CN101208451A - 溅射靶及光信息记录介质用薄膜 - Google Patents

溅射靶及光信息记录介质用薄膜 Download PDF

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CN101208451A
CN101208451A CNA2006800227856A CN200680022785A CN101208451A CN 101208451 A CN101208451 A CN 101208451A CN A2006800227856 A CNA2006800227856 A CN A2006800227856A CN 200680022785 A CN200680022785 A CN 200680022785A CN 101208451 A CN101208451 A CN 101208451A
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target
zns
sputtering target
recording medium
information recording
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CN101208451B (zh
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高见英生
矢作政隆
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Nippon Mining and Metals Co Ltd
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    • G11—INFORMATION STORAGE
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    • G11B7/26—Apparatus or processes specially adapted for the manufacture of record carriers
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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Abstract

本发明涉及一种溅射靶，其中，以硫化锌与由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，相对于全部构成成分的硫的比率为5至30重量％，XRD测定的立方晶系ZnS的(111)峰强度I1与六方晶系ZnS的(100)峰强度I2共存并且满足I1＞I2。本发明的目的在于提供在靶制造时或者通过溅射形成膜时可以防止靶破裂的高强度溅射靶及其制造方法，以及得到最适合作为保护膜使用的光信息记录介质用薄膜及其制造方法。

Description

溅射靶及光信息记录介质用薄膜
技术领域
本发明涉及一种溅射靶及光信息记录介质用薄膜(特别是作为保护膜使用)，所述溅射靶具有光信息记录介质保护层用薄膜中的非晶稳定性，在通过溅射形成膜时可以进行直流(DC)溅射，溅射时的电弧发电少并且可以减少由电弧放电而产生的颗粒(起尘)或结核，并且高密度且质量变动少，可以提高批量生产率。
背景技术
近年来，正在开发作为不需要磁头而可重写的高密度光信息记录介质的高密度记录光盘技术，并且引起了高度的关注。该光盘分为ROM(read-only)、R(write-once)、RW(rewritable)三种，特别是在RW(RAM)型中使用的相变化方式引起关注。以下简单地说明使用该相变化型光盘的记录原理。
相变化型光盘，通过激光照射使衬底上的记录薄膜加热升温而引起该记录薄膜的结构上的结晶学相变化(非晶性
Figure S2006800227856D00011
结晶)，进行信息的记录/再生，更具体而言，通过检测其相间的光学常数变化造成的反射率的变化而进行信息的再生。
上述相变化通过照射直径变窄至约数百nm至约数μm的激光而进行。此时，例如1μm的激光束以10m/s的线速度通过时，光盘上某点光照射的时间为100ns，需要在该时间内进行上述相变化与反射率的检测。
另外，为了实现上述结晶学的相变化即非晶与结晶的相变化，不仅对记录层而且对周围的电介质保护层或铝合金反射膜重复进行加热和急冷。
根据这些方面，相变化光盘被设计为用硫化锌-硅氧化物(ZnS/SiO2)类的高熔点电介质的保护层夹住Ge-Sb-Te类等记录薄膜层的两侧、并进一步设置铝合金反射膜的四层结构。
