CN104884668B - 用于切削工具的多层薄膜以及包含其的切削工具 - Google Patents
用于切削工具的多层薄膜以及包含其的切削工具 Download PDFInfo
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Abstract
本发明涉及一种用于切削工具的多层薄膜，其中包括总共四个薄层的单元膜被堆叠至少两次，以通过控制四个薄层之间的弹性模量和晶格常数的周期来实现与现存的多层薄膜相比增强的物理性质。在用于切削工具的多层薄膜中，根据本发明，包括薄层A、薄层B、薄层C和薄层D并以此顺序堆叠的单元薄膜被堆叠至少两次，其中，薄膜之间的弹性模量(k)是kA、kC>kB、kD，或kB、kD>kC、kA，并且薄膜之间的晶格常数(L)是LA>LB、LD>LC或LC>LB、LD>LA。
Description
技术领域
本公开涉及一种用于切削工具的多层薄膜，并且更具体地，涉及一种用于切削工具的多层薄膜，其中每个具有几纳米到几十纳米厚度的超晶格薄膜以A-B-C-D或A-B-C-B的形式被堆叠，其能够实现较小的质量变化和优异的耐磨性。
背景技术
从二十世纪八十年代，为了开发用于具有高硬度的切削工具的材料，已经提出了各种基于TiN的多层膜系统。
例如，通过交替地和重复地堆叠TiN或VN形成的几纳米厚度的多层膜提供了由在层之间具有与每个单层的晶格参数的差异无关的、带有共格界面的单晶格参数的所谓的超晶格形成的涂层，并且在这种情况下，与一般的每个单层的硬度相比，能够实现两倍或更高的硬度。因此，已经有将这种现象应用于用于切削工具的薄膜的各种尝试。
在这些超晶格涂层中改善的物理性质的原理已经被描述为强化机制(诸如，Koehler模型、Hall-Petch关系、以及共格应变模型)。通过控制A和B之间的晶格参数的差异、A和B之间的弹性模量的差异、或根据A和B材料交替沉积的堆叠期间，实现了这些强化机制。
通常，很难通过两种材料的交替堆叠应用两个或更多的强化机制的机制。具体地，在多个批次之间以及一批中的多层薄膜的堆叠期间具有严重偏差的批量生产条件下，难以制造出具有优异的耐磨性、具有均匀质量的多层薄膜。
因此，在通过交替堆叠如美国专利第5,700,551号所公开的两种或更多种材料的多层薄膜的形成中，照惯例常见的是，如图1所示，层被堆叠使得在弹性周期(实线)和晶格周期(虚线)彼此一致。然而，在这种情况下，很难同时利用上述各种强化机制，使得在改善多层薄膜的耐磨性上存在限制。
此外，组成通过交替堆叠形成的多层薄膜的每个薄膜通常具有非常小的大约几纳米到几十纳米的厚度，当这样形成的多层薄膜被长时间暴露于在切割期间产生的高温环境中时，使得在相邻薄膜之间也存在局限性，其在于通过构成薄膜的部件的相互扩散，多层薄膜的物理性质被恶化。
发明内容
技术问题
本公开的目的是在由超晶格形成的多层薄膜的形成中提供一种用于切削工具的多层薄膜，该多层薄膜通过调整多层薄膜的晶格周期和弹性周期具有与传统的超晶格涂层相比改进的耐磨性，使得两种或多种薄膜强化机制对多层薄膜起作用；以及提供一种涂有该多层薄膜的切削工具。
本发明的另一个目的是提供一种多层薄膜，其中，构成多层薄膜的薄层间的相互扩散被阻止，并且多层薄膜的强化效果与传统方法相比可以因此持续很长时间；以及提供一种涂有多层薄膜的切削工具。
技术方案
为了解决上述技术问题，本公开提供一种用于切削工具的多层薄膜，其中，各自以薄层A、B、C和D顺序地堆叠的单元薄膜被堆叠一次以上，其中薄层之间的弹性模量k满足关系kA、kC>kB、kD或kB、kD>kC、kA，以及薄层之间的晶格参数L满足关系LA>LB、LD>LC或LC>LB、LD>LA。
在根据本公开的多层薄膜中，优选的是，晶格参数L的最大值和最小值之间的差异为20％或更小。
在根据本公开的多层薄膜中，薄层B和D的组成元素可以与邻近于薄层B和D的薄层A和C的组成元素相同，或可以包括薄层A和C的组成元素中的至少一种。
在根据本公开的多层薄膜中，多层薄膜的平均晶格周期λL可以是它的平均弹性周期λk的两倍大。
在根据本公开的多层薄膜中，单元薄膜可以具有4nm至50nm的厚度。
在根据本公开的多层薄膜中，薄层B和D可以由相同材料形成。
此外，本公开提供了一种包括该多层薄膜的切削工具。
有益效果
通过控制构成多层薄膜的薄层之间的晶格参数的差异以及根据本公开的弹性模量的差异形成的多层薄膜可以同时满足用于强化薄膜的强化条件(诸如，弹性模量的大的差异、单元薄膜间的晶格参数的差异的最小化、以及各层之间的热膨胀系数的差异的最小化)，使得因此形成的多层薄膜还可以具有改进的物理性质。
此外，根据本公开的多层薄膜使薄层之间的组成差异最小化，并且因此阻止了层之间的相互扩散，由此即使是在高温下的切割环境中也可有利地保持多层薄膜的物理性质很长时间。
