CN112639159A - Mn-Ta-W-Cu-O系溅射靶及其制备方法 - Google Patents

Mn-Ta-W-Cu-O系溅射靶及其制备方法 Download PDF

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CN112639159A
CN112639159A CN201980058202.2A CN201980058202A CN112639159A CN 112639159 A CN112639159 A CN 112639159A CN 201980058202 A CN201980058202 A CN 201980058202A CN 112639159 A CN112639159 A CN 112639159A
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powder
sputtering target
atomic
target
raw material
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CN112639159B (zh
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加守雄一
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Dexerials Corp
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Dexerials Corp
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Abstract

提供溅射靶及其制备方法，所述溅射靶是在成分组成中含有Mn、Ta、W、Cu和O的Mn‑Ta‑W‑Cu‑O系溅射靶，相对密度为90%以上，并且含有Mn4Ta2O9的结晶相。

Description

Mn-Ta-W-Cu-O系溅射靶及其制备方法
技术领域
本发明涉及特别是对光信息记录介质的记录层的形成有用的Mn-Ta-W-Cu-O系溅射靶及其制备方法。
背景技术
近年来，在光信息记录介质(光盘)的领域中，随着所处理的数据的增大等，要求光盘的大容量化。光盘大致分为只读和记录型，记录型进一步细分为一次写入型和可重写型这2类。作为一次写入型的记录层材料，以往广泛研究了有机色素材料，但随着近年来的大容量化，无机材料也得到广泛研究。
作为使用无机材料的有用的记录方式，有利用以下事实的记录方式：通过对含有分解温度低的无机氧化物的记录层照射激光，记录层的物性变化，光学常数随之变化。作为无机氧化物材料，钯氧化物得到实用化。但是，由于Pd为贵金属，材料成本高，所以期望开发可代替钯氧化物而以低廉的材料成本实现的记录层。
作为以低廉的材料成本得到充分良好的记录特性的记录层，开发了由锰氧化物系材料构成的记录层。例如，在专利文献1中，公开了含有锰氧化物和W等多种无机元素的记录层以及为了形成该记录层而使用的溅射靶。
现有技术文献
专利文献
专利文献1：国际公开第2013/183277号。
发明内容
发明所要解决的课题
在这里，作为用于形成前述由锰氧化物和W等多种无机元素构成的记录层的溅射法，有使用由各自的元素构成的多个溅射靶的多元溅射法和使用含有多种元素的1片复合溅射靶的方法。在专利文献1中，公开了多元溅射法，但存在不仅装置大型化而导致成本上升，而且容易产生组成偏差的缺点。因此，优选使用1片复合溅射靶的溅射。另外，从生产能力的观点出发，与高频溅射相比，期望使用直流(DC)溅射。
但是，在由锰氧化物和W等多种无机元素构成的复合溅射靶中，容易含有WMnO4等绝缘粒。在DC溅射中，由于对复合溅射靶施加直流电压，所以在因复合溅射靶中的绝缘粒的影响而得不到充分的导电性的情况下，有产生异常放电(电弧)之虞。由于该成膜中的异常放电，对记录层造成损害，导致成品率降低。
本发明鉴于上述情况而成，其目的在于，提供在供DC溅射时抑制异常放电，并且可稳定地成膜的Mn-Ta-W-Cu-O系溅射靶及其制备方法。
解决课题的手段
为了达成上述目的，本发明提供一种溅射靶，所述溅射靶是在成分组成中含有Mn、Ta、W、Cu和O的Mn-Ta-W-Cu-O系溅射靶，相对密度为90%以上，并且含有Mn4Ta2O9的结晶相。
所述成分组成中，相对于合计100原子%的除O以外的构成元素，Ta和W合计的比例可低于65原子%。