其中，反射层和保护层除要求具有使记录层的非晶部与结晶部的反射率差增大的光学功能以外，还要求具有记录薄膜的耐湿性及热变形的防止功能、以及记录时的热条件控制的功能(参照杂志“光学”26卷1号第9至15页)。
如上所述，高熔点电介质的保护层需要具有对升温和冷却引起的热反复应力的耐性、以及这些热影响对反射膜和其它部位不能产生影响、并且自身薄、低反射率并且具有不变质的强度。从这个意义上说，电介质保护层具有重要作用。
上述电介质保护层是通过通常的溅射法形成的。该溅射法中，使包括正电极和负电极的衬底与靶对置，在惰性气体气氛下在这些衬底与靶间施加高电压产生电场，其利用的原理是：此时电离的电子与惰性气体撞击形成等离子体，该等离子体中的阳离子撞击靶(负电极)表面而驱赶出靶构成原子，该飞出的原子附着到对置的衬底表面上形成膜。
以往，主要在可重写型光信息记录介质的保护层中一般使用的ZnS-SiO2，由于光学特性、热特性、与记录层的密合性等方面具有优良特性，因此被广泛应用。而且，使用这样的ZnS-SiO2等陶瓷靶，以往形成了约数百至约数千的薄膜。
但是，对于这些材料而言，由于靶的体积电阻值高，因此不能通过直流溅射装置成膜，通常使用高频溅射(RF)装置。但是，该高频溅射(RF)装置，不仅装置自身昂贵，而且具有溅射效率差、电力消耗量大、控制复杂、成膜速度慢等很多缺点。
另外，为了提高成膜速度而施加高电力时，衬底温度上升，产生聚碳酸酯制衬底变形的问题。另外，ZnS-SiO2膜厚度厚，因此存在生产量低、成本增加的问题。
可重写型DVD，除激光波长缩短外，还强烈要求重写次数的增加、大容量化、高速记录，上述ZnS-SiO2也存在其它问题。
作为光信息记录介质的重写次数等劣化的原因之一，是以夹放在ZnS-SiO2中的方式配置的记录层材料在反复加热、冷却中，记录层与保护层之间产生空隙。因此，成为引起反射率等特性劣化的重要因素。
为了提高它们的密合性，提出了在记录层与保护层之间设置了以氮化物或碳化物为主成分的中间层的构成，但是随层压数增加产生生产量下降及成本增加的问题。
为了解决上述问题，考虑通过确保比保护层材料ZnS-SiO2更加稳定的非晶性，提高与记录层的密合性。
ZnO基同系物(参照非专利文献1)具有复杂的层状结构，因此具有稳定地保持成膜时的非晶性的特征，另外在使用的波长范围是透明的，并且也具有折射率与ZnS-SiO2接近的特性。
通过向ZnS中添加该ZnO基同系物，可以提高非晶性并且排除绝缘材料SiO2，因此期待可以稳定溅射特性，改善光信息记录介质的特性以及提高生产率。
一般地，作为使用以同系物为主成分的材料作为透明导电材料的例子，可以列举例如：通过激光磨削形成锌-铟类氧化物靶的方法(参照专利文献1)；含有导电性以及蓝色光透过性特别良好的非晶性氧化物的透明导电膜的例子(参照专利文献2)；耐湿性膜形成用靶的例子，其中以In和Zn为主成分，为In2O3(ZnO2)m(m＝2至20)，In与Zn(In/(In+Zn))的原子比为0.2至0.85(参照专利文献3)。
但是，上述形成透明导电膜的材料，作为光信息记录介质用薄膜(特别是作为保护膜使用)未必充分。
另一方面，在ZnS中添加有以ZnO为基础的同系物的复合靶存在的问题是，靶制造时或者高功率溅射时容易破裂。
非专利文献1：技术杂志“固体物理”，李春飞等著，Vol.35，No.1，2000，23至32页“同系物RMO3(ZnO)m(R＝In，Fe；M＝In，Fe，Ga，Al；m＝自然数)的调制结构的电子显微镜观察”
专利文献1：日本特开2000-26119号公报
专利文献2：日本特开2000-44236号公报
专利文献3：日本专利第2695605号公报
发明内容
本发明的目的在于得到在靶制造时或者通过溅射形成膜时可以防止靶破裂的高强度溅射靶及其制造方法，以及最适合作为保护膜使用的光信息记录介质用薄膜及其制造方法。
为了解决上述问题，本发明人进行了广泛深入的研究，结果发现通过采用以ZnS等硫族化锌和ZnO为主成分的复合化合物，并且控制由ZnS与氧化物的反应引起的比通常的纯ZnS更低温度下产生的ZnS的结晶相的重排，可以防止靶的破裂并且提高靶密度，由此无损作为保护膜的特性，可以进一步减少溅射时产生的颗粒或结核，提高膜厚度的均匀性。
基于这些发现，本发明提供了：
1)一种溅射靶，其中，以硫化锌与由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，硫相对于全部构成成分的比率为5至30重量％，XRD测定的立方晶系ZnS的(111)峰强度I1与六方晶系ZnS的(100)峰强度I2共存并且满足I1＞I2；
2)上述1)所述的溅射靶，其中，立方晶系ZnS的(111)峰的半值宽度的平均值为0.25以下，半值宽度的标准偏差为0.06以下；
