CN102597303A - Bi-Ge-O型烧结体溅射靶及其制造方法以及光记录介质 - Google Patents

Bi-Ge-O型烧结体溅射靶及其制造方法以及光记录介质 Download PDF

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CN102597303A
CN102597303A CN201080050662XA CN201080050662A CN102597303A CN 102597303 A CN102597303 A CN 102597303A CN 201080050662X A CN201080050662X A CN 201080050662XA CN 201080050662 A CN201080050662 A CN 201080050662A CN 102597303 A CN102597303 A CN 102597303A
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奈良淳史
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Abstract

本发明涉及一种Bi-Ge-O型烧结体溅射靶以及该靶的制造方法以及光记录介质，所述烧结体溅射靶含有铋（Bi）、锗（Ge）和氧（O），其特征在于，Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75，并且由作为结晶相的Bi12GeO20和Bi4Ge3O12两相构成；特别地提供Bi-Ge-O型烧结体溅射靶以及该靶的制造方法以及光记录介质，所述烧结体溅射靶耐热冲击性优良，可以高功率溅射因此可以预计生产效率大幅改善，并且在溅射时不产生靶的破裂、粉粒的产生少、可以稳定地制作高品质的薄膜，可以得到不产生记录位错误的光记录介质。

Description

Bi-Ge-O型烧结体溅射靶及其制造方法以及光记录介质
技术领域
本发明涉及Bi-Ge-O型烧结体溅射靶及该靶的制造方法以及光记录介质，特别地涉及耐热冲击性优良、可以高功率溅射因此可以预计生产效率大幅改善，并且在溅射时不产生靶的破裂、粉粒的产生少、可以稳定地制作高品质的薄膜，可以得到不产生记录位错误的光记录介质的Bi-Ge-O型烧结体溅射靶及该靶的制造方法以及光记录介质。
背景技术
一写多读型（WORM：Write Once Read Many）光记录介质，是通过蓝色波长区域（350~500nm）的激光也可以进行高密度记录的光记录介质，特别是具有多层具有高记录灵敏度的记录层的光记录介质。
为了应对高密度化的要求，通过多层化进行光盘的高密度化。使用蓝色LD的光盘也同样地进行了高密度记录用光记录介质的开发。
为了实现可以进行高密度多层记录的一写多读型光记录介质，当然需要为具有稳定的组成、结构的材料，而且需要为透光特性优良的膜，这样的材料大多为氧化物，一般而言熔点高，因此多数情况下使用溅射法作为成膜方法。
因此，需要适合得到这样的膜的溅射靶。但是，构成靶的化合物的形态、结构等对溅射特性也有影响，因此在将构成靶的化合物形成为适合必要的膜特性的物质时，是否可以稳定地进行良好的溅射成为问题。
使用溅射法在衬底上形成光记录介质用薄膜时，根据靶的材料有时会产生许多粉粒，从而使品质下降。特别是对于高记录密度介质，由粉粒等导致记录位产生错误是重大的问题。由此，会成为不合格品，从而产生成品率下降的问题。
以往，作为提出的光记录介质，提出了许多材料。例如，在专利文献1中，记载了在衬底上至少形成有记录层的光记录介质，其中，记录层的构成元素的主要成分为Bi和O（氧），含有B，并且含有选自Ge、Li、Sn、Cu、Fe、Pd、Zn、Mg、Nd、Mn和Ni中的至少一种元素X。
另外，在专利文献2中，记载了一种一写多读型光记录介质，其特征在于，记录层含有Bi、M（M为Mg、Al、Cr、Mn、Co、Fe、Cu、Zn、Li、Si、Ge、Zr、Ti、Hf、Sn、Mo、V、Nb、Y和Ta中的至少一种元素）和氧，记录有信息的记录标记部含有在该记录层中含有的元素的结晶和/或这些元素的氧化物的结晶。
此外，提出了专利文献3至专利文献8。其中，考虑了含有铋（Bi）、锗（Ge）和氧（O）的光记录介质的组合，也记载了通过烧结体靶的溅射将这些光记录介质成膜。但是，该Bi-Ge-O型烧结体溅射靶，存在如下问题：耐热冲击性弱，通过高功率进行溅射时大多会产生破裂、龟裂，由此产生粉粒，损害记录介质的品质。
现有技术文献
专利文献
专利文献1：日本特开2008-210492号公报
专利文献2：日本特开2006-116948号公报
专利文献3：日本特开2003-48375号公报
专利文献4：日本特开2005-161831号公报
专利文献5：日本特开2005-108396号公报
专利文献6：日本特开2007-169779号公报
专利文献7：日本特开2008-273167号公报
专利文献8：日本专利第4271063号公报
发明内容
本发明涉及Bi-Ge-O型烧结体溅射靶及该靶的制造方法以及光记录介质，特别是本发明的课题在于提供耐热冲击性优良、可以高功率溅射因此可以预计生产效率大幅改善，并且在溅射时不产生靶的破裂、粉粒的产生少、可以稳定地制作高品质的薄膜，可以得到不产生记录位错误的光记录介质的Bi-Ge-O型烧结体溅射靶及该靶的制造方法以及光记录介质。