所述溅射靶在所述成分组成中还可含有Zn。
所述溅射靶在所述成分组成中还可含有选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素。
相对于合计100原子%的除O以外的构成元素，所述选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素的合计含有率可为8原子%~70原子%。
另外，本发明提供一种制备方法，所述制备方法是所述Mn-Ta-W-Cu-O系溅射靶的制备方法，包括：混合工序，其中，将含有含锰粉末、金属钽粉末、含钨粉末和含铜粉末的混合粉末湿式混合10小时以上；和烧结工序，其中，在所述混合工序之后对所述混合粉末施加550kgf/cm2以上的压力并在750℃~950℃的温度下进行烧结。
所述含锰粉末可为锰氧化物粉末，所述含钨粉末可为金属钨粉末，所述含铜粉末可为金属铜粉末。
所述混合粉末还可含有锌氧化物粉末。
所述混合粉末还可含有由选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素的单质或化合物构成的粉末。
发明的效果
根据本发明，可提供在供DC溅射时抑制异常放电，并且可稳定地成膜的Mn-Ta-W-Cu-O系溅射靶及其制备方法。
附图说明
[图1] 表示实施例1和比较例1所涉及的溅射靶的X射线衍射谱图的图。
具体实施方式
以下，对本实施方式进行详细的说明。
[Mn-Ta-W-Cu-O系溅射靶]
本实施方式所涉及的Mn-Ta-W-Cu-O系溅射靶(以下简称为“靶”。)在成分组成中含有Mn、Ta、W、Cu和O，相对密度为90%以上，并且含有Mn4Ta2O9的结晶相。
根据本实施方式所涉及的靶，在供DC溅射时抑制异常放电，并且可稳定地成膜。
作为本实施方式所涉及的靶的成分比，无特殊限制，可根据目的适当选择。例如，相对于合计100原子%的除O(氧)以外的构成元素，Mn可为5原子%~40原子%，Ta可为10原子%~35原子%，W可为5原子%~30原子%，Cu可为5原子%~30原子%。
本实施方式所涉及的靶中，相对于合计100原子%的除O以外的构成元素，优选Ta和W合计的比例低于65原子%，也可低于60原子%，还可低于55原子%。相对于合计100原子%的除O以外的构成元素，与Ta和W合计的比例为65原子%以上相比，低于65原子%的情况有可容易地将相对密度调整为90%以上的倾向。关于下限，无特殊限制，但相对于合计100原子%的除O以外的构成元素，Ta和W合计的比例优选为25原子%以上。
本实施方式所涉及的靶在成分组成中还可含有Zn。关于成分比，无特殊限制，可根据目的适当选择。例如，相对于合计100原子%的除O以外的构成元素，Zn可为1原子%~35原子%。
本实施方式所涉及的靶中，还可根据需要含有其它的成分组成。通过适当含有其它的元素，例如在为了形成信息记录介质的记录层而使用靶的情况下，可调整记录层的透射率、反射率和记录灵敏度。作为其它的元素，例如可列举出选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素。
在含有选自上述Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素的情况下，其合计的含有率，例如在靶的构成元素中，相对于合计100%的除O以外的构成元素，可设为8原子%~70原子%。
另外，本实施方式所涉及的靶含有Mn4Ta2O9的结晶相。
靶中含有的结晶相可通过X射线衍射法来确认。靶的X射线衍射谱图的取得可依据常规方法来进行。例如，可以使用Rigaku Corporation制的SmartLab，对靶表面进行θ-2θ扫描，从而取得谱图。X射线衍射的测定条件可根据靶适当确定，例如可从以下的条件范围内选择：
X射线源：Cu-Kα射线
输出设定：20kV~100kV、10mA~100mA
测角范围：2θ=5°~80°
扫描速度：1°~4°(2θ/min)、连续扫描
发散狭缝：0.5°~2°
散射狭缝：0.5°~2°
进光狭缝：0.1mm~0.5mm。
靶的主要结晶相的衍射峰在以下的范围内被检出：
Mn4Ta2O9的衍射峰：31.5°±0.3°
MnTa2O6的衍射峰：29.7°±0.3°
W的衍射峰：40.26°±0.3°
MnO的衍射峰：35.16°±0.3°、40.99°±0.3°、59.18°±0.3°
MnWO4的衍射峰：29.8°±0.3°、30.23°±0.3°
ZnO的衍射峰：36.3°±0.3°
Cu的衍射峰：43.47°±0.3°、50.67°±0.3°。
