CN112831760A - 具有改进结构的NiW(X)溅射靶 - Google Patents
具有改进结构的NiW(X)溅射靶 Download PDFInfo
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- 238000005477 sputtering target Methods 0.000 title claims description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 27
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 18
- 239000003870 refractory metal Substances 0.000 claims abstract description 14
- 150000002739 metals Chemical class 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 229910052718 tin Inorganic materials 0.000 claims abstract description 10
- 238000005259 measurement Methods 0.000 claims abstract description 4
- 238000000634 powder X-ray diffraction Methods 0.000 claims abstract description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 8
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 description 18
- 239000000843 powder Substances 0.000 description 15
- 238000005507 spraying Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000007750 plasma spraying Methods 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- 238000007751 thermal spraying Methods 0.000 description 4
- 238000001513 hot isostatic pressing Methods 0.000 description 3
- 238000005546 reactive sputtering Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 229910017488 Cu K Inorganic materials 0.000 description 1
- 229910017541 Cu-K Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种溅射靶，该溅射靶包含Ni、W和任选的一种或多种选自难熔金属、Sn、Al和Si的另外的金属X，其具有0.4以上的归一化的峰强度比PIR＝INi/IW·(AW+Ax)/ANi其中，INi是Ni(111)峰的强度，IW是W(110)峰的强度，Aw是W在靶中的原子百分比分数，Ax是一种或多种选自难熔金属、Sn、Al和Si的另外的金属在靶中的总原子百分比分数，ANi是Ni在靶中的原子百分比分数，并且其中，峰的强度通过使用Cu‑Kalpha照射的X射线粉末衍射测定。
Description
技术领域
本发明涉及一种溅射靶，该溅射靶包括Ni、W和任选的一种或多种选自难熔金属、Sn、Al和Si的另外的金属X。
背景技术
NiW靶用于电致变色应用，最近特别是用在管状形式中。例如，US 2017/0003564A1公开了基于NiW(X)-氧化物的对电极用于电致变色玻璃的用途，其中X是可选的附加元素，例如Ta或Nb。
AT14157U1公开了通过使用粉末冶金路线来生产NiW溅射靶，该粉末冶金路线包括在1100至1450℃下对粉末混合物进行热等静压(HIP)，并且明确地教导了由于其所谓的缺点而不再使用热喷涂。但是，套管的HIP和粘合很昂贵，而且，如果靶长度超过0.5m，则会导致分段的靶。由于NiW靶用于氧反应溅射，由于分段的靶结构而导致的粘结间隙将导致重新沉积和电弧风险。
NiW(X)靶的另一种可能的制造技术是元素粉末混合物的等离子喷涂。然而，在这样的过程中，与使用HIP工艺相比，更多的氧被引入到靶中。此外，一旦超过一定厚度(通常为3至4mm)，直接喷涂工艺就会导致靶材料层裂纹。NiW(X)喷涂层中的应力很高，以至于一旦在靶层中形成裂纹，衬管就会变形为椭圆形。
发明内容
