CN113412344A - 具有包括含硼化物的扩散阻挡层的涂层的涂覆工具 - Google Patents

具有包括含硼化物的扩散阻挡层的涂层的涂覆工具 Download PDF

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CN113412344A
CN113412344A CN202080013015.5A CN202080013015A CN113412344A CN 113412344 A CN113412344 A CN 113412344A CN 202080013015 A CN202080013015 A CN 202080013015A CN 113412344 A CN113412344 A CN 113412344A
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coating
layer
substrate
boride
boron
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哈米德·博瓦蒂
尤尔根·拉姆
米利亚姆·阿恩特
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Oerlikon Surface Solutions AG Pfaeffikon
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Abstract

一种包括涂覆面的涂覆工具，涂覆面包括基材(1)，涂层(2)被沉积在基材所具有的表面上，其中，基材由含钴材料制成，并且其中，该涂层包括至少一个含硼层(20)，而所述至少一个含硼层(20)含有铝，该层所含的硼作为硼化物存在，因此该含硼层(20)能够形成用于提供扩散阻挡层作用的其它层，尤其是当该涂覆工具或涂覆面暴露于约600℃和1200℃之间范围内的温度时，用于阻止钴从基材表面扩散到该涂层。

Description

具有包括含硼化物的扩散阻挡层的涂层的涂覆工具
技术领域
很多工业加工过程都发生在严酷条件如高温下。这种严酷性也因苛求效率提升而被显著加剧。一种用于在这种工作条件下保护工业工具的做法是通过在工具表面上施加薄涂层而将工具与严酷环境分隔。在众多涂覆方法中，物理气相沉积(PVD)技术在学术界和行业中都已获得极大关注并且被公认获得巨大成功。
尽管如此，高温如今仍可能影响施加在工具表面上的涂层以及覆有涂层的工具表面(即覆有涂层的基材表面)。
一个众所周知的例子是涂覆的硬质合金切削刀具。在工具使用期间，尤其在由硬质合金制造或含有硬质合金的工具的情况下，可能发生的是因工具表面暴露在高温下而导致钴向外扩散到涂层中。此外，如果沉积是在高温下和采用高强度等离子体处理来进行的，钴向外扩散到基材表面可能早在沉积过程中已发生。
本发明要解决的问题
尽管采用了涂层，因为基材(如切削刀具的切削刃)在某些应用中(例如在切削含钛材料时)难免会暴露在高温下，故需要能够在涉及暴露于高温的应用中帮助避免基材表面损伤的涂层。
在本发明的上下文中，术语“高温”尤其是指在600℃至1200℃范围内的温度。
发明目的
本发明的主要目的是提供一种涂层，当涂覆的基材表面遇到高温时，涂层有助于抑制从基材表面至涂层的元素扩散。此问题通常可能出现在如下情况下：
1.在正被涂覆的基材表面上的涂层的形成过程中，例如因为在基材表面处由涂层沉积过程中的离子轰击造成的高温，或者
2.在涂覆基材的使用期间，例如因为涂覆的基材表面直接暴露于高温(例如当涂覆基材是要用在产生高温的涡轮机的一部分中的部件时)或涂覆基材间接暴露于高温(例如当高温是因为涂覆工具在机加工过程中与工件发生摩擦接触而产生)。
发明内容
