CN112236403B - 靶和用于制造靶的方法 - Google Patents
靶和用于制造靶的方法 Download PDFInfo
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- CN112236403B CN112236403B CN201980026614.8A CN201980026614A CN112236403B CN 112236403 B CN112236403 B CN 112236403B CN 201980026614 A CN201980026614 A CN 201980026614A CN 112236403 B CN112236403 B CN 112236403B
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- 238000000034 method Methods 0.000 title claims description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 75
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 58
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 57
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 239000010936 titanium Substances 0.000 claims abstract description 29
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000000704 physical effect Effects 0.000 claims abstract 2
- 238000002490 spark plasma sintering Methods 0.000 claims description 17
- 238000007731 hot pressing Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 7
- 238000005259 measurement Methods 0.000 claims description 6
- 238000009472 formulation Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 230000000996 additive effect Effects 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 229910052729 chemical element Inorganic materials 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 24
- 238000002156 mixing Methods 0.000 description 6
- 238000007373 indentation Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000000541 cathodic arc deposition Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000006115 industrial coating Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
一种用于物理气相沉积的靶，所述靶具有如下化学成分：‑以下化合物中的至少两种化合物的混合物：二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)的混合相((Ti,V)B2)，所述至少两种化合物为95mol％至100mol％‑0.01mol％至5mol％的碳(C)‑二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)的混合相((Ti,V)B2)以外的小于0.01mol％的硼化物，其中关于金属纯度方面，二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)的混合相((Ti,V)B2)的混合物以及碳(C)的总和至少为99.8mol％，而且具有如下物理特性：‑密度大于上文所限定的化学成分的理论密度的90％、优选地大于上文所限定的化学成分的理论密度的95％‑二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)的混合相((Ti,V)B2)的混合物的晶粒的平均粒度小于10微米、优选地小于3微米。
Description
技术领域
本发明涉及一种具有权利要求1的前序部分的特征的用于物理气相沉积的靶(涂层源)和一种具有权利要求9的特征的用于制造靶的方法。
背景技术
在现有技术中，物理气相沉积方法被大范围用于制造各种不同的层。由于这种层的应用范围广泛，必须能够沉积不同类型的涂层材料。
在此，在物理气相沉积的情况下使用各种不同的技术，诸如蒸发、阴极雾化(溅射沉积(sputter deposition))或电弧蒸发(阴极电弧沉积(cathodic arc deposition)或电弧源(Arc-Source)蒸发技术)。
