CN1214378C - 光学数据存储介质用记录材料,生产所述记录材料的方法和带有相应记录层的光学数据存储介质 - Google Patents

光学数据存储介质用记录材料,生产所述记录材料的方法和带有相应记录层的光学数据存储介质 Download PDF

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CN1214378C
CN1214378C CNB008071241A CN00807124A CN1214378C CN 1214378 C CN1214378 C CN 1214378C CN B008071241 A CNB008071241 A CN B008071241A CN 00807124 A CN00807124 A CN 00807124A CN 1214378 C CN1214378 C CN 1214378C
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A·扎菲洛夫
S·拉科夫斯基
J·巴卡吉瓦－埃尼瓦
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Abstract

除了阳离子染料和至少一种用作骤冷剂的物质外，本发明的记录介质含有用以增加光学数据存储装置稳定性的稳定剂，该装置有一个由本发明记录介质组成的记录层。所述稳定剂是带有一个或多个羟基、优选在记录介质中以酚离子形式存在、并构成用于染料阳离子的部分阴离子的酚。此外，记录介质中还可含有阴离子金属有机烯硫基配合物，其替代常用的骤冷剂，并且构成用于染料阳离子的另一部分阴离子。本发明的目的是生产一种用于数据存储介质记录层的记录材料，该记录材料不仅在记录层中而且在用于生产记录层的溶液中显示出与已知记录材料相比大大增强的稳定性。