本发明的目的通过提供一种涂覆基材来达成，其包括含钴(Co)的基材1和沉积在基材表面上的涂层2，该涂层包括至少一个含硼层20，其进一步包括铝并且其中硼以硼化物形式存在，其中，所述至少一个含硼层20被直接沉积在含钴基材1的表面上(见图3a)。
发明人观察到了含硼层20所含的硼化物出乎意料地具有抑制钴从含钴基材1扩散到涂层2的性能。
在由含钴材料制造的工具被用在机加工作业中的情况下，例如当采用硬质合金工具时，这种出乎意料的效果尤其对于避免基材损伤和涂层损伤是有用的。
发明人观察到了抑制扩散过程的机理是在基材表面与涂层之间的界面中起效的。
发明人观察到了包含Al-Co和B-Co的金属间相的含钴层21的形成(见图3a)，这至少发生在以下两种情况下：
1.当涂覆过程如此进行时，即，基材表面在涂层沉积过程中达到高温(例如由离子轰击造成)，和
2.当涂覆基材在使用过程中暴露于高温时。
因此可以抑制钴从含钴工件扩散至涂层，因为在基材1和涂层2之间界面中形成金属间相Al-Co和B-Co。
此外，当本发明的涂覆基材在含氧气氛中暴露于高温时，发明人观察到了进一步有利效果。这种进一步效果是在含硼层20上方形成含氧化铝层22(含Al-O层22)(见图3b)。此含Al-O层22阻止氧从所述气氛扩散至涂层中，通过这种方式，当涂覆工具暴露于含氧气氛时，也能够增强涂层在高温下的化学稳定性。
硼化物及其出色的性能是已知的且是现有技术。本发明允许在涉及暴露于高温的应用中，包括在含氧气氛中，使用硼化物涂层(其是很有前途的涂层材料)。这是可行的，因为本发明的涂覆工具通过在涂层和基材的界面处形成金属间化合物而产生更高的热稳定性且同时抑制钴扩散。
例如在使用由AlWB2组成的含硼层20情况下可以形成层21，其包含以下类型的金属间相：Al-Co和/或B-Co(例如AlCo、Al2Co5、Co2B和/或Co3B)。这些位于基材与层20之间的界面中的金属间相，允许涂层余部(如层20)保持完好无损。
此外，硼化物涂层的一个主要弱点是其抗氧化性差。
因此，通过包括铝-硼化物涂层，例如AlWB2，可以形成保护性Al-O层，其抑制氧气从周围气氛中向内扩散到该涂层。
这样一来，还可能的是达到以下效果，即在接触工件时，涂层材料本身也能够实现削弱的扩散，尤其是在工件含有快速扩散元素如钴的情况下。
本发明的涂层对于保护具有含钴基材的工具是特别有利的。
因此，根据本发明的优选实施例，本发明的涂层被沉积，其包括具有抑制钴扩散的性能的含硼化物层20(以下在本发明的上下文中也称为扩散阻挡层)，其中，该扩散阻挡层被直接沉积在该基材上。
发明的进一步说明
将借助一些例子和附图来更详细解释本发明。
附图说明
图1：SEM-EDX元素映射，示出在1100℃退火1小时之后钴从基材(含钴粘结剂的硬质合金工具的刀具)向外扩散到整个涂层范围(含钴岛的TiSiN涂层，所述钴岛是因为钴从硬质合金基材向外扩散而形成的)。
图2：涂覆的硬质合金的SEM横截面图像，其中可清楚看到钴耗区。
图3：在暴露于高温之前(图3a)和在暴露于高温之后(图3b)的本发明的涂覆基材的实施例。
以下说明和例子不应被理解为对本发明的限制。
图1呈现钴(Co)的SEM/EDX元素映射，其是以涂覆的硬质合金基材在1100℃退火60分钟之后的横截面中实现的。扫描电子显微镜(SEM)被用于完成该分析。元素映射是利用SEM的能量色散X射线光谱仪(EDX)探测器来达成的。在硬质合金基材(在此情况下是切削刀具)中的钴粘结剂以及分散在TiSiN涂层中的钴岛可被观察到。TiSiN涂层中的钴岛在退火前不存在。因此，发明人总结出在TiSiN涂层中的钴岛是因为钴在退火过程中扩散遍及涂层所形成的。
在此退火试验中所示出的“向外扩散”表明如下扩散过程，其可以如上所述地在沉积期间以及在涂覆基材使用期间发生。钴的扩散改变涂层化学成分及其性能。因此，钴的向外扩散可能导致弱的涂层工具界面并影响涂层性能，进而导致涂覆工具的使用寿命缩短。