3)上述1)或2)所述的溅射靶，其中，三价的阳性元素A为选自铝、镓、钇、镧中的一种以上成分的材料；
4)上述1)至3)任一项所述的溅射靶，其中，硫化物相的平均结晶粒径大于氧化物相的平均结晶粒径，并且为10μm以下；
5)上述1)至4)任一项所述的溅射靶，其中，相对密度为85％以上，基于三点弯曲强度(JIS R 1601)的强度平均值为50MPa以上，Weibull系数为5以上；
6)使用上述1)至5)任一项所述的溅射靶形成的光信息记录介质用薄膜。
发明效果
本发明以硫化锌与由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，因此可以实现非晶性的稳定，提高与光信息记录介质的记录层材料的密合性，由此可以提高特性，通过将相对密度提高到85％以上可以进行稳定的DC溅射。
另外，通过调节组成比可以进行DC溅射，具有可以提高成膜速度、提高溅射效率的显著效果。由此，具有可以减少成膜中溅射时产生的颗粒(起尘)或结核，质量变动少，提高批量生产率，并且可以稳定地以低成本制造具有光盘保护膜的光记录介质的显著效果。
另外，靶内的硫化物相的平均结晶粒径为10μm以下，以硫化锌与由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，通过具有这些成分均匀分散的组织，可以稳定溅射，均匀地成膜，另外具有可以形成特性优良的光信息记录介质用薄膜(保护膜)的效果。
具体实施方式
本发明的溅射靶以硫化锌与由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，硫相对于全部构成成分的比率为5至30重量％，由XRD测定的立方晶系ZnS的(111)峰强度I1与六方晶系ZnS的(100)峰强度I2混合存在并且满足I1＞I2。
以硫化锌与由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分的理由，是为了确保非晶稳定性，另外，相对于全部构成成分的硫的比率设定为5至30重量％的理由，同样是为了确保非晶稳定性，并且为了得到良好的光学特性和成膜速度。
另外，由XRD测定的立方晶系ZnS的(111)峰强度I1与六方晶系ZnS的(100)峰强度I2共存的理由，是为了防止破裂。由此，具有可以高速成膜、可以提供难以破裂的靶的显著效果。
在本发明的成分体系中，在通常的单相ZnS或ZnS-SiO2中不产生的低温(约70至约900℃)下产生ZnS的相转变。因此，在以往的ZnS-SiO2中不产生相转变的1000℃附近进行烧结和急冷时，高温相的六方晶系在靶内不均匀分布。已经发现，这种不均匀分布在靶内作为残余应变而积累，变得容易破裂。而且，当低温相与高温相共存时，发现低温相的XRD衍射中的半值宽度平均值为0.25以下，并且优选该半值宽度在靶内均匀。
优选立方晶系ZnS的(111)峰的半值宽度的平均值为0.25以下，半值宽度的标准偏差为0.06以下，由此破裂防止效果更大。关于三价阳性元素A，特别优选为选自铝、镓、钇、镧中的一种以上成分的材料。
另外，本发明的溅射靶中，优选硫化物相的平均结晶粒径大于氧化物相的平均结晶粒径，并且为10μm以下，相对密度为85％以上。这对于防止破裂更加有效。但是，这些条件不是必需要素，而是优选的条件。因此，应该知道本发明也可以应用于上述数值范围以外。
通过使用本发明的溅射靶，具有可以提高生产率、得到质量优良的材料、并且可以稳定地以低成本制造具有光盘保护膜的光记录介质的显著效果。
本发明的溅射靶，通过将各构成元素的氧化物粉末及硫族化物粉末进行常压烧结或者高温加压烧结，可以制造高密度的溅射用靶。烧结时，优选在1050℃以下进行烧结。由此，可以将ZnS的结晶相调节至希望的值，可以防止破裂。另外，在冷却时，优选保持500至850℃或者进行缓慢冷却。
由此，可以更有效地将ZnS(111)的半值宽度调节至希望的值。这些调节与以往的ZnS-SiO2有很大的不同。
另外，在烧结前，将以氧化锌为主成分的氧化物粉末均匀混合后，优选在800至1300℃进行煅烧，另外煅烧后，优选进一步粉碎至1μm以下。烧结可以在真空中或者氩气、氮气等惰性气体气氛中进行。另外，可以使用热压在高温下加压，此时的加压压力优选设定为150kgt/cm2以上。由此，可以得到相对密度为85％以上的溅射靶。
烧结前的氧化物粉末，优选形成以氧化锌为主成分的化合物。这是因为可以提高均匀性、更有效地发挥同系物的优点，使非晶性稳定。另外，烧结前的硫化锌粉末中所含的硫酸化物(硫酸根)是靶产生破裂的原因，因此应该尽可能地减少。
通过使用本发明的溅射靶，具有可以提高生产率、得到质量优良的材料、可以稳定地以低成本制造具有光盘保护膜的光记录介质的显著效果。
