CN105452543A - 金刚石涂层及沉积该涂层的方法 - Google Patents
金刚石涂层及沉积该涂层的方法 Download PDFInfo
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- CN105452543A CN105452543A CN201480043361.2A CN201480043361A CN105452543A CN 105452543 A CN105452543 A CN 105452543A CN 201480043361 A CN201480043361 A CN 201480043361A CN 105452543 A CN105452543 A CN 105452543A
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- diamond
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 128
- 239000010432 diamond Substances 0.000 title claims abstract description 127
- 238000000576 coating method Methods 0.000 title claims abstract description 77
- 239000011248 coating agent Substances 0.000 title claims abstract description 57
- 238000000151 deposition Methods 0.000 title claims description 24
- 238000000034 method Methods 0.000 title claims description 10
- 239000011159 matrix material Substances 0.000 claims description 37
- 230000012010 growth Effects 0.000 claims description 20
- 238000003475 lamination Methods 0.000 claims description 16
- 239000008246 gaseous mixture Substances 0.000 claims description 13
- 230000003698 anagen phase Effects 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 239000002019 doping agent Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 230000006911 nucleation Effects 0.000 claims description 7
- 238000010899 nucleation Methods 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 230000001186 cumulative effect Effects 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 150000004767 nitrides Chemical class 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 9
- 238000005498 polishing Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002113 nanodiamond Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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Abstract