此外，根据本公开的多层薄膜通过应用两个或多个强化机制具有改进的物理性质，使得即使批次之间具有较大的薄膜厚度的差异，质量变化也是小的。因此，多层薄膜在生产率方面也是有利的。
附图说明
图1示出了传统的超晶格多层薄膜中的弹性周期和晶格周期之间的关系。
图2示出了在根据本公开的超晶格多层薄膜中的弹性周期和晶格周期之间的关系。
图3示出了根据本公开的多层薄膜中的薄层间的组成差异。
图4是示出了根据基于(Ti1-xAlx)N的薄膜中铝含量的晶格参数的变化的曲线图。
图5是示出了根据本公开的示例1的多层薄膜和根据比较例的多层薄膜的车削性能测试结果的照片。
图6是示出了根据本公开的示例1的多层薄膜和根据比较例的多层薄膜的铣削性能测试结果的照片。
图7是示出了根据本公开的示例2的多层薄膜和根据比较例的多层薄膜的切削性能测试结果的照片。
具体实施方式
在下文中，将基于其示例性实施方式详细描述本公开，但是本发明构思不限于下面的实施方式。
本发明人发现，当弹性周期和晶格周期在单元薄膜的堆叠中被调整为彼此不同而不是使两个周期彼此一致时，两个或多个强化机制(即，Koehler模型机制和Hall-Petch关系机制)可以有效地起作用，特别是在层压超晶格薄膜上，并且因此改善了多层薄膜的耐磨性，并且在与单个强化机制主要起作用于其上的多层薄膜相比的大批量生产中也减小了质量变化，并且最终完成了本发明。
根据本公开的多层薄膜是多层薄膜，其中，各自以薄层A、B、C和D顺序地堆叠的单元薄膜被堆叠一次以上，其中，薄层之间的弹性模量k满足关系kA、kC>kB、kD或kB、kD>kC、kA，并且薄层之间的晶格参数L满足关系LA>LB、LD>LC或LC>LB、LD>LA。
图2示出了根据本公开的超晶格多层薄膜中弹性周期和晶格周期之间的关系的示例。如图2所示，可以看出，根据本公开的超晶格多层薄膜与图1的不同之处在于，弹性周期(实线)大约是晶格周期(虚线)的两倍大，并且弹性周期和晶格周期因此彼此不一致。
在与弹性模量相关的Koehler模型中，描述了当薄膜A和B的厚度变得足够小以至小于或等于对应于大约100个原子层的厚度的20纳米至30纳米时产生的强化效应，这是一种难以产生位错的临界厚度。另一方面，在Hall-petch模型中，其描述了由于晶格参数的差异区分的材料周期，描述了在较低的水平(即，几纳米)产生的强化效应。本发明的概念是弹性周期和晶格周期被调整为相互不一致，使得可以产生两种强化效果。
而且，当晶格参数L的最大值和最小值之差大于20％时，难以形成超晶格。因此，优选的是，调整晶格参数，使得如果可能的话产生的差值在20％或更小的范围内。
根据本公开的多层薄膜目的在于单元薄膜由四层形成，并且每个单元薄膜中的堆叠可以被配置为顺序A-B-C-D或A-B-C-B。也就是说，第二层和第四层可以由不同的材料或相同的材料形成。
此外，平均弹性周期和平均晶格周期之间的差值落在本发明的范围内，并且优选地，平均弹性周期可以是平均晶格周期的两倍大。
如图3A所示，当堆叠的薄层之间的浓度梯度(A层–C层)很大时，引起扩散的驱动力增加，使得在长时间暴露于较高温下的切割环境中的相互扩散的可能性变得更高。另一方面，如图3B所示，当堆叠的薄层之间的浓度梯度(A层-B层、B层-C层)很小时，引起扩散的驱动力减小，并且因此相互扩散也可以被延迟。
因此，为了尽可能多的减少相邻堆叠的薄层之间的组分差异，在根据本公开的多层薄膜中，薄层B和D的构成元素可以与邻近于薄层B和D的薄层A和C的构成元素相同，或者可以包括薄层A和C的构成元素中的至少一种。
[示例1]
在超晶格多层薄膜的形成之前，在该多层薄膜中，每一个是由四层薄层形成的单元薄膜被重复地堆叠至两层或更多层，单层薄膜被沉积，并且为了确定每个薄层的弹性模量，测量了组成单元薄膜的每个薄层的弹性模量。结果如表1所示。
作为物理汽相沉积(PVD)方法中的一种方法的电弧离子镀被用于单元薄膜的沉积。初始真空压强降至8.5*10-5Torr或更低，然后注入N2作为反应气体，并且在反应气体压强为40mTorr或更小(优选为10至35mTorr)、温度为400℃～600℃、以及衬底偏压为-30V至-150V的条件下进行沉积。
[表1]
| 薄膜 | 目标成分(at％) | 弹性模量(GPa) |
| TiN | Ti＝99.9 | 416 |
| TiAlN | Ti:Al＝75:25 | 422 |
| TiAlN | Ti:Al＝50:50 | 430 |
| AlTiN | Ti:Al＝33:67 | 398 |
| TiAlCrN | Ti:Al:Cr＝28:67:5 | 404 |
| TiAlSiN | Ti:Al:Si＝35:63:2 | 374 |
| TiCrN | Ti:Cr＝90:10 | 421 |
| TiSiN | Ti:Si＝95:5 | 382 |