本发明的溅射靶的密度提高，可以使孔减少并且使结晶粒微细，可以使靶的溅射面均匀且平滑，因此具有可以减少溅射时的颗粒或结核、并且可以延长靶寿命的显著效果，质量的变动少并且可以提高批量生产率。
实施例
以下，基于实施例和比较例说明本发明，但是，这些例子仅是用来说明的，本发明无论如何不受其限制。即，本发明仅由权利要求的范围所限制，本发明也包括实施例以外的各种变形。
(实施例1至8)
准备相当于4N的5μm以下的In2O3粉和相当于4N的1μm以下的Ga2O3 Al2O3粉、Y2O3粉、La2O3粉、以及相当于4N的平均粒径5μm以下的ZnO粉，按照表1所示摩尔比例进行混合，进行湿式混合并干燥后，在1100℃进行煅烧。
然后，将该复合氧化物粉末与相当于4N的平均粒径5μm以下的ZnS粉按照表1所示的摩尔比例进行混合。混合中，使用湿式球磨混合或者干式高速搅拌混合机使各粉末均匀分散。然后，将该混合粉末填充到碳制模具中，在温度900℃进行热压，形成靶。此时，在700至800℃保持2小时以后，进行缓慢冷却。
该靶的XRD测定的立方晶系ZnS的(111)峰强度I1与六方晶系ZnS的(100)峰强度I2共存，如表1所示，其比(XRDI1/I2)在1.5至12的范围。另外，立方晶系ZnS的(111)峰的半值宽度的平均值为0.18至0.22，该半值宽度的标准偏差在0至0.03的范围。
另外，从靶内任意三处取样测定密度(阿基米德法)，结果相对密度为85至97％，基于三点弯曲强度(JIS R 1601)的强度平均值在55至80MPa的范围，Weibull系数在6至12的范围。
靶内的ZnS相的平均结晶粒径均为4μm，氧化物相的平均结晶粒径在0.8至1.5μm的范围。以上数值均在本发明的目标数值范围内。另外，均未产生靶的破裂。
另外，使用加工为6英寸φ的靶进行溅射。溅射条件是：DC溅射、溅射功率1000W、Ar气压0.5Pa、以目标膜厚1500进行成膜。如表1所示，该成膜试样的折射率为2至2.2(波长633nm)，显示了良好的折射率。另外，非晶稳定性在1.1至1.5的范围，也显示了良好的值。
(比较例1至5)
准备相当于4N的5μm以下的In2O3粉和相当于4N的1μm以下的Ga2O3 Al2O3粉、Y2O3粉(比较例4中未添加)、以及相当于4N的平均粒径5μm以下的ZnO粉，按照表2所示摩尔比例进行混合，进行湿式混合并干燥后，在1100℃进行煅烧。
然后，将该复合氧化物粉末与相当于4N的平均粒径5μm以下的ZnS粉按照表2所示的摩尔比例进行混合。混合中，使用湿式球磨混合或者干式高速搅拌混合机使各粉末均匀分散。然后，将该混合粉末填充到碳制模具中，在温度900至1100℃进行热压，形成靶。如实施例所示，不经过在700至800℃保持2小时以上的过程而进行冷却。
该靶的XRD测定的立方晶系ZnS的(111)峰强度I1与六方晶系ZnS的(100)峰强度I2共存，如表2所示，其比(XRDI1/I2)在比较例1和比较例3中分别为0.6、0.8，在本发明的范围以外。另外，立方晶系ZnS的(111)峰的半值宽度的平均值为0.27至0.30，该半值宽度的标准偏差对于ZnS量在本发明条件以外的比较例1和比较例2中分别为0.07和0.08，在本发明的范围以外。
另外，从靶内任意三处取样测定密度(阿基米德法)，结果比较例5的相对密度为75％，密度显著下降。基于三点弯曲强度(JIS R 1601)的强度平均值，在比较例2和比较例4中分别为42MPa、30MPa。Weibull系数在比较例2和比较例5中分别低至4。
靶内的ZnS相的平均结晶粒径在比较例5中为12μm，在本发明的范围以外。另外，氧化物相的平均结晶粒径在比较例2中为5μm，在本发明的范围以外。比较例1中在制造中产生破裂，比较例2、3和5中靶中产生破裂，没有得到良好的靶。
另外，使用加工为6英寸φ的靶进行溅射。溅射条件是：DC溅射、溅射功率1000W、Ar气压0.5Pa、以目标膜厚1500进行成膜。如表2所示，比较例1在制造中产生靶破裂，因此不能评价。对于其余的成膜试样而言，折射率为2.2至2.3(波长633nm)，显示了良好的折射率。另外，非晶稳定性在比较例2中为3.2，在比较例4中为4.5，均劣化，一部分观察到形成结晶，膜的平坦性受损。
表1
  配合组成mol％   Swt％   XRDI1/I2   XRD I1平均半值宽度   标准偏差   相对密度％   平均强度MPa   Weibull系数  ZnS结晶粒径μm   氧化物相结晶粒径μm   破裂   折射率633nm   膜非晶性稳定性
 实施例1   ZnS∶In2O3∶Ga2O3∶ZnO＝64∶6∶6∶24   18.7   10   0.21   0   90   65   10   4   12   无   2.2   1.5