本发明涉及金刚石涂层,其特征在于它包含至少一个第一纳米晶金刚石层和第二微晶金刚石层的叠层。
Description
本发明涉及金刚石涂层,特别是具有小于20nm的粗糙度Ra的微晶金刚石涂层(MCD),其例如用于微观力学领域中的摩擦应用。
本发明还涉及该金刚石涂层的沉积方法,其经济地执行。本发明更具体地涉及应用于微机械零件的这类方法,排列所述微机械零件以与其它零件摩擦接触,微机械零件相对于所述其它零件为运动的。这些微机械零件可同样好地为移动零件,例如旋转零件,或者固定零件,例如轴承。作为非限定性实例,它们可以为用于机械钟表运动的微机械零件。
本发明还涉及包含具有涂有金刚石涂层的功能表面的基质的微机械零件。
现有技术中熟知将基质用微晶金刚石涂层涂覆以提高所述基质的耐磨性以及降低摩擦。
图1为根据现有技术的微晶层的示意性阐述。为产生该单晶金刚石涂层,在待涂覆基质2的表面上产生成核层1。该成核层例如包含由金刚石纳米颗粒形成的晶种,金刚石纳米颗粒以约1010个颗粒/cm2的涂层密度遍布于基质表面上。然后将基质放入热丝或等离子体化学气相沉积(CVD)反应器中,将气体混合物,通常甲烷-氢气混合物注入其中。在测定的压力、温度和气流条件下,金刚石单晶3由晶种以柱状方式生长至所需涂层厚度。微晶通常具有从基质向外扩张的棱锥柱状形状使得晶粒尺寸随着层厚度而提高,如图1所述。
对于摩擦应用和典型的抗磨性,使用具有约0.5-10μm的厚度的金刚石层。以该厚度,表面晶粒尺寸超过200nm且粗糙度(Ra)可达到大于50nm的值,这意味着在许多应用中不能实现满意的摩擦条件。
为克服该缺点,本领域技术人员因此不得不对沉积进行一个或多个随后的抛光操作以降低粗糙度。通常,这些抛光操作机械地或者通过等离子体方法进行。在所有情况下,这些抛光操作为长、困难、昂贵的且不提供对某些应用而言,特别是对涂覆微机械时钟组件如擒纵叉和/或擒纵轮齿而言令人满意的结果。
因此,本发明的目的是通过提供金刚石涂层,特别是具有小于20nm的粗糙度Ra的微晶金刚石涂层克服这些缺点,所述涂层比现有技术涂层更容易得到且更经济地执行。
本发明的目的还有提供具有在其整个厚度上改进的机械性能的微晶金刚石涂层。
本发明的目的还有提供在其可见外表面上具有小于100nm的晶粒尺寸而不管本发明涂层的总厚度的微晶金刚石涂层。
本发明的目的还有提供具有改进美学外观的外表面,尤其是具有改进的反射率且适用于光学领域的微晶金刚石涂层。
为此,本发明涉及金刚石涂层,其特征在于它包含至少一个第一纳米晶金刚石层和第二微晶金刚石层的叠层。
由于这些特征,本发明提供产生厚,即大于1μm,具有比具有相同厚度的微晶金刚石层更小的表面晶粒尺寸和相关粗糙度的微晶金刚石涂层的可能性。这是由于这一事实:单晶微晶生长来自由纳米晶金刚石层形成的成核层,其比由金刚石纳米颗粒形成的常规成核层致密得多。
根据一个优选实施方案,本发明涂层包含一系列的至少两个所述叠层,其中第一叠层的微晶金刚石层与下一叠层的纳米晶金刚石层接触。
由于棱锥柱状生长在形成涂层的各个叠层上再起动,这意味着该系列的本发明叠层以具有给定厚度的单一叠层的晶粒尺寸和粗糙度提供大的涂层厚度。
有利地,纳米晶层的厚度为50nm至1μm,微晶层的厚度为100nm至1μm,,优选纳米晶层的厚度为100-200nm微晶层的厚度为200-500nm。
优选纳米晶金刚石层表面的晶粒尺寸小于50nm,特别是小于30nm,甚至更优选小于10nm。
优选,本发明涂层的可见外表面的晶粒尺寸为约100nm。
本发明还涉及包含具有功能表面的基质的微机械零件,其中功能表面涂有包含至少一个第一纳米晶金刚石层和第二微晶金刚石层的叠层的金刚石涂层,基质的所述功能表面与所述涂层的纳米晶金刚石层接触。
有利地,基质选自包含硅、钛、锆、铪、钒、钽、钼、钨、硼的材料;后面材料的硼化物、碳化物、氮化物和氧化物,和陶瓷的组。
根据优选实施方案,本发明微机械零件可以为齿轮、齿杆、擒纵轮、擒纵叉杆、擒纵叉瓦、发条、主发条、摆轮游丝、心轴和/或枢轴承。
本发明还涉及通过在反应室中化学气相沉积而在基质上沉积金刚石涂层的方法,所述方法包括至少:
a)制备基质的步骤,
b)初始成核步骤,
c)使涂层在基质表面上生长的步骤,所述生长步骤包括至少一系列的2个连续阶段,包括纳米晶金刚石生长形成纳米晶金刚石层的阶段,其后微晶金刚石生长的另一阶段,其中纳米晶金刚石层用作用于微晶金刚石层生长的成核层。
优选,步骤c)重复多次。
有利地,在步骤c)的纳米晶金刚石生长阶段期间,调整沉积参数使得纳米晶金刚石晶粒尺寸不超过50nm,优选30nm,甚至更优选10nm,并设置步骤c)的微晶金刚石生长阶段的持续时间以实现200nm至1μm,优选200-500nm的微晶金刚石厚度。
优选,步骤c)的纳米晶金刚石生长阶段的持续时间使得可得到100-200nm的纳米晶金刚石厚度。
优选,基质选自包含硅、钛、锆、铪、钒、钽、钼、钨、硼的材料;后面材料的硼化物、碳化物、氮化物和氧化物,和陶瓷的组。
有利地,方法在热丝反应器中进行,且步骤c)期间的基质温度为500-1000℃。
根据一个优选实施方案,纳米晶金刚石生长阶段在以下条件下进行:
●持续时间1小时至5小时,
●将CH4/H2/X气体混合物加热,分别直接或间接活化,其中X表示掺杂剂气体,其中相对于总体积,掺杂剂气体的体积百分数为0%至10%,CH4的体积百分数为3%至9%,
●在1巴压力下的氢气流速为20-50升/分钟,优选40升/分钟,
●室中气体混合物的压力为2-6毫巴,
●基质温度为500-1000℃,
且微晶金刚石生长阶段在以下条件下进行:
●持续时间1小时至5小时,
●将CH4/H2/X气体混合物分别直接或间接加热,其中X表示掺杂剂气体,其中相对于总体积,掺杂剂气体的体积百分数为0%至10%,CH4的体积百分数为0,05%至1%,
●在1巴压力下的氢气流速为30-90升/分钟,优选60升/分钟,
●室中气体混合物的压力为0.5-2毫巴,且
●基质温度为500-1000℃。
附图简述
本发明的特征在参考附图阅读对仅作为非限定性实例给出的本发明优选实施方案的描述时更清楚地获悉,其中:
-已经描述的图1显示涂有根据现有技术的微晶金刚石涂层的基质的示意性横截面;
-图2显示涂有包含本发明叠层的微晶金刚石涂层的基质的横截面;
-图3显示涂有包含多个本发明叠层的微晶金刚石涂层的基质的横截面;
-图4a和4b分别为显示涂有根据本发明和根据现有技术的微晶金刚石涂层的基质的顶视图的扫描电子显微镜照片。
参考图1,看出涂有根据常规沉积方法沉积的微晶金刚石涂层3的基质2。应当指出微晶生长由分布于基质2表面上的由金刚石纳米颗粒形成的晶种1引发,并产生由从基质表面向外扩张的具有棱锥柱状几何的晶体形成的层。当层3的厚度提高时,晶体尺寸提高并确保涂层的可见外表面上的晶粒尺寸生长。晶粒尺寸的这一提高导致粗糙度提高,取决于涂层的预期应用,这可能是不理想的。
参考图2,看出涂有根据本发明沉积方法沉积的微晶金刚石涂层5的基质4。
不同于由单一微晶金刚石层3形成的现有技术涂层,单晶金刚石涂层由第一纳米晶金刚石层5a和第二微晶金刚石层5b的叠层形成,如图2所示。
应当指出以相同的微晶金刚石涂层表面厚度,与现有技术涂层相比,涂层的可见外表面上的晶粒尺寸更小,因此粗糙度降低。这是由于这一事实:微晶金刚石层的成核由为密闭层的纳米晶金刚石层产生,这提供比由简单分布在待涂覆基质表面上的金刚石纳米颗粒形成的常规晶种更密且更均匀的生长位数。例如,以约100nm的纳米晶层厚度和约200nm的微晶层厚度,所得晶粒尺寸的降低为约50%,且粗糙度Ra的降低为约30%。这清楚地显示于图4a和4b中。
另外,由于本发明金刚石涂层的层叠性质,以相同的金刚石涂层厚度,本发明涂层的微晶金刚石层比现有技术微晶金刚石涂层更薄。本发明金刚石涂层中微晶金刚石层的这一厚度降低还贡献于涂层外表面的晶粒尺寸和粗糙度Ra的降低。
参考图3,看到本发明涂层7的变化实施方案沉积于其上的基质6。在该变化方案中,涂层包含一系列的两个叠层5,如同参考图2所述的那些。
图4a和4b显示涂有微晶金刚石涂层的基质的顶视图的扫描电子显微镜照片,其中最终微晶金刚石层以相同的条件(一起在相同的反应器中),根据本发明由纳米晶层(图4a)以及根据现有技术由分布于基质表面的金刚石纳米颗粒沉积。清楚地看出,本发明涂层的晶粒尺寸比现有技术(对于250nm的微晶金刚石层厚度,通常为200nm)小50%(对于250nm的微晶金刚石层厚度,通常为100nm),且本发明涂层的粗糙度Ra与现有技术相比降低30%。
