术制得的靶标可用于涂层沉积，但由其他技术制得的复合靶标或合金靶标也可以使用。
如果有必要改善涂层的内聚性，则其可能推荐的是在各自涂层部分A和B的沉积开始时逐渐调整涂层参数如线圈电流和/或偏压(如通过使用斜坡)。
在大部分情况下，当涂层部分A和B的颗粒大小均低于30 nm时，根据本发明涂布的烧结碳化物切削工具显示具有特别良好的切削性能。特别地，在一些情况下，当涂层部分A的平均颗粒大小为约20 nm或更小，那么涂层部分B的平均颗粒大小为约10 nm或更小。
同样，如果涂层部分A中的Al原子百分比含量1-xA比涂层部分B中Al原子百分比含量1-XB低大约4 - 10%，则可以通过根据本发明涂布的切削工具获得对于一些应用特别良好的切削性能：
• 如果0.04≤((1-xB) - (1-xA))/(1-xA)≤0.10,
• 更具体地讲，如果0.04≤((1-xB) - (1-xA))/(1-xA)≤0.06
此外，涂层部分A中压缩应力比部分B低至少15%、优选至少低20%的根据本发明沉积涂层提供特别良好的切削性能。
根据本发明的涂层可施加在各种基底上。
特别地，根据本发明的涂层可用于保护将暴露于摩擦接触的表面。
根据本发明的涂层还可以改善暴露于摩擦接触的表面的若干摩擦性质，例如硬度、耐磨性、抗氧化性等。特别地，根据本发明的涂层可用于涂布机元件和工具。
根据本发明的涂层可特别有益于改善切削工具的切削性能。
例如，根据本发明涂布的切削工具的基底可包含或可由钢和/或烧结碳化物、和/或陶瓷、和/或立方氮化硼组成。
根据本发明沉积的(Al,Ti)N涂层的总体涂层厚度优选不小于0.5 μm并且不大于30 μm。

Claims (26)

1.(Al,Ti)N涂层，显示至少两个不同涂层部分A和B，所述涂层部分A和B均显示在纳米范围的颗粒大小的结构，其特征在于，所述涂层部分B沉积在所述涂层部分A上，所述涂层部分A显示比所述涂层部分B更大的颗粒大小和更高的弹性模量，
其中在涂层部分A中测得的与钛相关的铝原子百分比分数和压缩应力的至少一种低于在涂层部分B中测得的相应的与钛相关的铝原子百分比分数和压缩应力之一，
所述涂层部分A中的颗粒大小为5 nm至50 nm，和
所述涂层部分A中的颗粒大小gzA是所述涂层部分B中的颗粒大小gzB的至少1.25倍大。
2.根据权利要求1所述的(Al,Ti)N涂层，其特征在于所述涂层部分A中的颗粒大小为5nm至30 nm。
3.根据权利要求1所述的(Al,Ti)N涂层，其特征在于gzA≥1.5 gzB。
4.根据权利要求1所述的(Al,Ti)N涂层，其特征在于10 gzB≥ gzA ≥ 1.5 gzB。
5.根据权利要求1所述的(Al,Ti)N涂层，其特征在于4 gzB≥ gzA≥ 1.8 gzB。
6.根据权利要求1所述的(Al,Ti)N涂层，其特征在于涂层部分A和B均显示具有面心立方体结晶结构和显著(200)晶体学织构。
7.根据权利要求1所述的(Al,Ti)N涂层，其特征在于所述涂层部分A和B均具有37 GPa至55 GPa的硬度和/或410 GPa至450 GPa的弹性模量。
8.根据权利要求1所述的(Al,Ti)N涂层，其特征在于所述涂层部分A的厚度thA小于所述涂层部分B的涂层厚度thB。
9.根据权利要求8所述的(Al,Ti)N涂层，其特征在于1.2 thA≤thB≤8 thA。
10.根据权利要求8所述的(Al,Ti)N涂层，其特征在于1.5thA≤thB≤3 thA。
11.基底，其至少部分地涂布有根据权利要求1的(Al,Ti)N涂层。
12.根据权利要求11的基底，其特征在于所述基底为工具。
13.根据权利要求11的基底，其特征在于所述基底为切削工具，其包含钢、烧结碳化物、陶瓷和立方氮化硼的至少一种。
14.根据权利要求11的基底，其特征在于所述涂层部分A沉积在基底的表面上。
15.涂布根据权利要求11的基底的方法，其特征在于，至少(Al,Ti)N涂层的涂层部分A和/或涂层部分B是借助于PVD技术来沉积。
16.根据权利要求15所述的方法，其特征在于，至少对于沉积(Al,Ti)N涂层的涂层部分A和/或涂层部分B，使用反应性电弧离子电镀沉积技术，由此将包含钛和铝的至少一个靶标用作源材料，并且对于所述涂层形成，将含氮或基本上含氮的气体用作反应气体。
17.根据权利要求15所述的方法，其特征在于，至少对于沉积(Al,Ti)N涂层的涂层部分A和/或涂层部分B，使用电弧蒸发器，所述电弧蒸发器包含阴极、紧邻阴极布置的阳极和磁装置，其中所述磁装置允许磁场的流线引向阳极。
18.根据权利要求15所述的方法，其特征在于，沉积所述涂层部分A使用的线圈电流值比沉积所述涂层部分B使用的线圈电流值更高。
19.根据权利要求15所述的方法，其特征在于，在待涂布的基底上沉积(Al,Ti)N涂层的涂层部分B施加的偏压比沉积涂层部分A所施加的偏压的负值更低。
20.在基底上沉积涂层的PVD方法，所述涂层具有至少两个不同涂层部分A和B，所述涂层部分A和B具有不同的颗粒大小，所述涂层部分A显示比所述涂层部分B更大的平均颗粒大小，其特征在于，涂层部分A的反应气体的电子温度和电离的至少一种与涂层部分B的反应气体的相应的电子温度和电离的至少一种不同。
21.根据权利要求20所述的PVD方法，其特征在于，所述PVD方法是反应性电弧蒸发PVD方法。
22.根据权利要求21所述的PVD方法，其特征在于，对于沉积涂层部分A和/或沉积涂层部分B，使用至少一个电弧蒸发器，所述电弧蒸发器包含阴极、紧邻阴极布置的阳极和磁装置，其中所述磁装置允许磁场的流线引向阳极。
23.根据权利要求20所述的PVD方法，其特征在于，沉积涂层部分A使用的线圈电流值比沉积所述涂层部分B使用的线圈电流值更高。
24.根据权利要求20所述的PVD方法，其特征在于，待涂布的基底上沉积涂层部分A施加的负偏压比沉积涂层部分B所施加的负偏压的绝对值更低。
25.根据权利要求20所述的PVD方法，其特征在于，使用相同类型的靶材料沉积涂层部分A和涂层部分B，所述靶材料由相同的元素组成，并在原子百分比方面具有相同的化学组成。
26.根据权利要求20所述的PVD方法，其特征在于，沉积涂层部分A和/或涂层部分B使用的至少一个靶标通过粉末冶金技术制得。
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