CN1930622B - 光学记录介质 - Google Patents

光学记录介质 Download PDF

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CN1930622B
CN1930622B CN200580008136.6A CN200580008136A CN1930622B CN 1930622 B CN1930622 B CN 1930622B CN 200580008136 A CN200580008136 A CN 200580008136A CN 1930622 B CN1930622 B CN 1930622B
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石见知三
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Ricoh Co Ltd
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Abstract

本发明的光学记录介质包括透明基底、记录层、光学反射层和保护层，其中上述后三层依次在基底上形成，并且能在记录线速度为27.9m/s或更高下进行记录。光学反射层的特征在于该层包括Ag和主要由Ag制成的合金中的任何一种，并且光学反射层的x-射线衍射光谱满足关系式0.2＜I(200)/I(111)＜0.4，其中I(111)是(111)面的x-射线衍射峰的强度，而I(200)是(200)面的x-射线衍射峰的强度，该强度是当相对于光学透明基底的表面的入射角为θ时通过基于θ-2θ方法的x-射线衍射测定的。

Description

光学记录介质
技术领域
本发明涉及一种其中使用包含Ag或Ag合金的反射层的具有非常可靠的存储稳定性的光学记录介质。
背景技术
近年来，包括CD和DVD(数字通用盘)作为其典型实例的光盘以及其记录和再现的驱动器(drives)已经在世界上广泛普及。这些盘需要非常可靠的存储稳定性，因为它们用于存储数据信息、图像等。进一步，随着盘的减价的加速，光盘制造商需要降低材料成本，但需要增加其生产率并且确保光盘的存储可靠性。
有两种类型的光盘，即可记录型和可重写型。前者，可记录型光盘一般使用有机染料作为记录材料，而后者，可重写型光盘一般使用无机染料作为记录材料。对于这些光盘，设置反射率标准，以便允许通用的驱动播放器(drive player)再现这种光盘。可记录型光盘也要求保持高的反射率，因为应确保与驱动播放器的兼容性。选择每一种具有高反射率的材料用于反射层，因为用于可记录型光盘的记录层具有吸收激光束的性能。作为典型的材料，有Au、Ag和Ag合金。在这方面，在ROM盘(只读存储盘)的情况中，其中没有用于吸收激光束的层，并且ROM盘为反射提供了充足的空间，因此使用廉价的Al。Au和Ag合金分别具有(特别是Au具有)比Ag低的反射率，并且比Ag贵，但是具有优异的耐久性。迄今为止已经研究了具有反射率下降较少且耐久性好的Ag合金。也已经提交了使用Ag合金的专利申请，但是这种申请因为反射率的障碍不能用于实际用途中。另一方面，Ag反射层的成膜条件也影响记录性能。较高速度记录和较高密度记录导致这种影响增加。
例如，如日本专利(JP-B)No.3373626所述，如果通过改变溅射条件来改变I(200)/I(111)以便改变Ag反射层的膜质量，则这将影响记录性能。然后，该专利限定Ag反射层的膜质量具有I(200)/I(111)≤0.2。此外，如日本专利申请特许公开(JP-A)No.2001-344825所述，发现：改变Ag膜的质量会影响光学记录介质的存储可靠性。该专利申请限定Ag反射层的膜质量具有I(200)/I(111)＞0.4。