下文描述本发明微晶金刚石涂层在由包含待涂覆微机械零件的硅片形成的基质上的示例沉积,所述微机械零件通过易碎固定元件保持在晶片上。
涂层5通过在热丝反应室中化学气相沉积(CVD)而沉积在基质4上。
在放入反应室中以前,将基质4在氢氟酸浴中清洗以除去原生氧化物层并增强会用于生长第一纳米晶金刚石层的金刚石纳米颗粒在其表面的附着。
然后将基质4放入包含溶剂,通常异丙醇且金刚石纳米颗粒悬浮的浴中。纳米颗粒的尺寸通常为5-15nm。然后借助超声搅拌该浴以将金刚石纳米颗粒附着在基质表面上。
然后将基质4风干或者在惰性气流,例如氮气流中干燥以完成基质制备步骤。
然后将制备的基质置于反应室中的台上,优选容许气体围绕基质自由流动,然后将室排空,通常以小于1毫巴的真空。
然后将基质借助加热器直接和/或通过由反应器灯丝辐射的热间接加热至沉积温度。通常,沉积温度为500-1000℃,例如约750°的温度。
当达到沉积温度时,将CH4/H2气体混合物注入反应室中。CH4的百分数相对于总体积为3%至9%,优选6%,且在1巴压力下的氢气流速为20-50升/分钟,优选40升/分钟。室中气体混合物的压力则为2-6毫巴,优选4毫巴。这些条件引发成核和由金刚石纳米颗粒的纳米晶金刚石生长步骤并构成初始成核步骤。
然后保持初始成核步骤条件以使纳米晶金刚石层至少在容许形成纳米晶金刚石层的厚度,通常在100nm的厚度上生长。
该厚度当然可取决于待得到的所需最终涂层硬度改变,并且达一微米,尽管已知如果涂层的纳米晶金刚石层具有较大的厚度,则本发明涂层的硬度会是较低的。
纳米晶金刚石生长构成本发明金刚石涂层生长步骤的一个阶段。
当实现所需纳米晶金刚石厚度时,改变反应室中的条件以使微晶金刚石层生长。为此,改进CH4相对于CH4/H2气体混合物总体积的百分数并且变成0.05%至1%,优选0.1%的值,且在1巴压力下的氢气流速变成30-90升/分钟,优选60升/分钟的值。然后使室中气体混合物的压力返回0.5-2毫巴,优选1毫巴的值。在这些沉积条件下,金刚石生长以微晶形式进行,下面纳米晶层的晶粒形成未来微晶层的晶种。
当实现所需厚度时,微晶金刚石层生产阶段中断一次。为得到具有降低的表面晶粒尺寸(通常约100nm)和小于20nm的粗糙度Ra且适用于摩擦应用的微晶金刚石层,微晶金刚石层的厚度应优选不超过500nm。
对于其中需要大于1μm的金刚石涂层厚度的应用,重复纳米晶金刚石和微晶金刚石层的一系列连续沉积直至实现所需厚度。
不言而喻,本发明不限于恰好描述的实施方案且本领域技术人员可不偏离如所附权利要求书所定义的本发明范围而预期各种简单的改进和变化。
Claims (20)
1.意欲用于涂覆基质的金刚石涂层,其特征在于涂层包含至少一个第一纳米晶金刚石层和第二微晶金刚石层的叠层,其中最接近基质的金刚石层为纳米晶的且距离基质最远的金刚石层为微晶的。
2.根据权利要求1的金刚石涂层,其特征在于涂层包含一系列的至少两个所述叠层,其中第一叠层的微晶金刚石层与下一叠层的纳米晶金刚石层接触。
3.根据权利要求1或2的金刚石涂层,其特征在于纳米晶金刚石层的厚度为50nm至1μm。
4.根据权利要求3的金刚石涂层,其特征在于纳米晶金刚石层的厚度为100-200nm。
5.根据前述权利要求中任一项的金刚石涂层,其特征在于微晶金刚石层的厚度为100nm至1μm。
6.根据权利要求5的金刚石涂层,其特征在于微晶金刚石层的厚度为200-500nm。
7.根据前述权利要求中任一项的金刚石涂层,其特征在于纳米晶金刚石层表面上的晶粒尺寸为小于50nm,优选小于30nm,甚至更优选小于10nm。
8.包含具有功能表面的基质的微机械零件,其特征在于所述功能表面涂有根据权利要求1-7中任一项的涂层,且所述功能表面与所述涂层的纳米晶金刚石层接触。
9.根据权利要求8的微机械零件,其特征在于基质选自包含硅、钛、锆、铪、钒、钽、钼、钨、硼的材料;后面材料的硼化物、碳化物、氮化物和氧化物,和陶瓷的组。