作为表示本实施方式所涉及的靶为高密度的指标，在本说明书中使用相对密度。靶的相对密度为90%以上，越高越优选。
需说明的是，相对密度是指，将靶的原料成分烧结后的实测密度相对于假设将靶的原料粉100%填充而计算的情况下的假想密度的比例。为了计算相对密度，首先进行靶的尺寸测定和重量测定，计算实测密度。接着，使用以下的计算式计算相对密度：
相对密度(%)=(烧结体的实测密度/假想密度)×100。
需说明的是，本实施方式所涉及的靶的形状无任何限定，可制成圆盘状、圆筒状、四边形板状、长方形板状、正方形板状等任意的形状，可根据靶的用途适当选择。另外，关于靶的宽度和纵深的大小(在圆形的情况下为直径)，也可在mm级~m级程度的范围内根据靶的用途适当选择。例如，在靶为圆形的情况下，通常直径为50mm~300mm左右。厚度也是同样的，但通常为1mm~20mm左右。
另外，虽然靶特别是对光信息记录介质的记录层的形成有用，但用途无任何限定。
[靶的制备方法]
接下来，对本实施方式所涉及的靶的制备方法进行说明。本实施方式所涉及的制备方法包括混合工序和烧结工序。
首先，在混合工序中，将含有含锰粉末、金属钽粉末、含钨粉末和含铜粉末的混合粉末湿式混合10小时以上。
作为含锰粉末，可根据目的适当选择，可列举出由Mn的单质或化合物构成的粉末等。其中，优选锰氧化物。作为锰氧化物，例如可使用Mn3O4、Mn2O3、MnO、MnO2、MnO3、Mn2O7等。它们可单独使用1种，或将2种以上并用。在上述锰氧化物中，根据烧结温度与熔点的关系，优选Mn3O4。
作为含锰粉末的平均粒径，无特殊限定，例如可设为3μm~15μm左右。
作为金属钽粉末的平均粒径，无特殊限定，例如可设为1μm~53μm左右。
作为含钨粉末，可根据目的适当选择，例如可列举出由W的单质构成的金属钨粉末等。
作为含钨粉末的平均粒径，无特殊限定，例如可设为1μm~10μm左右。
作为含铜粉末，可根据目的适当选择，例如可列举出由Cu的单质构成的金属铜粉末等。
作为含铜粉末的平均粒径，无特殊限定，例如可设为1μm~50μm左右。
在上述混合粉末中也可含有锌氧化物粉末。作为锌氧化物粉末，例如可使用ZnO。
作为锌氧化物粉末的平均粒径，无特殊限定，例如可设为0.1μm~3μm左右。
另外，也可根据所制备的靶的所期望的目的，在混合粉末中含有上述含锰粉末、金属钽粉末、含钨粉末、含铜粉末和锌氧化物粉末以外的其它的粉末。作为其它的粉末，例如可列举出由选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素的单质或化合物构成的粉末。
作为湿式混合的方法，无特殊限制，可根据目的适当选择，例如可列举出使用以往公知的球磨装置的湿式混合方法等。
湿式混合时间设为10小时以上。通过将混合时间设为10小时以上，可将混合粉末充分地混合。特别是在使用锰氧化物作为含锰粉末的情况下，导致了促进烧结中的锰氧化物的固相反应，抑制烧结后的氧化锰的结晶相的残留。混合时间优选设为12小时以上，更优选设为16小时以上，进一步优选设为20小时以上。若混合24小时，则混合的效果饱和。
接着，在烧结工序中在550kgf/cm2以上的压力、750℃~950℃的温度下将混合粉末烧结。需说明的是，1kgf/cm2相当于98.1kPa。
作为烧结法，无特殊限制，可根据目的适当选择，例如可列举出在惰性气体气氛中的热压、热等静压法(HIP法：Hot Isostatic Pressing)等。
关于烧结时施加的压力，只要是550kgf/cm2以上即可。优选为600kgf/cm2以上，更优选为700kgf/cm2以上，进一步优选为800kgf/cm2以上。虽然也取决于靶的成分组成等其它的烧结条件，但若将烧结时的压力设为低于550kgf/cm2，则难以使靶的相对密度为90%以上。
关于烧结温度，只要是750℃~950℃即可，也可为800℃~900℃。
烧结时间无特殊限定，可适当选择，且可设为通常进行的1小时~6小时左右的烧结时间。
经过以上工序，可制备相对密度为90%以上、并且含有Mn4Ta2O9的结晶相的Mn-Ta-W-Cu-O系溅射靶。
需说明的是，除了上述混合工序和烧结工序以外，本实施方式所涉及的制备方法也可包括其它的工序。作为其它的工序，例如可列举出为了形成溅射靶的形状而进行的混合粉末的成型工序。
实施例
接下来，对本发明的实施例进行说明，但本发明并不限定于这些实施例。
[溅射靶的制备方法]
<实施例1>
在实施例1中，作为原料粉末，准备以下粉末。