因此，本发明的目的是提供一种改进的NiW(X)溅射靶材料，其允许生产具有增加的厚度以便提供更长的靶寿命并由此延长溅射设备的运行时间的无裂纹靶。此外，一个目的是提供一种NiW(X)溅射靶材料，该材料允许生产具有增加的长度而没有会引起电弧问题的粘结间隙的靶。
因此，本发明提供了一种溅射靶，该溅射靶包含Ni、W和任选的一种或多种选自难熔金属、Sn、Al和Si的另外的金属X，其具有0.4以上的归一化的峰强度比
PIR＝INi/IW·(AW+Ax)/ANi
其中，
INi是Ni(111)峰的强度，
IW是W(110)峰的强度，
Aw是W在靶中的原子百分比分数，
Ax是一种或多种选自难熔金属、Sn、Al和Si的另外的金属在靶中的总原子百分比分数，
ANi是Ni在靶中的原子百分比分数，
并且其中，峰的强度通过使用Cu-Kalpha照射的X射线粉末衍射测定。
可以将本发明的溅射靶制造成增加的厚度，从而在使用时提供更长的靶寿命，并且在反应溅射期间显示出减少的电弧。此外，降低了在靶制造过程中由于裂纹产生的风险，并且使由于破裂的和报废的靶导致的生产成本增加最小化。
可以通过如下所述的具有改善的沉积条件的热喷涂工艺获得本发明的溅射靶。使用导致本发明靶的PIR的改善的条件，厚度通常可以增加30％至50％，即，通过等离子体喷涂可以获得厚度大于4mm，优选大于5mm的无裂纹靶。
具体实施方式
在本发明的意义中，难熔金属是Ti、V、Cr、Mn、Zr、Nb、Mo、Ru、Rh、Hf、Ta、Re、Os和Ir。
优选地，根据本发明的溅射靶的归一化的峰强度比为0.42以上，更优选为0.44以上，再更优选为0.45以上。
对于其中溅射靶包含另外的金属X(例如Ta)，即X的分数＞0原子％的实施方式，溅射靶优选具有0.42以上，更优选0.45以上，更优选0.46以上，最优选0.49以上的归一化的峰强度比。
通常，根据本发明的溅射靶具有不大于1.0或不大于0.80的归一化的峰强度比。
溅射靶中的原子比Ni/W优选为0.5至10，更优选为0.75至9，最优选为1至8。
除Ni和W之外，溅射靶中包含的任选的另外的金属X优选选自难熔金属。
除Ni和W之外，溅射靶中包含的任选的另外的金属X更优选选自Ta、Nb和Mo，最优选地，X为Ta。
在一个优选的实施方式中，溅射靶包括Ni、W和选自难熔金属、Sn、Al和Si的另一种金属X，或由Ni、W和选自难熔金属、Sn、Al和Si的另一种金属X组成，更优选地，溅射靶包括Ni、W和选自难熔金属的一种金属X，或由Ni、W和选自难熔金属的一种金属X组成，还更优选地，溅射靶包括Ni、W和选自Ta、Nb和Mo的一种金属X，或由Ni、W和选自Ta、Nb和Mo的一种金属X组成，最优选地，溅射靶包括Ni、W和为Ta的一种金属X，或由Ni、W和为Ta的一种金属X组成。
在另一个优选的实施方式中，溅射靶由Ni和W组成。
优选地，在根据本发明的溅射靶中，Ni以45至90原子％，更优选50至85原子％的量存在。
在优选实施方式中，其中，溅射靶包括Ni、W和在如前所定义的任何实施方式中的一种或多种金属X，或溅射靶由Ni、W和在如前所定义的任何实施方式中的一种或多种金属X组成，Ni优选以45至85原子％的量存在，更优选以50至80原子％的量存在。
在溅射靶由Ni和W组成的优选实施方式中，溅射靶中的原子比Ni/W优选为0.5至10，更优选为0.75至8，最优选为1至6。
优选地，在根据本发明的溅射靶中，W以7至50原子％，更优选10至45原子％，还更优选12至40原子％，最优选15至35原子％的量存在。
在优选实施方式中，其中，溅射靶包括Ni，W和在如前所定义的任何实施方式中的一种或多种金属X或溅射靶由Ni，W和在如前所定义的任何实施方式中的一种或多种金属X组成，W优选以7至50原子％，更优选10至40原子％，还更优选12至35原子％的量存在。
在优选实施方式中，其中，溅射靶包括Ni、W和在如前所定义的任何实施方式中的一种或多种金属X，或溅射靶由Ni、W和在如前所定义的任何实施方式中的一种或多种金属X组成，X优选以3至20原子％的量存在，更优选以5至17原子％的量存在。
例如，在溅射靶由Ni、W和Ta组成的优选实施方式中，Ta优选以3至20原子％的量存在，更优选以5至17原子％的量存在。
本发明的溅射靶的厚度优选大于4mm，更优选大于5mm。
通常，本发明的溅射靶的厚度不大于20mm，或者不大于10mm。
本发明的溅射靶的长度优选大于1m，更优选大于1.5m。
通常，本发明的溅射靶的长度不大于4m，或者不大于3m。
通常，溅射靶是其中基质具有管状形状的管状靶。作为管状基质，通常使用非磁性不锈钢管。
本发明的NiW(X)溅射靶可以用用于形成溅射靶的方法生产，所述方法包括在相对“冷”的条件下，例如在实施例中举例说明的，热喷涂将要在溅射靶中含有的金属的粉末混合物。
因此，例如，可以使在喷涂过程中向粉末中添加的热量保持相对较小和/或为了将靶层沉积在基体上，可以将所形成的靶层的温度选择为具有较低的温度，例如40℃以下。
另一方面，温度应>18℃，因为在膜沉积过程中溅射靶的使用会使得溅射力产生热。该热量导致衬管和靶层热膨胀。由于SST衬管显示出比靶层更强的热膨胀，因此如果在等离子喷涂过程中在过低的温度下沉积靶层，则会产生裂纹风险。