10.根据权利要求8或9的微机械零件,其特征在于零件包括齿轮、齿杆、擒纵轮、擒纵叉杆、擒纵叉瓦、发条、主发条、摆轮游丝、心轴和/或枢轴承。
11.通过在反应室中化学气相沉积而将金刚石涂层沉积在基质上的方法,所述方法包括至少:
a)制备基质的步骤,
b)初始成核步骤,
c)生长步骤,所述生长步骤包括至少一系列的2个连续阶段,包括纳米晶金刚石生长形成纳米晶金刚石层的阶段,其后微晶金刚石生长的另一阶段,其中纳米晶金刚石层用作用于微晶金刚石层生长的成核层。
12.根据权利要求11的沉积方法,其特征在于步骤c)重复多次。
13.根据权利要求11或12的沉积方法,其特征在于在步骤c)的纳米晶金刚石层生长阶段期间,设置沉积参数使得纳米晶金刚石晶粒尺寸不超过50nm,优选30nm,甚至更优选10nm。
14.根据权利要求11-13中任一项的沉积方法,其特征在于步骤c)的微晶金刚石生长阶段的持续时间可产生200nm至1μm,优选200-500nm的微晶金刚石厚度。
15.根据权利要求11-14中任一项的沉积方法,其特征在于步骤c)的纳米晶金刚石生长阶段的持续时间可产生100-200nm的纳米晶金刚石厚度。
16.根据权利要求11-15中任一项的沉积方法,其特征在于基质选自包含硅、钛、锆、铪、钒、钽、钼、钨、硼的材料;后面材料的硼化物、碳化物、氮化物和氧化物,和陶瓷的组。
17.根据权利要求11-16中任一项的沉积方法,其特征在于方法在热丝反应器中进行。
18.根据权利要求11-17中任一项的沉积方法,其特征在于步骤c)期间的基质温度为500-1000℃。
19.根据权利要求11-18中任一项的沉积方法,其特征在于纳米晶金刚石生长阶段在以下条件下进行:
●持续时间1小时至5小时,
●将CH4/H2/X气体混合物加热,分别直接或间接活化,其中X表示掺杂剂气体,其中相对于总体积,掺杂剂气体的体积百分数为0%至10%,CH4的体积百分数为3%至9%,
●在1巴压力下的氢气流速为20-50升/分钟,优选40升/分钟,
●室中气体混合物的压力为2-6毫巴,优选4毫巴
●基质温度为500-1000℃。
20.根据权利要求11-19中任一项的沉积方法,其特征在于微晶金刚石生长阶段在以下条件下进行:
●持续时间1小时至5小时,
●将CH4/H2/X气体混合物分别直接或间接加热,其中X表示掺杂剂气体,其中相对于总体积,掺杂剂气体的体积百分数为0%至10%,CH4的体积百分数为0,05%至1%,
●在1巴压力下的氢气流速为30-90升/分钟,优选60升/分钟,
●室中气体混合物的压力为0.5-2毫巴,优选1毫巴,
●基质温度为500-1000℃。
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EP13179159.2A EP2832899A1 (fr) | 2013-08-02 | 2013-08-02 | Revêtement de diamant et procédé de dépôt d'un tel revêtement |
EP13179159.2 | 2013-08-02 | ||
PCT/EP2014/064043 WO2015014562A1 (fr) | 2013-08-02 | 2014-07-02 | Revetement de diamant et procede de depot d'un tel revetement |
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RU2660878C2 (ru) | 2018-07-10 |
WO2015014562A1 (fr) | 2015-02-05 |
CN105452543B (zh) | 2018-10-23 |
EP2832899A1 (fr) | 2015-02-04 |
US20160186363A1 (en) | 2016-06-30 |
RU2016107491A (ru) | 2017-09-07 |
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