| TiVN | Ti:V＝95:5 | 412 |
| TiNbN | Ti:Nb＝95:5 | 406 |
| TiZrN | Ti:Zr＝95:5 | 377 |
| CrN | Cr＝99.9 | 475 |
| CrAlN | Cr:Al＝50:50 | 367 |
| AlCrN | Cr:Al＝30:70 | 403 |
| AlCrSiN | Cr:Al:Si＝30:65:5 | 338 |
可以使用XRD分析跟随单层薄膜的形成获得构成多层薄膜的每个单元薄膜的晶格参数，但是在本公开的实施方式中，使用现有的实验和从理论获得的原子的、离子的和共价半径确定每个单元薄膜的晶格参数。具体地，通过根据原子比定量地应用共价半径到B1立方结构来计算晶格参数。
如图4所示，在基于(Ti1-xAlx)N的薄膜的情况下，晶格参数倾向于随着铝含量增加而近似地线性降低，并且因此可以通过下面的公式1获得基于(Ti1-xAlx)N的薄膜的晶格参数。
[等式1]
晶格参数：a＝4.24-0.125x(x是铝的摩尔比率)。
在本公开的示例1中，由根据本公开的方法形成的基于TiAlN的多层薄膜与由传统方法形成的基于TiAlN的多层薄膜进行比较。作为物理汽相沉积(PVD)方法中的一种方法的电弧离子镀被用于沉积。初始真空压强降至4mPa或更小，在具有-600V的基板上执行离子清洗。N2作为反应气体被注射，并且Ar和Kr被用作惰性气体。沉积压强为500mPa～700mPa，并且为了控制堆叠周期，表格的阴极功率和转速分别被调整为2000W至14000W和0.5RPM至3RPM。在腔室的内部温度为400℃～600℃以及基板偏压为-60V至-150V的条件下执行沉积。
如下表2所示设定多层薄膜的堆叠结构和组成成分。每个由四层薄层组成的单元薄膜被重复地堆叠总共200次，使得由四层薄层形成的单元薄膜的周期为10nm～20nm，并且因此获得具有最终膜厚度为2.5μm至3.5μm的多层薄膜。在这种情况下，可从Korloy得到的P30级A30材料(型号：SPKN1504EDSR-SM)被用作用于铣削的基板，并且可从Korloy得到的M30级PP9030材料(型号：CNMG120408-HS)被用作用于车削的基板。
[表2]
通过铣削和车削的方式进行如上沉积的多层薄膜的切削性能评估。在铣削测试中，SKD11(宽度：100mm、长度：300mm)被用作工件，并且在切削速度是250m/min、每齿进给量0.2mm/tooth、以及进料2mm的干燥条件下进行切削。通过在加工为900mm之后比较磨损状况来评估铣削性能。结果被示于图5中。
如图5所示，可以看到，在SKD11的加工期间磨损主要如月牙洼磨损(crater wear)的方式进行，并且可以确认的是，对比于比较例1-10至1-12，示例1-1至1-9中的月牙洼磨损性能被提高。
在车削测试中，STS316被用作工件，并且在切削速度为200m/min、每齿进给量0.25mm/tooth、进料1.5mm的潮湿条件下进行切削。通过在连续加工3分钟之后比较磨损状况来评估车削性能。结果被示于图6中。
如图6所示，可以看到，在STS316的加工期间磨损主要如月牙洼磨损的方式进行，并且可以确认的是，对比于比较例1-10至1-12，示例1-1至1-9中的月牙洼磨损性能被提高。
优选实施例
[示例2]
在本公开的示例2中，将由根据本公开的方法形成的基于AlCrN的多层薄膜与由传统方法形成的基于AlCrN的多层薄膜进行对比。
如下表3所示设定多层薄膜的堆叠结构和组成成分。各自由四层薄层组成的单元薄膜被重复地堆叠总共180次，使得平均晶格周期为5nm至10nm，并且弹性周期是10nm至20nm，并且因此获得具有最终膜厚度为2.5μm至3.5μm的多层薄膜。在这种情况下，可以从Korloy得到的M30级PP9030材料(型号：CNMG120408-HS)被用作其上沉积有多层薄膜的基板。
[表3]
在如上沉积的多层薄膜的切削性能评估中，SM45C(直径：100mm，高度：120mm)被用作工件，并且在切削速度250m/min、每齿进给量0.25mm/tooth、以及进料1.5mm的干燥条件下进行切削。在加工端面30次之后比较磨损状况。结果被示于图7中。
如图7所示，对比于比较例2-3，本公开的示例2-1和2-2示出了改进的月牙洼磨损形式。
换句话说，可以看出，通过控制根据本公开的弹性周期和晶格周期堆叠的超晶格多层薄膜表现出与其它情况下相比改善的耐磨性。
工业适用性
根据本公开的多层薄膜可以被适当地用作用于切削工具的膜。
Claims (7)
1.一种用于切削工具的多层薄膜，其中，所述薄膜是通过各自以薄层A、B、C和D顺序地堆叠的单元薄膜被重复地堆叠两层或更多层而形成的，
其中，所述薄层之间的弹性模量k满足关系kA、kC>kB、kD，或kB、kD>kC、kA，并且