靶适合于在PVD(physical vapor deposition，物理气相沉积)工艺中使用以将层沉积到为此所设置的衬底材料上。在本发明的上下文中，术语靶应理解为溅射靶或电弧阴极。
视材料而定，这些靶通过不同的技术来制造。在此，原则上可以在粉末冶金与熔融冶金工艺之间进行区分。在粉末冶金技术的情况下，存在多种不同的可能性，这些可能性必须根据靶的成分在考虑合成元素的特性的情况下来选择。示例性地，这里可列举压制、烧结、热等静压(HIP)、锻造、轧制、热压(HP)或火花等离子烧结(SPS)以及也包括它们彼此间的组合。
通用靶和方法在WO 2008/96648 A1、JP 05195199、JP55128560和WO 2011/137472A1中予以描述。
尤其是，JP55128560描述了对具有至少两种不同的二硼化物的烧结体的制造，其中强制使用硼化物形式的如镍、铁和钴那样的金属作为粘合剂和烧结助剂，以便补偿在烧结温度比较低的情况下制造的孔隙率低的缺点。不利的是：在使用烧结体作为靶时，这些金属影响沉积层的纯度。
还公知的是：借助于共溅射来制造由二硼化钛(TiB2)和二硼化钒(VB2)构成的层，其中使用由基本上纯二硼化钛(TiB2)和基本上纯二硼化钒(VB2)构成的单独靶。不利的是：在工业涂层工艺中，由于这些单独靶与旋转衬底的空间分开而不可避免地形成多层的层而不是化学均匀的层。
发明内容
本发明的任务是提供一种通用靶和一种用于制造靶的通用方法，该靶的密度高，利用该靶能制造高纯度的、化学均匀的层并且该靶具有细晶粒且各向同性的微观结构。
该任务通过一种具有权利要求1的特征的靶和一种具有权利要求9的特征的方法来解决。本发明的有利的实施方式在从属权利要求中限定。还寻求对在物理气相沉积方法(PVD)中使用按照本发明的靶来将薄层沉积在衬底上的保护。
本发明在不使用诸如镍、钴或铁那样的粘合剂或烧结助剂作为粉末状添加剂的情况下应用，因为按照本发明的用于制造靶的方法在温度比较高的情况下进行。但是，这不可避免地导致结构在这些高温下会非常强烈地粗化，这对于用作靶来说又会是不利的。本发明避免了该粗化，其方式是使用由至少两种不同的相、即二硼化钛(TiB2)、二硼化钒(VB2)以及也许碳、优选地石墨(如果碳不是以一种或两种相二硼化钛(TiB2)或二硼化钒(VB2)的杂质的形式存在的话)组成的粉末。这确保了尽管压缩温度比较高仍保持细晶粒的微观结构。
按照本发明，以下化合物中的至少两种化合物的混合物的总和：二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)在烧结期间形成的混合相((Ti,V)B2)以及碳(C)至少为99.8mol％。这是在不考虑如氧(O)、氮(N)或氢(H)的这样的元素情况下的金属纯度。
能用于按照本发明的方法的粉末配方包括：
-二硼化钛(TiB2)和二硼化钒(VB2)的为95mol％至100mol％的混合物
-以及必要时0.01mol％至5mol％的碳(C)。
由于二硼化钛(TiB2)和/或二硼化钒(VB2)有杂质，在根据本发明的靶中，可能检测到二硼化钛(TiB2)和二硼化钒(VB2)以外的硼化物(小于0.01mol％)。
在本发明的一个实施例中规定：碳(C)以石墨形式存在。
对于所有在下文讨论的按照本发明的靶的粉末配方的混合物来说，示例性地使用了如下粉末：
-粒度的d50值为2.4μm的TiB2
-粒度的d50值为7.0μm的VB2
-粒度小于6μm的石墨粉末。
这些粉末以TiB2/VB2/C的比例为74/24/2mol％混合并且已在具有研磨球的研磨设备中被研磨。研磨完的粉末混合物通过在30MPa的压力和2000℃的温度下的热压来压缩。
在本发明的一个实施例中规定：二硼化钛(TiB2)和二硼化钒(VB2)均匀分布地存在于靶中，使得在选择大小分别为至少1mm2的至少五个方形或圆形的不同的测量区域的情况下，在相应的测量区域的表面上确定的平均化学成分与从所有被选择的测量区域计算出的平均化学成分的偏差不超过20％、优选地不超过10％。
在下表中示出了不同的按照本发明的靶的三个这样的测量系列：
能良好地看出：这些靶中的每个靶的在相应的测量区域的表面上确定的平均化学成分只是最小程度地与从所有被选择的测量区域计算出的平均化学成分有偏差。
在本发明的一个实施例中规定：在靶的X射线检查中，能看出没有优选的结晶学方面的晶粒取向的各向同性结构，其中由二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)的混合相((Ti,V)B2)构成的混合物的晶粒的长径比小于1.5、优选地小于1.2、特别优选地基本上为1。
在本发明的一种实施方式中规定：只有二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)的混合相((Ti,V)B2)以X射线可标识的相的形式存在。
在本发明的一个实施例中，关于该方法规定：热压或火花等离子烧结(SPS)在为至少20MPa、优选地至少30MPa的压力下进行。
通过热压的制造的示例是：
-通过在球磨机中的研磨来制造的TiB2/VB2 75/25mol％粉末混合物
-在规格为238x353mm的工具中热压成尺寸为32x238 x353毫米的板并具有以下参数：
o 2000℃
o 252吨的力，这相当于29.5MPa的压力
o在烧结温度下为30分钟的保持时间。
板所达到的密度为4.54g/cm3，并且因此约为该材料的为4.64g/cm3的理论密度的97.8％，这通过75mol％的理论密度为4.5g/cm3的TiB2与25mol％的理论密度为5.1g/cm3的VB2的混合规则来计算。