可以相信，与没有Ni的产品的喷涂过程相比，在喷涂NiW(X)靶层的过程中，会释放大量的热量，因此现有技术的喷涂过程会在喷涂的NiW(X)靶层中产生应力，并且可能还会引入大量的金属间相。
此外，相信在实施例中举例说明的改进的喷涂方法中，在所生成的溅射靶中可以增加未反应的，即元素Ni(和W)的分数。认为金属间相的体积分数也降低了。这些效果有助于降低所形成靶的应力水平，从而可以生产出较厚的靶。
改进方法和现有技术方法的XRD图谱都没有揭示出可归因于金属间相的峰，而SEM分析清楚地证明了这两种情况下它们的存在。认为元素金属滴的快速淬灭和较短的反应时间会防止靶中金属间区域的充分结晶。
可以使用输出功率为65kW以下的燃烧器，以及使用160g/min以下的粉末进给率执行热喷涂。
可以以2.45g/(kW·min)以上，更优选2.5g/(kW·min)以上的粉末进给率/燃烧器输出速率进行热喷涂。
优选地，在用于喷涂的粉末混合物中使用的粉末的粒度为30至120μm。
在用于制造本发明的NiW(X)溅射靶的热喷涂工艺中，通常将数千至高达10,000ppm的氧气引入靶材料中。然而，由于NiW(X)靶用于在氧气存在下通过反应溅射形成氧化层，因此这并不是不利的。
定义/测量方法
a)归一化的峰强度比(PIR)
通过评估所生成靶的Cu-Kalpha XRD图谱来确定PIR。
为此，将hkl＝(111)的在2θ＝44.5°处的最强Ni线的峰强度INi与hkl＝(110)的在2θ＝40.3°处的最强W线的峰强度IW相比较。
归一化的峰强度比PIR的计算方法如下：
PIR＝INi/IW·(AW+Ax)/ANi
其中，
INi是Ni的(111)峰的强度，IW是W的(110)峰的强度，Aw是W在靶中的原子百分比分数，Ax是一种或多种选自难熔金属、Sn、Al和Si，例如Ta的另外的金属X在靶中的总原子百分比分数，且ANi是Ni在靶中的原子百分比分数。
由于Ni和W或其他元素在喷涂过程中的沉积效率不同，用于生产靶的粉末混合物的元素组分和靶本身之间可能会发生位移。需要明确的是：ANi、Ax和AW是指实际靶组分，例如可用ICP或XRF测量。
b)金属粉末粒度的测量方法
根据国际标准ISO 13320“颗粒尺寸分析–激光衍射方法”，使用激光衍射系统“Fritsch ANALYSETTE 22 MicroTec plus”，通过激光衍射测量干燥金属粉末的粒度分布。
实施例
为了说明本发明，实施了若干实施例和比较例。通过在管式混合器中混合元素粉末3小时来制备喷涂粉末。通常，粒度范围为30至120μm的粉末会产生合适的结果。特别是对于W，应避免太大的粒度。这些粉末混合物用于在外径(OD)为133mm，长度为550mm，末端被罩环覆盖的SST管上等离子喷涂。
在表1中列出了比较Ni/W/Ta靶和根据本发明的靶的热喷涂条件。
表1：
*)在沉积靶层期间，通过校准的红外温度计测量靶管的表面。通过与喷枪一起行进，在喷涂区后面50厘米处进行测量。
在下表2中，给出了实施例1和3以及比较例2和4的靶的性质。实施例1和3的靶是使用本发明的喷涂方法制备的，而比较例2和4的靶是使用比较方法制备的，两种方法的条件如表1中所示。
根据沿靶长度是否出现宏观裂纹和/或衬管是否显示椭圆度来评估生产的靶的质量，结果也列于表2中：
“良好”是指：沿靶长度无宏观裂纹，并且无衬管直径133.0>±0.5mm的椭圆度。
“不良”是指：沿靶长度至少有一个宏观裂纹和/或衬管直径133.0>±0.5mm的椭圆度。
表2：
Claims (9)
1.溅射靶，其包含Ni、W和任选的一种或多种选自难熔金属、Sn、Al和Si的另外的金属X，其具有0.4以上的归一化的峰强度比
PIR＝INi/IW .(AW+Ax)/ANi
其中，
INi是Ni(111)峰的强度，
IW是W(110)峰的强度，
Aw是W在所述靶中的原子百分比分数，
Ax是一种或多种选自难熔金属、Sn、Al和Si的另外的金属在所述靶中的总原子百分比分数，
ANi是Ni在所述靶中的原子百分比分数，
并且其中，峰的强度通过使用Cu-Kalpha照射的X射线粉末衍射测定。
2.根据权利要求1所述的溅射靶，其中，所述归一化的峰强度比为0.42以上。
3.根据权利要求1或2所述的溅射靶，其中，所述溅射靶中的原子比Ni/W为0.5至10。
4.根据前述权利要求中任一项所述的溅射靶，其中，所述任选的另外的金属X选自难熔金属。
5.根据前述权利要求中任一项所述的溅射靶，其中，所述任选的另外的金属X选自Ta、Nb和Mo。
6.根据前述权利要求中任一项所述的溅射靶，其中，所述任选的另外的金属X是Ta。
7.根据前述权利要求中任一项所述的溅射靶，其中，Ni以45至90原子％的量存在。
8.根据前述权利要求中任一项所述的溅射靶，其中，W以7至50原子％的量存在。
9.根据前述权利要求中任一项所述的溅射靶，其中，X以3至20原子％的量存在。
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