所述薄层之间的晶格参数L满足关系LA>LB、LD>LC或LC>LB、LD>LA，
其中，所述薄层A为CrN，或者所述薄层A为CrSiN，且所述薄层B、C和D为AlCrN。
2.根据权利要求1所述的多层薄膜，其中，所述晶格参数L的最大值和最小值之间的差是20％或更小。
3.根据权利要求1所述的多层薄膜，其中，所述薄层B和所述薄层D的构成元素与邻近于所述薄层B和所述薄层D的所述薄层A和所述薄层C的构成元素相同，或包括所述薄层A和所述薄层C的所述构成元素中的至少一种。
4.根据权利要求1所述的多层薄膜，其中，所述多层薄膜的平均晶格周期λL是所述多层薄膜的平均弹性周期λk的两倍大。
5.根据权利要求1或2所述的多层薄膜，其中，所述单元薄膜具有4nm至50nm的厚度。
6.根据权利要求1或2所述的多层薄膜，其中，所述薄层B和所述薄层D由相同材料形成。
7.一种涂有根据权利要求1或2所述的多层薄膜的切削工具。
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- 2012-12-27 KR KR1020120155125A patent/KR101471257B1/ko active IP Right Grant
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2013
- 2013-05-21 CN CN201380068331.2A patent/CN104884668B/zh active Active
- 2013-05-21 US US14/653,266 patent/US20150337459A1/en not_active Abandoned
- 2013-05-21 DE DE112013006267.4T patent/DE112013006267T5/de not_active Ceased
- 2013-05-21 WO PCT/KR2013/004426 patent/WO2014104495A1/ko active Application Filing
- 2013-05-21 RU RU2015130314A patent/RU2613258C2/ru active
- 2013-11-14 CN CN201380068184.9A patent/CN104870684B/zh active Active
- 2013-11-14 DE DE112013006240.2T patent/DE112013006240B4/de active Active
- 2013-11-14 WO PCT/KR2013/010334 patent/WO2014104573A1/ko active Application Filing
- 2013-11-14 US US14/649,551 patent/US20150307998A1/en not_active Abandoned
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| CN1587434A (zh) * | 2004-08-05 | 2005-03-02 | 上海交通大学 | TiN/SiO2纳米多层膜及其制备方法 |
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2014104573A1 (ko) | 2014-07-03 |
| WO2014104495A1 (ko) | 2014-07-03 |
| DE112013006267T5 (de) | 2015-09-24 |
| CN104870684B (zh) | 2017-09-08 |
| RU2015130314A (ru) | 2017-01-31 |
| DE112013006240T5 (de) | 2015-10-08 |
| DE112013006240B4 (de) | 2023-06-29 |
| US20150337459A1 (en) | 2015-11-26 |
| KR20140085016A (ko) | 2014-07-07 |
| KR101471257B1 (ko) | 2014-12-09 |
| US20150307998A1 (en) | 2015-10-29 |
| CN104870684A (zh) | 2015-08-26 |
| RU2613258C2 (ru) | 2017-03-15 |
| CN104884668A (zh) | 2015-09-02 |
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