在本发明的一个实施例中，关于该方法规定：热压或火花等离子烧结(SPS)在真空中或在惰性保护气体环境中进行。
对于本领域技术人员而言，关于粒度、密度、掺杂、纯度以及通过热压或SPS的制造方法而言，在本公开中所描述的由TiB2/VB2混合物构成的靶的微观结构能转用于硼化物的其它组合，尤其是能转用于硼化物TiB2、VB2、CrB2、ZrB2、NbB2、MoB2、MoB、HfB2、TaB2、WB2、W2B5的组合。在这些混合物的情况下涉及至少两种硼化物的体系，例如由两种硼化物构成的二元体系或者也包括三种、四种或还更多种硼化物同时在一种混合物中所构成的体系。
附图说明
依据附图来讨论本发明的实施例。在此：
图1示出了由纯TiB2构成的不是按照本发明的靶的REM(扫描电子显微镜)图像；
图2示出了由纯TiB2构成的另一不是按照本发明的靶的REM图像；
图3a、b示出了由TiB2/VB2构成的两个按照本发明的靶的REM图像；
图4示出了由TiB2/VB2构成的按照本发明的靶的REM图像；
图5示出了由TiB2/VB2构成的按照本发明的靶的REM图像；
图6示出了由TiB2/VB2构成的按照本发明的靶的REM图像；
图7a、b示出了根据图3b的按照本发明的靶的X射线图像(XRD)以及X射线图像(XRD)的放大片段；
图8示出了在由TiB2/VB2 75/25mol％构成的根据本发明的靶的情况下进行硬度测试的结果的照片图像；
图9示出了在根据图4的靶的情况下进行硬度测试的结果的照片图像；
图10示出了在根据图5的靶的情况下进行硬度测试的结果的照片。
具体实施方式
图1和2示出了纯TiB2材料的结构的示例，该纯TiB2材料是在不同温度下被压缩的，以便达到相对应地高的密度。为了便于比较，在两张图中选择了相同的放大部分。如果温度过高，则已经发生强烈的晶粒粗化。
图1示出了在1650℃下被热压的纯TiB2。该结构的晶粒仍相对细，估计平均粒度为2μm。材料的密度为4.43g/cm3，并且因此约为TiB2的为4.52g/cm3的理论密度的98％。
图2示出了在1700℃下被热压的纯TiB2。该结构已经部分地相对强烈地粗化，其中单个晶粒大于10μm。材料的密度约为TiB2的理论密度的98.5％。
图3至5示出了按照本发明的靶的示例，其中在二硼化钛(TiB2)和/或二硼化钒(VB2)和/或二硼化钛(TiB2)与二硼化钒(VB2)的混合相((Ti,V)B2)的混合物中钛(Ti)与钒(V)的分子比例在1:99至99:1的范围内，优选地在10:90至90:10的范围内。在图3至5中的TiB2/VB2材料的结构没有示出任何纹理化以及晶粒的长径比基本上为1的各向同性结构。
图3a示出了由TiB2/VB2 75/25mol％材料构成的靶的细节，该材料在1900℃下通过SPS被压缩。该材料的密度为4.19g/cm3，并且因此约为该材料的为4.64g/cm3的理论密度的90％，这通过75mol％的理论密度为4.5g/cm3的TiB2与25mol％的理论密度为5.1g/cm3的VB2的混合规则来计算。
图3b示出了由TiB2/VB2 75/25mol％材料构成的靶的细节，该材料在2000℃下通过SPS被压缩。该材料的密度为4.49g/cm3，并且因此约为该材料的为4.64g/cm3的理论密度的97％，这通过75mol％的理论密度为4.5g/cm3的TiB2与25mol％的理论密度为5.1g/cm3的VB2的混合规则来计算。
图4示出了由TiB2/VB2 87.5/12.5mol％材料构成的靶的细节，该材料在2000℃下通过SPS被压缩。该材料的密度为4.52g/cm3，并且因此约为该材料的为4.57g/cm3的理论密度的99％，这通过87.5mol％的理论密度为4.5g/cm3的TiB2与12.5mol％的理论密度为5.1g/cm3的VB2的混合规则来计算。
图5示出了TiB2/VB2 93.75/6.25mol％材料，该材料在2000℃下通过SPS被压缩。该材料的密度为4.46g/cm3，并且因此约为该材料的为4.53g/cm3的理论密度的98％，这通过93.75mol％的理论密度为4.5g/cm3的TiB2与6.25mol％的理论密度为5.1g/cm3的VB2的混合规则来计算。
上文所描述的按照本发明的靶是通过SPS方法来制造的，该SPS方法是分别在真空中被执行的。
为了进行比较，图6示出了仍始终具有高孔隙率的结构(因为在最低可接受温度下被压缩)、即通过SPS在1750℃下被压缩的TiB2/VB2 75/25mol％材料。该材料的密度为4.01g/cm3，并且因此约为该材料的为4.64g/cm3的理论密度的86％，这通过75mol％的理论密度为4.5g/cm3的TiB2与25mol％的理论密度为5.1g/cm3的VB2的混合规则来计算。
在图7a和7b中，能看到用于在具有根据图3b的成分的靶上进行相分析的X射线照相频谱。令人感兴趣的是TiB2、(Ti,V)B2和VB2的反射特性。本领域技术人员主要能将这三个相TiB2、(Ti,V)B2和VB2分配给该频谱。
图8至10分别示例性示出了在TiB2/VB2混合靶上测量的HV30硬度压痕。为了关于硬度的有代表性的结论，这里分别以三个HV30硬度压痕作为基础。
图8示出了三个HV30硬度压痕中的在由TiB2/VB2 75/25mol％构成的靶的情况下的HV30硬度压痕。
图9示出了三个HV30硬度压痕中的在由TiB2/VB2 87.5/12.5mol％构成的靶的情况下的HV30硬度压痕。
图10示出了三个HV30硬度压痕中的在由TiB2/VB2 93.75/6.25mol％构成的靶的情况下的HV30硬度压痕。