Mn3O4粉末(纯度：99.9%以上，平均粒径：10μm)
W粉末(纯度：99.9%以上，平均粒径：5μm)
Ta粉末(纯度：99.9%以上，平均粒径：6μm)
Cu粉末(纯度：99.9%以上，平均粒径：30μm)
称量上述原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=25:30:25:20(原子%)。将秤量的各原料粉末连同各原料粉末的合计重量的0.5倍的氧化锆球(直径为5mm)和0.5倍的乙醇放入容器中，用球磨装置，进行20小时的湿式混合。使用孔径为2mm的筛，从含有经混合的上述原料粉末的浆料溶液中分离氧化锆球。将浆料溶液加热干燥，使用孔径为250μm的筛进行破碎，得到混合粉末。接着，对于上述混合粉末，在850℃的烧结温度下施加2小时、800kgf/cm2的压力，从而在氩气氛中进行热压，制作了溅射靶。溅射靶的形状为圆盘状，尺寸为直径50mm。
<实施例2>
在实施例2中，除了实施例1中使用的原料粉末以外，还使用以下原料粉末。
ZnO粉末(纯度：99.9%以上，平均粒径：2μm)
称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu:Zn=20:30:25:15:10(原子%)，并将烧结温度设为800℃，除此之外，通过与实施例1相同的方法制作溅射靶。
<实施例3>
在实施例3中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=25:25:25:25(原子%)，并通过与实施例1相同的方法制作溅射靶。
<实施例4>
在实施例4中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=25:20:25:30(原子%)，并通过与实施例1相同的方法制作溅射靶。
<实施例5>
在实施例5中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=30:20:20:30(原子%)，并通过与实施例1相同的方法制作溅射靶。
<实施例6>
在实施例6中，使用与实施例2相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu:Zn=25:20:20:25:10(原子%)，并将烧结温度设为800℃，除此之外，通过与实施例1相同的方法制作溅射靶。
<实施例7>
在实施例7中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=20:30:30:20(原子%)，并通过与实施例1相同的方法制作溅射靶。
<实施例8>
在实施例8中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例与实施例1相同，并将烧结温度设为800℃，除此之外，通过与实施例1相同的方法制作溅射靶。
<实施例9>
在实施例9中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例与实施例1相同，并将烧结时的压力设为600kgf/cm2，除此之外，通过与实施例1相同的方法制作溅射靶。
<比较例1>
在比较例1中，代替实施例1中使用的Ta粉末，使用以下原料粉末。
Ta2O5粉末(纯度：99.9%以上，平均粒径：4μm)
称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=25:30:25:20(原子%)，并将烧结温度设为1050℃，将烧结时的压力设为500kgf/cm2，除此之外，通过与实施例1相同的方法制作溅射靶。
<比较例2>
在比较例2中，除了比较例1中使用的原料粉末以外，还使用以下原料粉末。
ZnO粉末(纯度：99.9%以上，平均粒径：2μm)
称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu:Zn=20:30:25:15:10(原子%)，并通过与比较例1相同的方法制作溅射靶。
<比较例3>
在比较例3中，使用与比较例1相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=20:30:35:15(原子%)，并通过与比较例1相同的方法制作溅射靶。
<比较例4>
在比较例4中，使用与比较例1相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=20:30:30:20(原子%)，并通过与比较例1相同的方法制作溅射靶。