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，通过将分散系Bi12GeO20粒子微粒化，各个粒子在加热、冷却时的热膨胀、热收缩量减少，耐热冲击性提高。
基于这些发现，本发明提供：
1）一种Bi-Ge-O型烧结体溅射靶，含有铋（Bi）、锗（Ge）和氧（O），其特征在于，Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75，并且由作为结晶相的Bi12GeO20和Bi4Ge3O12两相构成。
2）如上述1）所述的Bi-Ge-O型烧结体溅射靶，其特征在于，Bi12GeO20与Bi4Ge3O12的摩尔比为（Bi12GeO20/Bi4Ge3O12）<0.56。
3）如上述1）或2）所述的Bi-Ge-O型烧结体溅射靶，其特征在于，靶烧结体中的Bi12GeO20的最大粒径为3μm以下。
4）如上述1）至3）中任一项所述的烧结体溅射靶，其特征在于，通过在200℃加热30分钟后进行水中急冷而对靶施加热冲击时，该热冲击前后的平均弯曲强度下降率为50%以下。
5）一种光记录介质，其通过使用1）至4）中任一项所述的靶进行溅射而成膜。
另外，本发明提供：
6）一种Bi-Ge-O型烧结体溅射靶的制造方法，其特征在于，
将Bi12GeO20粉末与Bi4Ge3O12粉末作为起始原料并进行热压，由此制作烧结体，所述Bi12GeO20粉末通过将14.3摩尔%的GeO2粉末和85.7摩尔%的Bi2O3粉末混合后进行固相反应而得到，所述Bi4Ge3O12粉末通过将60.0摩尔%的GeO2粉末和40.0摩尔%的Bi2O3粉末混合后进行固相反应而得到。
7）如上述6）所述的Bi-Ge-O型烧结体溅射靶的制造方法，其特征在于，将Bi12GeO20粉末和Bi4Ge3O12粉末作为起始原料，以Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75的方式将它们混合后，在600~840℃、加压0~400kg/cm2的条件下进行热压，由此制作烧结体。
8）如上述6）或7）所述的Bi-Ge-O型烧结体溅射靶的制造方法，其特征在于，使用微粉碎到平均粒径为1μm以下的Bi12GeO20粉末。
发明效果
本发明的Bi-Ge-O型烧结体溅射靶，特别地具有如下优良效果：耐热冲击性优良，可以高功率溅射因此可以预计生产效率大幅改善，并且在溅射时不产生靶的破裂、粉粒的产生少、可以稳定地制作高品质的薄膜，可以得到不产生记录位错误的光记录介质。
附图说明
图1是表示实施例1中得到的烧结体的扫描电镜观察结果的照片。
图2是表示比较例1中得到的烧结体的扫描电镜观察结果的照片。
具体实施方式
本发明的Bi-Ge-O型烧结体溅射靶，含有铋（Bi）、锗（Ge）和氧（O），其特征在于，Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75，并且由作为结晶相的Bi12GeO20和Bi4Ge3O12两相构成。使用该组成的记录膜，为可以通过多层化实现高密度记录的适合组成，可以稳定地进行良好的溅射成膜。
一般而言，在将氧化铋（Bi2O3）和氧化锗（GeO2）的粉末作为起始原料，将其烧结来制作该组成靶的情况下，成为Bi12GeO20和Bi4Ge3O12两相共存的组成。
不过，Bi12GeO20和Bi4Ge3O12的热膨胀系数差异大，因此耐热冲击性极弱，产生在使用高功率溅射成膜时产生破裂的问题。顺便说一下，Bi12GeO20的热膨胀系数为1.39×10-5，Bi4Ge3O12的热膨胀系数为6.00×10-6。
另一方面，在该组成范围内，得到Bi4Ge3O12为基质，Bi12GeO20粒子分散的体系。此时发现：通过将分散系Bi12GeO20粒子微粒化，可以减少各个粒子的加热、冷却时的热膨胀、热收缩量，提高耐热冲击性。
另外发现：以Bi2O3和GeO2为起始原料，在Bi12GeO20和Bi4Ge3O12共存的状态下进行微粉碎时，Bi4Ge3O12被选择性地微粉碎，而分散系Bi12GeO20难以粉碎。
因此，通过以Bi12GeO20和Bi4Ge3O12为起始原料，并预先将Bi12GeO20微粉碎，可以实现耐热冲击性的提高。
结果，可以提高靶的耐热冲击性，由此可以得到如下显著优点：可以进行高功率成膜，可以提高生产效率。
另外，可以得到如下效果：引起破裂或龟裂的粉粒的产生显著减少，可以制作稳定的高品质的薄膜，可以制作不产生记录位错误、而且可以实现高记录密度的光记录介质。
Bi12GeO20与Bi4Ge3O12的摩尔比为（Bi12GeO20/Bi4Ge3O12）<0.56对于提高耐热冲击性是有效的。
另外，将靶烧结体中的Bi12GeO20微细化时，最大粒径为3微米以下，优选平均粒径为1μm以下更加有效。所述的靶，可以实现如下特性：通过在200℃加热30分钟后进行水中急冷而施加热冲击时，该热冲击前后的平均弯曲强度下降率为50%以下。
现有的Bi12GeO20和Bi4Ge3O12两相共存而组成的靶的情况下，所述热冲击前后的平均弯曲强度下降率超过80%，与此相对，本发明实现了显著的改善效果。由此抑制靶的热冲击造成的破裂时，就可以直接评价靶的特性。