这些测量结果总结在下表中：
Claims (20)
1.一种用于物理气相沉积的靶，所述靶具有如下化学成分：
-以下化合物中的至少两种化合物的混合物：二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2，所述至少两种化合物为95mol％至100mol％
-0.01mol％至5mol％的碳C
-二硼化钛TiB2、二硼化钒VB2和/或二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2以外的小于0.01mol％的硼化物，
其中二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中的至少两种化合物的混合物以及碳C的总和至少为99.8mol％，并且不需要烧结助剂作为粉末状添加剂，而且具有如下物理特性：
-密度大于上述所限定的化学成分的理论密度的90％
-二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中的至少两种化合物的混合物的晶粒的平均粒度小于10微米，其中在二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中的至少两种化合物的混合物中钛Ti与钒V的原子摩尔比在87.5:12.5至10:90的范围内。
2.根据权利要求1所述的靶，其中所述靶所具有的密度大于上述所限定的化学成分的理论密度的95％。
3.根据权利要求1所述的靶，其中二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中的至少两种化合物的混合物的晶粒的平均粒度小于3微米。
4.根据权利要求1所述的靶，其中所述碳C以石墨形式存在。
5.根据权利要求1至4中任一项所述的靶，其中只有二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2以X射线可标识的相为形式存在。
6.根据权利要求1至4中任一项所述的靶，其中二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2均匀分布地存在于所述靶中，使得在选择大小分别为至少1mm2的至少五个方形或圆形的不同的测量区域的情况下，在相应的测量区域的表面上确定的平均化学成分与从所有被选择的测量区域计算出的平均化学成分的偏差不超过20％。
7.根据权利要求6所述的靶，其中在相应的测量区域的表面上确定的平均化学成分与从所有被选择的测量区域计算出的平均化学成分的偏差不超过10％。
8.根据权利要求1至4中任一项所述的靶，其中在所述靶的X射线检查中，能看出晶粒取向的各向同性结构，其中二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中的至少两种化合物的混合物的晶粒的长径比小于1.5。
9.根据权利要求8所述的靶，其中二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中的至少两种化合物的混合物的晶粒的长径比小于1.2。
10.根据权利要求8所述的靶，其中二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中的至少两种化合物的混合物的晶粒的长径比为1。
11.根据权利要求1至4中任一项所述的靶，其中钛Ti、钒V、硼B和碳C以外的化学元素溶解在二硼化钛TiB2、二硼化钒VB2、二硼化钛TiB2与二硼化钒VB2的混合相(Ti,V)B2中并且不能作为单独的相以X射线照相技术被探测到。
12.根据权利要求1至4中任一项所述的靶，其中所述靶的HV30维氏硬度大于1500HV30。
13.根据权利要求12所述的靶，其中所述靶的HV30维氏硬度大于2000HV30。
14.一种制造根据权利要求1至13中任一项所述的靶的方法，其中以粉末为形式存在的二硼化钛TiB2和以粉末为形式存在的二硼化钒VB2以及粉末状的碳被混合并且以机械方式被研磨，并且这样制造的粉末配方在成型工具中借助于热压或火花等离子烧结来被压缩，其特征在于，
所述粉末配方包括：
-二硼化钛TiB2和二硼化钒VB2的为95mol％至100mol％的混合物
-以及0.01mol％至5mol％的碳C
其中，二硼化钛TiB2和二硼化钒VB2的混合物以及碳C的总和至少为99.8mol％，
而且所述热压或火花等离子烧结利用至少1750℃的温度来进行。
15.根据权利要求14所述的方法，其中所述热压或火花等离子烧结利用至少1850℃的温度来进行。
16.根据权利要求14所述的方法，其中所述热压或火花等离子烧结利用至少1950℃的温度来进行。
17.根据权利要求14所述的方法，其中所述热压或火花等离子烧结在至少20MPa的压力下进行。
18.根据权利要求17所述的方法，其中所述热压或火花等离子烧结在至少30MPa的压力下进行。
19.根据权利要求14至18中任一项所述的方法，其中所述热压或火花等离子烧结在真空中或在惰性保护气体气氛中进行。
20.根据权利要求1至13中任一项所述的靶在物理气相沉积方法中用于将薄层沉积在衬底上的应用。
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| CN106756849A (zh) * | 2016-12-21 | 2017-05-31 | 深圳先进技术研究院 | 一种具有过渡金属硼化物涂层的pcb用微钻及其制备方法 |