<比较例5>
在比较例5中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例为Mn:W:Ta:Cu=20:30:35:15(原子%)，并通过与实施例1相同的方法制作溅射靶。
<比较例6>
在比较例6中，使用与实施例1相同的原料粉末，称量原料粉末，使得各含有金属的比例与实施例1相同，并将烧结时的压力设为500kgf/cm2，除此之外，通过与实施例1相同的方法制作溅射靶。
[评价]
对于在上述实施例1~9和比较例1~6中制作的溅射靶，进行结晶相中含有的Ta系复合氧化物的鉴别、相对密度测定和异常放电次数的测定。各评价如下进行。将得到的评价结果示出于表1中。
<结晶相中含有的Ta系复合氧化物的鉴别>
通过X射线衍射法，进行溅射靶的结晶相中含有的Ta系复合氧化物的鉴别。在X射线衍射中，使用Rigaku Corporation制的SmartLab，进行θ-2θ扫描，从而得到X射线衍射谱图。作为代表例，将实施例1和比较例1所涉及的溅射靶的X射线衍射谱图示出于图1中。试验条件如下所示：
X射线源：Cu-Kα射线
输出设定：30kV、15mA
测角范围：2θ=15°~70°
扫描速度：2°(2θ/min)、连续扫描
发散狭缝：1°
散射狭缝：1°
进光狭缝：0.3mm。
<相对密度>
为了计算在上述实施例1~9和比较例1~6中制作的溅射靶的相对密度，进行溅射靶的尺寸测定和重量测定，计算实测密度。接着，使用以下的计算式计算相对密度：
相对密度(%)=(烧结体的实测密度/烧结体的假想密度)×100。
<异常放电次数的测定>
用In焊剂将在上述实施例1~9和比较例1~6中制作的溅射靶粘接在无氧铜制的垫板上。将这些溅射靶安装在溅射装置上，进行真空排气至1×10-4Pa以下后，导入Ar气和O2气，使装置内压力为0.3Pa。氧的比例(O2/Ar+O2)设为70%。用DC电源施加5W/cm2的电力，进行30分钟的溅射，利用电弧计数器测定溅射中的异常放电的次数。
[表1]
Figure DEST_PATH_IMAGE002
根据以上结果，确认含有Mn4Ta2O9的结晶相、并且相对密度为90%以上的Mn-Ta-W-Cu-O系溅射靶可抑制异常放电次数。
另外，比较使用相同的原料粉末在相同的烧结条件下制作的实施例1、5、7和比较例5时，确认有Ta和W的含有比越高，则相对密度越低的倾向。
此外，比较除了烧结时的压力以外，利用完全相同的条件制作的实施例1、9和比较例6时，确认有烧结时的压力越高，则相对密度越高的倾向。

Claims (9)

1.溅射靶，所述溅射靶是在成分组成中含有Mn、Ta、W、Cu和O的Mn-Ta-W-Cu-O系溅射靶，
相对密度为90%以上，并且含有Mn4Ta2O9的结晶相。
2.根据权利要求1所述的溅射靶，其中，相对于合计100原子%的除O以外的构成元素，Ta和W合计的比例低于65原子%。
3.根据权利要求1或2所述的溅射靶，其中，在所述成分组成中还含有Zn。
4.根据权利要求1~3中任一项所述的溅射靶，其中，在所述成分组成中还含有选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素。
5.根据权利要求4所述的溅射靶，其中，相对于合计100原子%的除O以外的构成元素，所述选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素的合计含有率为8原子%~70原子%。
6.根据权利要求1~5中任一项所述的Mn-Ta-W-Cu-O系溅射靶的制备方法，所述制备方法包括：
混合工序，其中，将含有含锰粉末、金属钽粉末、含钨粉末和含铜粉末的混合粉末湿式混合10小时以上；和
烧结工序，其中，在所述混合工序之后对所述混合粉末施加550kgf/cm2以上的压力并在750℃~950℃的温度下进行烧结。
7.根据权利要求6所示的制备方法，其中，所述含锰粉末为锰氧化物粉末，所述含钨粉末为金属钨粉末，所述含铜粉末为金属铜粉末。
8.根据权利要求6或7所述的制备方法，其中，所述混合粉末还含有锌氧化物粉末。
9.根据权利要求6~8中任一项所述的制备方法，其中，所述混合粉末还含有由选自Mg、Ag、Ru、Ni、Zr、Mo、Sn、Bi、Ge、Co、Al、In、Pd、Ga、Te、V、Si、Cr和Tb的至少1种元素的单质或化合物构成的粉末。
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