图2在SEM横截面图像中呈现这种界面的例子。该照片显示出在基材表面与涂层之间的界面中的空穴形成，这是由钴向外扩散引起的。另外，可以在涂层的第一部段中看到钴的聚集。机械性能的削弱因此是显见的。
如上所述，在沉积过程中和在涂覆基材工作过程中可能出现或引发扩散过程。在沉积过程中，在PVD过程中的基材温度通常在300℃与600℃之间，即低于600℃至1200℃的温度范围，该温度范围是明确与扩散相关的。但是，沉积过程的特点不仅是中性元素会聚在表面处，还有高能离子的同时轰击。这将在基材的最上层表面产生更高得多的“温度”，并且增强钴原子扩散的迁移能力。在另一情况下，在涂覆基材的工作过程中，与工件接触的涂覆工具表面(例如切削刀具的切削刃)可能变得很热并且可能超过1000℃，例如用于钛合金的机加工。在这些条件下也引起钴扩散。
本发明的第一目的是提供一种涂层，其抑制钴在高温下从基材材料扩散进入涂层。
本发明的另一目的是提供一种涂层，其在室温以及高温下就硬度和杨氏模量而言具有出色的机械性能。
二元和三元Al-B化合物显示出极具吸引力的性能，例如超过50GPa的高硬度，这使之成为有前途的耐磨涂层备选方案，用于在严酷环境中保护切削刀具和部件。
借助PVD的Al-B基涂层的组成在一定程度上是由被用于溅射或阴极电弧蒸发的靶的组成决定的。
根据本发明的一个优选实施例，该涂层或该涂层的至少一部分通过使用PVD(物理气相沉积)溅射技术，优选是非反应性PVD溅射技术来产生，即，仅采用非反应性气体如氩气作为工艺气体。
根据本发明的另一个优选实施例，(用于产生本发明涂覆工具的)涂层或该涂层的至少一部分是通过使用PVD(物理气相沉积)阴极电弧蒸发技术且优选是非反应性PVD阴极电弧蒸发技术来沉积的，即，没有采用工艺气体或仅采用非反应性气体例如氩气作为工艺气体。
根据这些工艺过程中的参数(靶成分和制造；蒸发过程；反应性惰性气体背景气氛；基材偏电压等)，除了元素组成外，Al-B基涂层还能够根据相应的相图含有不同的Al-B相。
此外，本发明的一个重要贡献是防止氧朝着基材/涂层界面和朝着基材扩散，这种扩散引发钴通过涂层向外扩散。因为Al-B基涂层固有地含有与氧反应的Al，故它在涂层表面处以及在氧能够扩散到的区域中形成Al-O，其作为扩散阻挡。
另一方面，在因为氧的缺乏而不存在该机制的区域中，钴扩散也被减弱。在这里，高温引起金属间相Al-Co和B-Co的形成，其减弱钴元素的扩散。
确切说，本发明涉及一种涂层体系，其包括至少一个扩散阻挡层，其中，所述至少一个扩散过渡层是：
-AlB2层或含AlB2的层，或者
-AlWB2层或含AlWB2的层，或者
-由AlB2和AlWB2组成的层或含AlB2和AlWB2的层，或者
-由AlN和AlB2组成的层或含AlN和AlB2的层，或者
-由AlN和AlWB2组成的层或含AlN和AlWB2的层，或者
-过渡金属硼化物(TM硼化物)层或含TM硼化物的层，其中，TM是选自以下组的一种或多种过渡金属：3d、4d和5d元素，该层还含有Al。
在含钴基材与含硼化物层之间的过渡区中，含Al和W的梯度层可以被添加，以在沉积过程中获得改善的附着性并且抑制钴向外扩散至基材表面。
本发明的涂层可以被沉积为显示出包含一个或多个上述扩散阻挡层的整体的或分层的涂层结构。
在涂覆工具暴露于高温的应用范围内，例如在钛铝化合物的切削中，本发明的涂层可被用于涂覆硬质合金工具。
在涂覆工具暴露于高温的应用范围内，这样的应用优选是镍基、钴基或镍钴基超合金的切削，本发明的涂层可被用于涂覆硬质合金工具。
在这些层中优选含有铝，因为铝对于达成对钴向外扩散进入该涂层的抑制是重要的。在这些层中优选存在硼化物化合物，因为硼化物化合物可能对于提供出色的性能例如出色的硬度，尤其是超过35GPa的硬度是至关重要的，这在不同的操作中，例如在不同的切削工具应用中是极其重要的性能。
