CN105492652A - TiB2层及其制造 - Google Patents

TiB2层及其制造 Download PDF

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CN105492652A
CN105492652A CN201480038313.4A CN201480038313A CN105492652A CN 105492652 A CN105492652 A CN 105492652A CN 201480038313 A CN201480038313 A CN 201480038313A CN 105492652 A CN105492652 A CN 105492652A
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workpiece
tib
maximum
layer
coating
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CN105492652B (zh
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徳尼斯·库拉珀夫
西格弗里德·克拉斯尼策尔
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Oerlikon Surface Solutions AG Pfaeffikon
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Oerlikon Trading AG Truebbach
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/067—Borides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3464—Sputtering using more than one target
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3426—Material

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Physical Vapour Deposition (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Laminated Bodies (AREA)

Abstract

本发明涉及具有涂层的工件，涂层包括至少一个TiB2层，其特征是，该TiB2层具有以下织构，该织构在XRD图谱中造成显示出鲜明的(002)取向的明显的峰。本发明还涉及制造具有涂层的这种工件的方法。

Description

TiB2层及其制造
本发明涉及包含至少一个TiB2层的涂层。
已知的是TiB2作为层膜材料被用于工具。例如在US4820392中描述了如何借助雾化法(溅射)将TiB2层施加至工具。尽管如此施加的材料的特点是具有良好的机械性能和摩擦学性能，但在实践中力求获得更高的密度和更高的硬度。
因为TiB2是熔点很高的材料，故无法经济地使用所谓的电弧气化，其可导致较密、进而较硬的层膜。
在类似火花气化领域内“移动”溅射层的密度和硬度的一种已知的可能方式就是所谓的HIPIMS法(HIPIMS＝高功率脉冲磁控溅射)。在此溅射法中，对溅射阴极提供高功率脉冲密度，这导致从阴极雾化的材料以高百分比被电离化。如果现在对待涂覆工件施以负压，则这些离子被朝向工件加速，这导致很密的层膜。
溅射阴极必须以脉冲方式接受功率，以便给其时间，以散走伴随功率而来的热输入。因此，在HIPIMS方法中作为功率源需要脉冲发生器。该脉冲发生器须能够输出很高但很短的功率脉冲。当今可获得的脉冲发生器显示出不高的灵活性，这涉及到例如脉冲高度和/或脉冲持续时间。理想地应该输出矩形脉冲。但在大多数情况下，在一个脉冲内的功率输出明显取决于时间，这直接影响到层膜性能例如硬度、附着性、固有应力等。另外，涂覆速率因偏离矩形曲线而受到不利影响。
尤其是，这些困难提出了与可再现性相关的问题。
因此，人们需要这样的方法，据此可以借助磁控溅射在高功率下产生TiB2层。根据本发明，这些层借助溅射法来产生，此时出现功率源的始终高的功率输出。在此，采用多个溅射阴极。不同于在传统的HIPIMS方法中，没有使用脉冲发生器，而是首先只对第一溅射阴极供应该功率源的全功率和进而高功率密度。随后，第二溅射阴极与该功率源的输出相连。此时首先少量通过，这是因为第二溅射阴极的阻抗在此时刻比第一溅射阴极的阻抗高得多。只有当第一溅射阴极与功率源的输出分开时，功率输出才基本上通过第二溅射阴极进行。相应的高功率磁控溅射法在WO2013060415中有详细描述。一般，功率源此时以60kW数量级运行。溅射阴极按照时间平均所经受的典型功率就数量级而言处于8kW。
现在，本发明人已经发现，当这样的方法在以陶瓷靶如TiB2靶作为溅射阴极运行时，做到了生成具有很好机械性能的可再现的层膜。另外，本发明人已经发现，在这种非反应性处理过程中可通过工作气体分压的调节来直接影响层膜粗糙性，确切说没有显著地不利影响到上述的机械性能。
例如，制造多个TiB2层。这些层具有以下织构，该织构在XRD图谱中造成显示出鲜明的(001)取向的、明显的峰。这样的取向被证明在需要硬质材料层的很多应用中是很有利的。
为了证明工作气体分压对表面粗糙度的影响，以不同的氩气流量来工作。因此，在80sccm的氩气流量情况下测得表面粗糙度Ra＝0.14μm和Rz＝0.115μm，在160sccm氩气流量情况下测得表面粗糙度Ra＝0.115μm和Rz＝0.095μm，在300sccm氩气流量情况下测得表面粗糙度Ra＝0.06μm和Rz＝0.05μm。在所用的涂覆设备中，80sccm的氩气流量对应于0.2Pa分压，160sccm的氩气流量对应于0.4Pa分压，300sccm的氩气流量对应于0.75Pa分压。这如图1所示。
与此相比，所述层的硬度和层的E模量保持恒定良好。这如图2所示。
即，利用本发明公开了一种用于高效经济地制造方法TiB2层的方法。该方法导致具有迄今未知的硬度还伴随有很低的表面粗糙度的TiB2层。这尤其与应用在滑动表面上的用途相关地是很让人感兴趣的。迄今的传统PVD溅射法不允许制造如此坚硬的TiB2层。

Claims (7)