 实施例2   ZnS∶In2O3∶Ga2O3∶ZnO＝80∶2∶2∶16   25.6   12   0.19   0.02   97   80   12   4   1   无   2.3   1.1
 实施例3   ZnS∶In2O3∶Ga2O3∶ZnO＝50∶9∶15∶26   13.0   5   0.22   0.01   86   60   9   4   1   无   2.3   1.3
 实施例4   ZnS∶In2O3∶Al2O3∶ZnO＝25∶10∶5∶60   7.5   1.5   0.22   0.03   85   55   6   4   0.8   无   2   1.3
 实施例6   ZnS∶In2O3∶Al2O3∶ZnO＝50∶19∶6∶25   12.5   9   0.21   001   90   73   11   4   1.1   无   2.1   1.2
 实施例7   ZnS∶In2O3∶Y2O3∶ZnO＝65∶3∶2∶30   20.7   8   0.2   0.01   89   62   8   4   1.5   无   2.2   1.4
 实施例8   ZnS∶In2O3∶La2O3∶ZnO＝70∶7∶3∶20   20.3   7   0.18   0.02   92   58   10   4   1.5   无   2.2   1.5
 比较例1   ZnS∶In2O3∶Al2O3∶ZnO＝15∶15∶10∶60   4.2   0.6   0.3   0.07   90   52   6   6   0.9   制造中破裂   -   -
 比较例2   ZnS∶In2O3∶Al2O3∶ZnO＝94∶1∶1∶4   30.5   5   0.27   0.08   92   42   4   4   5   靶中破裂   2.3   3.2
 比较例3   ZnS∶In2O3∶Ga2O3∶ZnO＝65∶7∶7∶21   18.4   0.8   0.24   0.05   96   65   10   8   1   靶中破裂   2.2   1.1
 比较例4   ZnS∶In2O3∶ZnO＝60∶10∶30   17.4   7   0.23   0.05   95   60   7   4   1.5   无   2.2   4.5
 比较例5   ZnS∶In2O3∶Y2O3∶ZnO＝75∶3∶7∶15   22.0   20   0.24   0.04   75   30   4   12   1.2   靶中破裂   2.3   1.1
产业实用性
本发明以硫化锌和由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，可以稳定非晶性，提高与光信息记录介质的记录层材料的密合性的特性，并且可以通过相对密度达到85％以上的高密度化从而实现稳定的DC溅射。
另外，通过调节组成比可以进行DC溅射，靶的控制性容易，具有可以提高成膜速度、并且提高溅射效率的显著效果。另外，由此具有可以减少成膜中溅射时产生的颗粒(起尘)或结核，质量变动少并且可以提高批量生产率，可以稳定地以低成本制造具有光盘保护膜的光记录介质的显著效果。
另外，靶内的硫化物相的平均结晶粒径为10μm以下，以硫化锌和由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，具有这些成分均匀分散的组织，由此，溅射稳定，可以均匀地成膜，作为用于形成特性优异的光信息记录介质用薄膜(保护膜)的溅射靶是特别有用的。

Claims (6)

1.一种溅射靶，其中，以硫化锌与由氧化铟、氧化锌及其它三价阳性元素A构成的氧化物为主要成分，硫相对于全部构成成分的比率为5至30重量％，XRD测定的立方晶系ZnS的(111)峰强度I1与六方晶系ZnS的(100)峰强度I2共存并且满足I1＞I2。
2.权利要求1所述的溅射靶，其中，立方晶系ZnS的(111)峰的半值宽度的平均值为0.25以下，半值宽度的标准偏差为0.06以下。
3.权利要求1或2所述的溅射靶，其中，三价的阳性元素A为选自铝、镓、钇、镧中的一种以上成分的材料。
4.权利要求1至3任一项所述的溅射靶，其中，硫化物相的平均结晶粒径大于氧化物相的平均结晶粒径，并且为10μm以下。
5.权利要求1至4任一项所述的溅射靶，其中，相对密度为85％以上，基于三点弯曲强度(JIS R 1601)的强度平均值为50MPa以上，Weibull系数为5以上。
6.使用权利要求1至5任一项所述的溅射靶形成的光信息记录介质用薄膜。
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