通过阻止钴向外扩散到涂层中，保证了本发明的这些涂层在高温应用过程中保持完好无损的独特性能。
在本发明的上下文中，二元硼化物和三元硼化物可以例如通过非反应性物理气相沉积(PVD)溅射技术来合成，其中，仅采用氩气作为工艺气体。二元硼化物靶在氩气氛下被溅射以合成二元硼化物，两个二元硼化物靶，例如WB2和AlB2的同时溅射合成具有广泛化学成分范围的三元硼化物，在此情况下是WAlB2。在后者的这种组合合成情况下，合成涂层的化学成分可以依据施加至每个二元硼化物靶的功率和其溅射速率变化来调节。为了达成稳定工艺过程所需要的工艺气体压力范围为0.3至0.9Pa。通过在上述范围内调节工艺气体压力来保证工艺过程稳定性。400～600℃基材温度范围保证了在采用从浮动偏压至50伏的低偏电压值时所需的迁移能力。在这种设定条件中，可以获得有利的晶体结构，同时硼化物涂层的残余应力水平没有造成涂层剥离。
为了在基材表面和硼化物之间沉积中间层/梯度层，优选采用具有超过20原子％的W的Al-W靶。
以上所举例子描述了溅射沉积。当然，也可以通过阴极电弧蒸发来沉积Al-B基涂层。在此过程中，靶Al-B或含有Al-B-W的靶被用作阴极。
本发明的最重要方面可被归总如下：
一种涂覆工具，包括涂覆面，该涂覆面包括作为涂覆工具组成部分的基材表面和沉积在该基材表面上的涂层，其中，该基材表面由含钴和/或含镍的材料制造，并且其中，该涂层包括至少一个含硼化物层，其中，所述至少一个含硼化物层由硼化物制造或由含硼化物材料制造，并且其中，所述至少一个含硼化物层是扩散阻挡层，当该涂覆工具或涂覆面暴露于在约600℃至1200℃之间范围内的温度时，该扩散阻挡层阻止钴和/或镍从基材表面扩散至该涂层。
上述的扩散阻挡层优选含有以下组成地制造：
-AlB2或者
-AlWB2或者
-AlB2和AlWB2或者
-TM硼化物，其中，TM是选自以下组的一个或多个过渡金属：3d、4d和5d元素，该层还含有铝。
在本发明的一个特别优选实施例中，上述的扩散阻挡层是AlWB2层。
在本发明的一个进一步优选实施例中，该基材表面由硬质合金制造或含有硬质合金或者由任何其它含钴材料制造。
在本发明的一个更优选实施例中，该基材表面由镍合金或含镍材料碳化物制造或者由任何其它含镍材料制造。
在本发明的一个更优选实施例中，除了扩散阻挡层外，该涂层还包括含有Al和W的层，但该层优选不是硼化物层。
在本发明的一个更优选实施例中，上述的含有Al和W但优选不是硼化物层的层是金属层Al-W层，其作为中间层(或夹层)被沉积在所述基材与扩散阻挡层之间。
在本发明的一个更优选实施例中，上述的中间层是梯度层。
本发明还涉及根据上述实施例之一或其组合的涂覆工具的用途，其中，该涂覆工具或涂覆面暴露于在约600℃和1200℃之间范围内的温度。
本发明还涉及根据前述实施例之一或其组合的涂覆工具的用途，其中，涂覆工具的基材是硬质合金，并且在扩散阻挡层上方沉积有金刚石层。在这样的情况下，不需要在金刚石层沉积之前对硬质合金基材进行脱钴预处理。
本发明还涉及一种用于涂覆根据前述权利要求1至7之一的涂覆工具的方法，其特点是，涂层是利用PVD，尤其是非反应性PVS(物理气相沉积)溅射而成的。
在本发明一个更优选实施例中，在上述方法中，氩被用作工艺气体。
在本发明一个更优选实施例中，在上述方法中，至少一个二元硼化物靶被溅射，尤其用于合成二元硼化物且优选用于同时溅射两个二元硼化物靶例如WB2和AlB2。
-在本发明一个更优选实施例中，在上述方法中，在溅射过程中采用0.3至0.9Pa压力范围。
在本发明一个更优选实施例中，在上述方法中，在溅射过程中采用400至600℃的温度范围。