本发明也包括通过使用所述靶进行溅射而成膜的光记录介质。
在制造Bi-Ge-O型烧结体溅射靶时，将Bi12GeO20粉末与Bi4Ge3O12粉末作为起始原料并将它们混合后进行热压，由此制作烧结体，所述Bi12GeO20粉末通过将14.3摩尔%的GeO2粉末和85.7摩尔%的Bi2O3粉末混合后进行固相反应而得到，所述Bi4Ge3O12粉末通过将60.0摩尔%的GeO2粉末和40.0摩尔%的Bi2O3粉末混合后进行固相反应而得到。
另外，制造本申请发明的Bi-Ge-O型烧结体溅射靶时，特别有效的是：将Bi12GeO20粉末和Bi4Ge3O12粉末作为起始原料，以Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75的方式将它们混合后，在600~840℃、加压0~400kg/cm2的条件下进行热压，由此制作烧结体。
此时，使用微粉碎到平均粒径为1μm以下的Bi12GeO20粉末也是有效的。
该烧结条件是可以得到均匀组成的靶的适合条件。通过上述范围以外的烧结条件也可以制造靶，但是靶品质的重现性差，因此期望设定为上述范围。另外，所述原料阶段的Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75，直接反映到靶上，可以得到相同组成比的靶。
实施例
以下，基于实施例和比较例进行说明。另外，本实施例仅仅是例子，无论如何不限于该实施例。即，本发明仅受权利要求书的限制，本发明也包括本发明所包括的实施例以外的各种变形。
（实施例1）
将纯度3N（99.9%）的氧化铋和氧化锗的粉末作为起始原料，预先准备Bi12GeO20粉末和Bi4Ge3O12粉末，配合16.67摩尔%的Bi12GeO20粉末和83.33摩尔%的Bi4Ge3O12粉末使Bi与Ge的原子数比为0.67，然后进行混合，再将混合后的粉末填充到碳制模具中，在温度700℃、压力250kg/cm2的条件下进行热压。
将热压后的烧结体精加工而得到靶。靶的相对密度为96%（100%密度为7.15g/cm3）。
该烧结体通过X射线衍射测定确认为Bi12GeO20和Bi4Ge3O12两相结构。
然后，该烧结体的扫描电镜观察照片示出于图1。由此确认，Bi4Ge3O12为基质（照片的灰色部分）、Bi12GeO20为分散系（照片的白色部分）。另外确认：Bi12GeO20的最大粒径为3μm以下，平均粒径为1μm以下。
然后，通过在200℃加热30分钟后在水中急冷而对该靶施加热冲击。然后，依照JIS标准1601实施弯曲试验（从靶中的任意5个部位取宽度4±0.1mm、高度3±0.1mm、长度40~50mm的试验片进行测定，并求出5个点的测定结果的平均值），测定该热冲击前后的平均弯曲强度比（强度的下降率）。该测定结果同样地示出于表1。根据测定部位而多少存在偏差，但是均低于50%，强度的下降率少。
然后，使用该靶，在玻璃衬底上以1kW预溅射约1小时后，以2kW的功率将溅射10s和停止5s的循环重复进行10000次，在该溅射循环作业后，打开腔室通过目测观察靶的异常，完全没有观察到靶上产生破裂或龟裂。另外，溅射中粉粒的产生也少。
结果，本申请发明的实施例为具有如下优良效果的良好的靶：不产生破裂，可以提高生产效率，并且可以稳定地制作高品质的薄膜，可以得到不产生记录位错误的光记录介质。
表1
Figure BDA00001618537500091
（比较例1）
将纯度3N（99.9%）的氧化铋和氧化锗的粉末作为起始原料，配合50.0摩尔%的GeO2粉末和50.0摩尔%的Bi2O3粉末使Bi与Ge的原子数比为0.67，然后进行混合，再将混合后的粉末填充到碳制模具中，在温度730℃、压力250kg/cm2的条件下进行热压。
将热压后的烧结体精加工而得到靶。靶的相对密度为103%（100%密度为7.44g/cm3）。
通过该烧结体的X射线衍射测定，确认靶的结晶相为Bi12GeO20和Bi4Ge3O12两相结构。
然后，该烧结体的扫描电镜观察照片示出于图2。由此确认，Bi4Ge3O12为基质（照片的灰色部分）、Bi12GeO20为分散系（照片的白色部分）。另外确认：Bi12GeO20的最大粒径为8μm以下，平均粒径为4μm以下。
然后，通过在200℃加热30分钟后在水中急冷而对该靶施加热冲击。然后，依照JIS1601实施弯曲强度试验。该热冲击前后的平均弯曲强度比（强度的下降率）的测定结果同样地示出于表1。结果，平均弯曲强度的下降率为82.1%。
然后，使用该靶，在玻璃衬底上以1kW预溅射约1小时后，以2kW的功率将溅射10s和停止5s的循环重复进行10次，在该溅射循环作业后，打开腔室通过目测观察靶的异常，发现靶产生破裂。另外，与实施例相比，粉粒的产生显著增加。认为这可能是由于溅射中靶的破裂而引起的。
产业实用性
根据本发明的Bi-Ge-O型烧结体溅射靶及其制造方法，特别地具有如下优良效果：耐热冲击性优良，可以高功率溅射因此可以预计生产效率大幅改善，并且在溅射时不产生靶的破裂、粉粒的产生少、可以稳定地制作高品质的薄膜，可以得到不产生记录位错误的光记录介质。可以提供可以提高光记录介质的成膜的生产效率，从而适合制造光记录介质的靶。