然而，尽管所希望的是Ag反射层具有优异的存储性能并且对记录质量决不具有消极的影响，但是发现：在上述专利的膜质量的范围内形成的Ag反射层对存储性能或记录性能具有消极的影响。
在形成记录凹点(pit)中，当将激光束引入盘中时，盘的记录层吸收激光束将其变成热，并且然后通过热分解形成记录凹点，并且此时热扩散的方式对记录性能具有极大的影响。通过改变成膜的溅射条件以形成反射层，将改变反射层的每一个表面的形成。同时，邻近记录层的反射层的条件改变也会影响热传导率。因而，反射层的成膜条件对记录性能具有显著的影响。
特别是在高速记录的情况下，热扩散的方式非常重要，因为引入具有大量能量(power)的快速入射光束。
发明内容
本发明的目的是提供一种使用包括Ag或主要由Ag制成的合金的反射层的光学记录介质，该反射层具有高的反射率并且比金反射层便宜，消除在记录性能中再现信号的波形的失真和在高温和湿度条件下存储稳定性的恶化，这两者均是包括Ag或主要由Ag制成的合金的反射层的缺点。
以下发明可以解决上述缺点：
本发明提供一种光学记录介质，包括透明基底；具有有机染料为主要成分的记录层；光学反射层；保护层，
其中记录层、光学反射层和保护层依次在基底上形成，可在27.9m/s或更高的记录线速度下记录，并且光学反射层包括Ag和主要由Ag制成的合金中的任何一种。光学反射层特征在于：该层包括Ag和主要由Ag制成的合金中的任何一种，并且该光学反射层的x-射线衍射光谱满足关系式：0.2＜I(200)/I(111)＜0.4，其中I(111)是(111)面的x-射线衍射峰的强度，而I(200)是(200)面的x-射线衍射峰的强度，该强度是当相对于光学透明基底的表面的入射角为θ时通过基于θ-2θ方法的x射线衍射测定的。
具体实施方式
下面将对上述发明进行进一步解释：
为了同时满足存储性能和记录性能，本发明使用满足上述条件的光学反射层。在低记录速度下(在1x到4x＝3.5m/s到14.0m/s的范围内)，本发明并不显示显著的效果，但是在记录速度为6x、8x和12x(＝20.9m/s、27.9m/s和42.0m/s)的情况下显示出本发明和现有技术之间的显著区别(在下文实施例和对比例中描述)。
可记录的光盘的成膜通常通过在其上刻有导向槽的透明基底上形成包括有机染料的记录层并且进一步通过在记录层上形成反射层和保护层来进行。对于使用粘结材料的盘如DVD，通过粘结层在保护层上进一步粘结另一(覆盖)基底。
透明基底通过使用其上预先刻有导向槽的压模的注塑来制备，并且一般聚碳酸酯用于该材料，聚碳酸酯是非常透明并且能生产的(productive)。
对于记录层，使用具有有机染料作为主要成分的记录材料。在本文中，具有主要成分是指其中使用足以保证优异的记录性能的量的染料，然而，这通常是指使用仅仅包括染料的记录层，除了按需要添加添加剂如粘结剂和稳定剂以外。
为了形成记录层，在普通的过程中，将有机染料溶于溶解该有机染料但是不溶解基底的溶剂中，并且由此将制备的涂覆溶液通过旋涂均匀地涂覆于基底上。在将涂覆溶液涂覆之后，使记录层退火(anneal)，除去溶剂残余。记录层通常的厚度范围为30nm到150nm。
接着，通过溅射在记录层上形成反射层，并且然后在其上通过旋涂涂覆紫外线固化树脂，并且通过紫外线固化，形成保护层。
有机染料该实例包括：花青染料、酞菁染料、萘菁(naphthalocyanine)染料、蒽醌染料、偶氮染料、包含金属的偶氮染料、三苯甲烷染料、方酸类(squarylium)染料、chroconium染料、甲
Figure G2005800081366D00031
染料、azulenium染料、二硫酚金属配合物染料和靓苯胺金属配合物染料.并且，对于染料涂覆溶剂，适用于以上染料的溶剂选自醇、酮、酯、醚、芳香族烃、卤代烷等.
对于反射层，使用Ag或主要由Ag制成的合金。优选的是：在合金中Ag的含量优选为98重量％或更多，以确保存储稳定性。添加到主要由Ag制成的合金中的元素是金、铜、钯、锑、铑、铂、钛、钼、锆、钽、钨、钒等。