在本发明一个更优选实施例中，在上述方法中，在溅射过程中采用低于50伏的偏电压值。
在本发明一个更优选实施例中，在上述方法中，为了沉积中间层Al-W，使用具有高于20原子％的W的靶。
根据本发明的涂覆工具的所有上述实施例可被用于机加工超合金材料。
在本发明的上下文中，扩散硼化物层可被用作扩散阻挡层，用于阻止不同于钴和镍的其它元素扩散。

Claims (17)

1.一种涂覆工具，包括涂覆面，该涂覆面包括基材(1)，该基材具有其上沉积涂层(2)的表面，其中，该基材由含钴材料制造，并且其中，该涂层包括至少一个含硼层(20)，其特征是，所述至少一个含硼层(20)含有铝，并且该层所含的硼以硼化物形式存在，由此该含硼层(20)能够形成用于提供扩散阻挡层作用的其它层，尤其当该涂覆工具或该涂覆面暴露于约600℃和1200℃之间范围内的温度时，用于阻止钴从该基材表面扩散至该涂层。
2.根据权利要求1所述的涂覆工具，其特征是，该含硼层(20)被制造为含有以下组分：
-AlB2或者
-AlWB2或者
-AlB2和AlWB2或者
-TM硼化物，其中，TM是选自以下组的一个或多个过渡金属：3d、4d和5d元素。
3.根据前述权利要求1至2之一所述的涂覆工具，其特征是，该涂层(2)包括形成在该基材(1)和所述至少一个含硼层(20)之间的第一其他层(21)，所述第一其他层(21)含有Al-Co金属间相和B-Co金属间相。
4.根据权利要求3所述的涂覆工具，其特征是，该涂层(2)包括形成在所述至少一个含硼层(20)上方的第二其他层(22)，所述第二其他层(22)含有Al-O。
5.根据前述权利要求1至2之一所述的涂覆工具，其特征是，该基材表面由硬质合金制造或含有硬质合金。
6.根据前述权利要求2至5之一所述的涂覆工具，其特征是，除了该扩散阻挡层外，该涂层还包括含有Al和W的层，但该层优选不是硼化物层。
7.根据权利要求6所述的涂覆工具，其特征是，所述含有Al和W的但优选不是硼化物层的层是金属层Al-W层，该金属层Al-W层是作为在该基材和该扩散阻挡层之间的中间层来沉积的。
8.根据权利要求7所述的涂覆工具，其特征是，该中间层是梯度层。
9.根据前述权利要求1至8之一所述的涂覆工具的用途，其特征是，该涂覆工具或该涂覆面暴露于在600℃和1200℃之间范围内的温度。
10.一种涂覆根据前述权利要求1至7之一所述的涂覆工具的方法，其特征是，该涂层或该涂层的至少一部分是通过使用PVD溅射技术，特别是非反应性PVD溅射技术来制造的。
11.根据权利要求10所述的方法，其特征是，氩被用作工艺气体。
12.根据权利要求11所述的方法，其特征是，至少一个二元硼化物靶被溅射，尤其用于二元硼化物的合成且优选用于两个二元硼化物靶，例如WB2和AlB2，的同时溅射。
13.根据权利要求10至12之一所述的方法，其特征是，在溅射过程中采用0.3至0.9Pa的压力范围。
14.根据权利要求10至13之一所述的方法，其特征是，在溅射过程中采用在400℃至600℃范围内的基材温度。
15.根据权利要求10至14之一所述的方法，其特征是，在溅射过程中采用低于50伏的偏电压值。
16.根据权利要求10至15之一和6和/或7所述的方法，其特征是，为了沉积该中间层Al-W，使用含有高于20原子％的W的靶。
17.一种用于涂覆根据前述权利要求1至7之一所述的涂覆工具的方法，其特征是，该涂层或该涂层的至少一部分是通过使用PVD阴极电弧蒸发技术，优选是非反应性PVD阴极电弧蒸发技术来制造的。
CN202080013015.5A 2019-02-08 2020-02-10 具有包括含硼化物的扩散阻挡层的涂层的涂覆工具 Pending CN113412344A (zh)

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