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| DE3512986A1 (de) * | 1985-04-11 | 1986-10-16 | Kernforschungszentrum Karlsruhe Gmbh, 7500 Karlsruhe | Viellagige, hochverschleissfeste hartstoffschutzschicht fuer metallische, stark beanspruchte oberflaechen oder substrate |
| JPH09202966A (ja) * | 1996-01-23 | 1997-08-05 | Nippon Seimitsu Kk | 薄膜形成方法 |
| DE10005612A1 (de) * | 2000-02-09 | 2001-08-16 | Hauzer Techno Coating Europ B | Verfahren zur Herstellung eines Gegenstandes und Gegenstand |
| US7857948B2 (en) * | 2006-07-19 | 2010-12-28 | Oerlikon Trading Ag, Trubbach | Method for manufacturing poorly conductive layers |
| JP2008179853A (ja) | 2007-01-24 | 2008-08-07 | Hitachi Tool Engineering Ltd | ホウ化物含有ターゲット材 |
| US8821701B2 (en) * | 2010-06-02 | 2014-09-02 | Clifton Higdon | Ion beam sputter target and method of manufacture |
| 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 |
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2018
- 2018-04-20 AT ATGM50075/2018U patent/AT16481U1/de unknown
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2019
- 2019-04-12 CN CN201980026614.8A patent/CN112236403B/zh active Active
- 2019-04-12 EP EP19717489.9A patent/EP3781538B1/de active Active
- 2019-04-12 JP JP2020555911A patent/JP7425741B2/ja active Active
- 2019-04-12 WO PCT/EP2019/059517 patent/WO2019201796A1/de active Application Filing
- 2019-04-16 TW TW108113201A patent/TWI750469B/zh active
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| US4259119A (en) * | 1979-03-27 | 1981-03-31 | Director-General Of The Agency Of Industrial Science And Technology | Boride-based refractory materials |
| US4546089A (en) * | 1982-12-30 | 1985-10-08 | Corning Glass Works | Group 4b boride and VB2 /YB2 |
| CN1680215A (zh) * | 2005-01-14 | 2005-10-12 | 李根法 | 生产结构陶瓷的共晶复合粉末烧结助剂及其制备方法 |
| CN102869807A (zh) * | 2010-05-04 | 2013-01-09 | 攀时欧洲公司 | 二硼化钛靶子 |
| CN106756849A (zh) * | 2016-12-21 | 2017-05-31 | 深圳先进技术研究院 | 一种具有过渡金属硼化物涂层的pcb用微钻及其制备方法 |
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Also Published As
| Publication number | Publication date |
|---|---|
| JP7425741B2 (ja) | 2024-01-31 |
| EP3781538B1 (de) | 2024-09-04 |
| TWI750469B (zh) | 2021-12-21 |
| JP2021521335A (ja) | 2021-08-26 |
| AT16481U1 (de) | 2019-10-15 |
| WO2019201796A1 (de) | 2019-10-24 |
| CN112236403A (zh) | 2021-01-15 |
| EP3781538A1 (de) | 2021-02-24 |
| TW201943866A (zh) | 2019-11-16 |
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