一般使用溅射用于反射层的成膜。对于为了进行溅射而引入的气体，一般使用惰性稀有气体，并且根据可用性和成本主要选择氩气。对于溅射条件，有溅射功率、溅射时间、溅射气体压力等。通过改变这些条件，可以控制膜的厚度和质量。特别地，已知可以通过改变溅射气体压力来控制反射层的质量。
考虑到对记录层和成膜时间没有任何消极的影响，1kW到4kW的溅射功率范围是合适的。
反射层的质量可以通过I(200)/I(111)的数值来检查，I(111)是(111)面的x-射线衍射峰的强度，而I(200)是(200)面的x-射线衍射峰的强度，该强度是当相对于光学透明基底的表面的入射角为θ时通过基于θ-2θ方法(如日本专利申请特许公开(JP-A)No.07-110964中所述的一种评估薄膜的方法)的x-射线衍射测定的。如果I(200)/I(111)的数值为0.4或更大，则存储稳定性的可靠性会增加，但是其记录性能会变差，并且如果I(200)/I(111)的数值为0.2或更小，则存储稳定性的可靠性会变差，但是对记录性能没有消极的影响。因此，为了同时满足记录性能和存储稳定性的可靠性，I(200)/I(111)的数值应该为0.2＜I(200)/I(111)＜0.4，更优选0.21≤I(200)/I(111)≤0.39。另外，如果增加溅射气体压力，该I(200)/I(111)的数值会增加。
对于反射层，尤其是当使用纯Ag或包含少量的一种或多种添加剂的Ag合金，其是能实现具有在8x或更高的高记录线速度的情况下所要求的高反射率的反射层的材料时，限定作为I(200)/I(111)的x-射线衍射强度使得能同时满足存储稳定性的可靠性和以8x或更高的记录线速度的记录性能。
反射层具有厚度为约70nm到约170nm，并且优选设置为100nm到140nm。如果膜厚度太薄，则由于透过的激光束而不能获得满意的反射率，而如果太厚，则记录灵敏度和记录性能会变差，因为热量将在记录时逃逸。
对于保护层，使用有机材料如紫外线固化树脂和热固性树脂。尤其是，优选使用紫外线固化树脂，因为用该树脂容易进行成膜。
保护层通常具有厚度为约3μm到约15μm。太薄的层或太厚的层均不是优选的。如果保护层的厚度太薄，则耐久性会下降，而如果太厚，则这会导致机械性能(弯曲)的劣化。
根据本发明，可以提供一种使用包括Ag或主要由Ag制成的合金的反射层的光学记录介质，该反射层具有高的反射率并且比金反射层便宜，消除在记录性能中再现信号的波形的失真和在高温和湿度条件下存储稳定性的恶化，这两者均是包括Ag或主要由Ag制成的合金的常规型反射层的缺点。
[实施例]
下文将参考实施例和对比例对本发明进行更详细的说明；然而本发明不局限于这些公开的实施例。
[实施例1到3；对比例1到3]
为了检查本发明的有利效果，准备DVD+R盘的生产试验，并且对其进行评估。
将由以下化学式1表示的方酸类(squarylium)染料和由以下化学式2表示的甲染料溶于氟醇溶剂(TFP：2，2，3，3-四氟丙醇)中，以制备涂覆溶液。通过旋涂将涂覆溶液涂覆到具有直径为120mm和厚度为0.6mm的通过注塑制备的聚碳酸酯基底上，并且然后在90℃下15分钟的退火过程中除去溶剂残余，以便形成具有厚度为50nm的记录层。
化学式1
化学式2
接着，通过溅射形成包括纯度为99.99重量％的Ag的反射层，并且将紫外线固化树脂(由DAINIPPON INK AND CHEMICALS，INC.制造的SD1700)旋涂在其上，并且通过紫外线固化，以便形成具有厚度为4μm到8μm的保护层。