1.一种具有涂层的工件，所述涂层包括至少一个TiB2层，其特征是，所述TiB2层具有至少50GPa的硬度。
2.根据权利要求1的工件，其特征是，所述TiB2层具有以下织构，该织构在XRD图谱中造成显示出鲜明的(001)取向的、明显的峰。
3.根据权利要求1或2的工件，其特征是，该工件的表面在涂覆之后随即具有最大为0.14μm、优选最大为0.115μm且尤其优选最大为0.095μm的表面粗糙度Ra，如果减去未涂覆的工件表面的贡献。
4.根据权利要求1至3之一的工件，其特征是，该工件的表面在涂覆之后随即具有最大为0.115μm、优选最大为0.095μm且尤其优选最大为0.05μm的表面粗糙度Rz，如果减去未涂覆的工件表面的贡献。
5.一种用包含TiB2的层涂覆工件的方法，其包括以下步骤：
给涂覆室装入待涂覆的工件，
如下执行非反应性溅射法：对至少两个TiB2靶交替施以高于20kW的直流功率源的功率，所述功率源有时在靶上导致局部大于0.2A/cm2的电流密度，其中，所述靶按时间平均来说必须耗用不超过10kW的功率。
6.根据权利要求5的方法，其特征是，为了溅射，至少有时候维持不低于0.2Pa、优选不低于0.4Pa且尤其优选不低于0.75Pa的工作气体分压。
7.根据权利要求6的方法，其特征是，该工作气体至少包含氩气。
CN201480038313.4A 2013-07-03 2014-06-30 TiB2层及其制造 Active CN105492652B (zh)

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DE102013011075.0A DE102013011075A1 (de) 2013-07-03 2013-07-03 TiB2 Schichten und ihre Herstellung
DE102013011075.0 2013-07-03
PCT/EP2014/001781 WO2015000576A1 (de) 2013-07-03 2014-06-30 Tib2 schichten und ihre herstellung

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CN108251803A (zh) * 2016-12-29 2018-07-06 深圳先进技术研究院 TiB2自润滑涂层及其制备方法和耐磨构件
CN109136608A (zh) * 2018-08-22 2019-01-04 北京理工大学 一种取向可控的TiB晶须增强钛基复合材料的制备方法
CN112359395A (zh) * 2020-10-15 2021-02-12 安徽工业大学 一种金属硼化物涂层及其制备方法
CN113981369A (zh) * 2021-10-28 2022-01-28 赣州澳克泰工具技术有限公司 多层涂层系统及其制备方法

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CN115612984A (zh) * 2022-09-09 2023-01-17 中国科学院金属研究所 一种应力和结构梯度的二硼化钛涂层及其制备方法

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CN105755440A (zh) * 2016-04-19 2016-07-13 中国科学院宁波材料技术与工程研究所 一种耐海水腐蚀的硬质涂层及其制备方法
CN105755440B (zh) * 2016-04-19 2019-04-02 中国科学院宁波材料技术与工程研究所 一种耐海水腐蚀的硬质涂层及其制备方法
CN108251803A (zh) * 2016-12-29 2018-07-06 深圳先进技术研究院 TiB2自润滑涂层及其制备方法和耐磨构件
CN108251803B (zh) * 2016-12-29 2020-06-02 深圳先进技术研究院 TiB2自润滑涂层及其制备方法和耐磨构件
CN107740043A (zh) * 2017-10-25 2018-02-27 深圳先进技术研究院 掺杂CaF2的TiB2涂层、CaF2和TiB2复合涂层、其制备方法和应用及刀具
CN109136608A (zh) * 2018-08-22 2019-01-04 北京理工大学 一种取向可控的TiB晶须增强钛基复合材料的制备方法
CN112359395A (zh) * 2020-10-15 2021-02-12 安徽工业大学 一种金属硼化物涂层及其制备方法
CN112359395B (zh) * 2020-10-15 2021-09-24 安徽工业大学 一种金属硼化物涂层的制备方法
CN113981369A (zh) * 2021-10-28 2022-01-28 赣州澳克泰工具技术有限公司 多层涂层系统及其制备方法

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IL243433B (en) 2019-06-30
KR102234455B1 (ko) 2021-04-01
JP2016527392A (ja) 2016-09-08
RU2016103250A (ru) 2017-08-09
MY186024A (en) 2021-06-15
PH12015502841A1 (en) 2018-08-20
WO2015000576A1 (de) 2015-01-08
BR112015032908B1 (pt) 2022-03-15
EP3017078A1 (de) 2016-05-11
SG11201510769SA (en) 2016-02-26
HUE053539T2 (hu) 2021-07-28
CA2916769C (en) 2022-03-08
PL3017078T3 (pl) 2021-06-28
DE102013011075A1 (de) 2015-01-08
MX2016000044A (es) 2016-05-31
BR112015032908A2 (zh) 2017-07-25
IL243433A0 (en) 2016-02-29
JP6561048B2 (ja) 2019-08-14
KR20160029815A (ko) 2016-03-15
CA2916769A1 (en) 2015-01-08
US20160186306A1 (en) 2016-06-30
EP3017078B1 (de) 2020-12-16
CN105492652B (zh) 2018-09-28
US10378095B2 (en) 2019-08-13

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