Claims (8)

1.一种Bi-Ge-O型烧结体溅射靶，含有铋（Bi）、锗（Ge）和氧（O），其特征在于，Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75，并且由作为结晶相的Bi12GeO20和Bi4Ge3O12两相构成。
2.如权利要求1所述的Bi-Ge-O型烧结体溅射靶，其特征在于，Bi12GeO20与Bi4Ge3O12的摩尔比为（Bi12GeO20/Bi4Ge3O12）<0.56。
3.如权利要求1或2所述的Bi-Ge-O型烧结体溅射靶，其特征在于，靶烧结体中的Bi12GeO20的最大粒径为3μm以下。
4.如权利要求1至3中任一项所述的烧结体溅射靶，其特征在于，通过在200℃加热30分钟后进行水中急冷而对靶施加热冲击时，该热冲击前后的平均弯曲强度下降率为50%以下。
5.一种光记录介质，其通过使用权利要求1至4中任一项所述的靶进行溅射而成膜。
6.一种Bi-Ge-O型烧结体溅射靶的制造方法，其特征在于，
将Bi12GeO20粉末与Bi4Ge3O12粉末作为起始原料并进行热压，由此制作烧结体，
所述Bi12GeO20粉末通过将14.3摩尔%的GeO2粉末和85.7摩尔%的Bi2O3粉末混合后进行固相反应而得到，
所述Bi4Ge3O12粉末通过将60.0摩尔%的GeO2粉末和40.0摩尔%的Bi2O3粉末混合后进行固相反应而得到。
7.如权利要求6所述的Bi-Ge-O型烧结体溅射靶的制造方法，其特征在于，将Bi12GeO20粉末和Bi4Ge3O12粉末作为起始原料，以Bi与Ge的原子数比为0.57<(Bi/(Bi+Ge))<0.75的方式将它们混合后，在600~840℃、加压0~400kg/cm2的条件下进行热压，由此制作烧结体。
8.如权利要求6或7所述的Bi-Ge-O型烧结体溅射靶的制造方法，
其特征在于，使用微粉碎到平均粒径为1μm以下的Bi12GeO20粉末。
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