此外，由与上述基底相同的聚碳酸酯制造的假(dummy)基底通过使用粘结剂(DVD003，可以从Nippon Kayaku Co.，Ltd.得到)粘结到保护层上，以便获得DVD+R盘。使用由Balzers制造溅射装置用于Ag反射层的溅射，并且溅射功率固定为2kW。使用氩气用于溅射，并且通过在仔细观测安装在溅射装置上的真空计的同时调整氩气的流速使气体压力在1.0×10-3毫巴到2.0×10-2毫巴的范围内变化。
通过改变溅射时间形成Ag层，使膜厚度变成约125nm。
反射层的膜厚度的测量通过使用由CMI制造的x-射线膜测量仪来进行，并且也测量在各种条件下形成的反射层的x-射线衍射光谱。使用x-射线分光仪(X′pertPRO；由Philips Electronics N.V.制造)在以下条件下测量x-射线衍射光谱：
X-射线发生器    Cu密封管
X-射线管电压    45kv
X-射线管电流    40mA
通过使用由Pulstec Industrial Co.，Ltd.制造的DDU-1000(具有记录和再现波长为658nm))来评估记录性能，以便测量最低抖动(最小抖动值)和在改变记录功率时的功率余量(power margin)ΔP/Po。ΔP表示能满足抖动标准的记录功率的宽度，并且Po表示最低抖动时的记录功率。在8x(线速度：27.9m/s)下进行记录评估，并且在1x(线速度：3.5m/s)下进行再现评估。
存储稳定性的可靠性的评估通过测量在测试存储稳定性之前在4x下进行记录的盘的PI误差(最大值)，并且然后通过在80℃的高温和85％RH的高湿度的条件下该盘存储300小时之后测量PI误差(存档(archive)测试)来进行。
表1显示结果：
表1
Figure G2005800081366D00071
如表1所示，当增加氩气压力时，I(200)/I(111)的数值增加。当I(200)/I(111的数值为0.4或更大时，如对比例2和3，记录性能变差(最低抖动增加，并且功率余量变窄)。
如对比例1，当I(200)/I(111)的数值为0.2或更小时，存储稳定性变差(储存测试之后的PI误差显著增加)。
在实施例2和对比例3的各个盘上以1x、4x、8x和12x进行记录。表2显示用实施例1中相同的方式评估的各自的最低抖动结果。
表2
Figure G2005800081366D00072
表2显示，记录速度增加越高，反射层越可能影响记录性能。尤其，当记录速度在8x或更高时，记录性能中的差距(gap)变得显著。
实施例4和5
除了使用银合金ANC(AgNdCu)作为反射层的材料以外，用实施例1中相同的方法制备DVD+R盘并且进行评估。表3显示该结果。应该注意：NdCu的含量在表3中显示。实施例4和实施例5的合金的精确组成比分别是Ag98.2Nd0.8Cu1.0和Ag97.7Nd1.0Cu1.3。
表3
从表3可以看出：增加添加到Ag中的NdCu的量会增加存储稳定性的可靠性但是会降低反射率。因此，Ag合金的纯度优选为98重量％或更大。

Claims (3)

1.一种光学记录介质，包括：
透明基底；
具有主要成分为有机染料的记录层；
光学反射层；和
保护层，
其中该记录层、该光学反射层、和该保护层依次在该基底上形成，能在记录线速度为27.9m/s或更高下进行记录，
其中该光学反射层包括主要由Ag制成的合金，并且该光学反射层的x-射线衍射光谱满足以下关系式：
0.2＜I(200)/I(111)＜0.4
其中I(111)是(111)面的x-射线衍射峰的强度，而I(200)是(200)面的x-射线衍射峰的强度，该强度是当相对于光学透明基底的表面的入射角为θ时通过基于θ-2θ方法的x-射线衍射测定的，
其中该主要由Ag制成的合金进一步包括Nd和Cu。
2.根据权利要求1的光学记录介质，
其中该主要由Ag制成的合金包含98重量％或更多的Ag。
3.根据权利要求1的光学记录介质，
其中该光学反射层具有厚度为70nm到170nm。
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