Description

光学数据存储介质用记录材料，生产所述记录材料的 方法和带有相应记录层的光学数据存储介质
技术领域
本发明涉及光学数据存储介质领域，特别是可用激光写入和读取的光学数据存储介质。本发明涉及该种数据存储介质记录层的记录材料，涉及生产该记录材料的方法，并涉及有一个由所述记录材料组成的记录层的光学数据存储介质，它们各自在相应的独立权利要求中描述。
背景技术
可用激光写入和读取的光学数据存储介质(例如，CD-R、DVD-R、DVD-RAM、DVD-RW或HD)通常包含一种通常由聚碳酸酯组成的盘状透明载体，并在一侧包含一种通常为螺旋形的记录槽，且这一侧通常被三层覆盖。这三层是记录层、反射层和保护清漆层。记录层直接位于由槽构成的载体一侧的载体物质上，并由记录材料组成。该介质含有一种染料或染料混合物，其光学特性可通过激光束(写字光束)来改变。反射层在记录层上，通常由金属组成(例如银、金或铝)。保护清漆层在反射层上，通常由树脂清漆组成，可被紫外线硬化。
为了写入，数据存储介质沿着槽(转动的)的方向相对于激光束(写入光束)移动，并由激光写入，借此，激光穿过载体和记录层对准到反射层上。此过程中，写入光束的波长范围和能量是以这样一种方式设计的，即记录层中吸收激光光线导致局部加热，通过局部加热，载体物质和记录层之间产生泡状坑，并且记录层中的化学反应导致该层含有的染料的光学特性局部改变(例如脱色/漂白)。光学数据存储介质上的记录实质上是由一系列被写入光束改变的具有坑和化学变化的染料或染料混合物的点和未改变的点组成的。
为了读取，数据存储介质被再次沿着槽的方向相对于激光束移动，此处，激光束的强度比写入光束低，并通过载体和记录层再次对准到反射层上。在改变点或未改变点处的激光束的反射变化(更强或更弱的反射)被定作读取信号。
该种数据存储介质的生产方法，例如，可包括下列步骤：
·通过注模法制备聚碳酸酯载体，
·用一种溶液涂布旋转载体，该溶液中，记录材料的成分被溶解或作为胶体包含在有机溶剂或有机溶剂混合物中，通过离心力将溶液涂布于载体，多余溶液离心弃掉，
·通过挥发除去溶剂或溶剂混合物，
·通过“喷镀”涂布反射层，
·涂布和使保护清漆硬化。
上述步骤通常连续进行，优选与检查步骤一起完成。这种检查步骤大多用于中间体的光学控制和消灭次品。
人们在不断地对上述数据存储介质提出要求，这些要求首先与写入和读取速度有关、与写入和读取质量有关、与耐用性有关、最后但并不是最不重要的一点是与价格有关。数据存储介质的读写特性以及耐用性和价格在很大程度上取决于记录层的特性，因而对这一层的要求多而且是多种多样。特别是，这一层必须能使得发生写入过程中适宜的化学反应，快速写入必须需要尽可能少的能量，同时，这一层应该是化学上尽可能稳定的，以保证高耐用性。记录层的化学稳定性也很重要，因为在很大程度上它将决定反射层上是否要使用非常贵金属和价格昂贵的金属，或是否较少的贵金属就足够。此外，用于生产记录层的记录材料溶液要借助于离心力涂布，因而应该具有如精确限定的流变特性，以使得生成的记录层具有非常精细和均匀的厚度，并且能被迅速毫无问题地干燥。
数据存储介质记录层中常用的、具有可被写入光束改变光学特性的染料为，例如，阳离子次甲基或多次甲基染料(花青染料、酞菁染料、偶氮染料或金属甲)，可从商业渠道买到，例如，作为氯化物、溴化物、氟化物、高氯酸盐、四氟硼酸盐或带有砜阴离子或碳酸阴离子。为使染料的光学特性易于被写入光束改变，记录材料中除了染料以外还含有所谓的骤冷剂。
适用于数据存储介质记录层的染料已经公开，例如下列出版物：BP-0403797，WO-93/22142，WO-98/14612，WO-99/37717，WO-99/05221，WO-98/34988，US-5900348(次甲基和多次甲基或花青染料)，JP-52047824，JP-58069255，JP-07314897(酞菁染料)，US-5731054，US-5922504(金属甲染料)。也建议使用含有两种或三种上述染料的染料混合物。
骤冷剂也可在市场上得到，例如，Nippon Kayako Co.Ltd的商品IRG 23或IRG 003。
显然，含有上述已知染料和骤冷剂的溶液是不太稳定的，因为骤冷剂易分解。由于这一原因，用于制备记录层的溶液不能大量生产和贮存，特别是不能无限制地循环。也很显然，带有只含有所述染料和骤冷剂的记录层的数据存储介质只能以有限的速度写入。此外，这种记录层对反射层有腐蚀作用，使得后者必须用银或金制造，以保证数据存储介质足够的耐用性。
出版物US-5436113中描述了一种带有记录层的光学数据存储介质，该记录层含有用于稳定作用的苯酚。
发明内容
本发明的目的是生产一种用于数据存储介质记录层的记录材料，该记录材料不仅在记录层中而且在用于生产记录层的溶液中显示出与已知记录材料相比大大增强的稳定性。
本发明的目的可通过光学数据存储介质记录层的记录材料、制备该记录材料的方法或所述数据存储介质来实现，它们各自在相应的独立权利要求中予以定义。
本发明是基于这样的想法：通过加入带有一个或若干个羟基的酚、有利的是被取代的酚的形式的稳定剂使记录材料稳定。酚以酚离子的形式存在于记录材料中，并代替阳离子染料中部分常用的抗衡离子(如高氯酸离子)。用金属有机烯硫基(thiolene)配合物阴离子替代阳离子染料中另一部分抗衡离子，可使记录材料更进一步地稳定，所述阴离子也可起骤冷剂的作用，使得在此种情况下不需要向记录材料中加入常规骤冷剂。特别适用于本目的的是有中央金属原子的阴离子烯硫基配合物，其中金属原子至少有两个价。
在含有有常规阴离子的阳离子染料(或若干种阳离子染料混合物)和商业上可买到的骤冷剂的记录材料和这种介质的溶液中，如果还含有有利的是被取代的酚作为稳定剂时，则显示出大大增强的稳定性。用酚，特别是相应的酚离子代替部分常规阴离子，会使这一效果更加增强。进一步替代阴离子和用阴离子金属有机烯硫基配合物代替骤冷剂会使稳定性进一步增强。
按照本发明使记录材料的稳定性提高产生了下列优点：
·含有该记录材料的数据存储介质在写入或非写入情况下都更加耐用，
·由于记录材料的腐蚀性较小，在反射层可使用较少贵的因而相应地便宜的金属如铝代替银或金，
·用于生产记录层的溶液可以使用更长的时间，特别是，它实质上可以没有任何限制地循环，因而不会产生对环保有害的废弃物。
也很显然，直接从记录材料稳定性增强来看，含有本发明记录材料的数据存储介质除了上述优点外，还具有比已知数据存储介质更进一步的优点。这些进一步的优点与写入和读取质量有关，特别是：
·对写入和读取很重要的记录层的光学特性得到改善，
·坑的边界清晰，
·所述数据存储介质在最高速度(至少高达16x)下能以非常好的质量写入，
·记录材料溶液的流变特性更好，因而能被更快地涂布于载体，具有更好的槽纹填充和均匀性，因此可用作更薄、更快的干燥层，由于这一结果不但写入和读取质量得以改善，而且循环时间被缩短，因为使用更少的染料，产品的生产更加便宜，
·记录材料易溶于生产光学数据存储介质常用的所有溶剂。
本发明的光学数据存储介质记录材料因此包含下列组分：
·阳离子染料(次甲基或多次甲基染料(花青染料)、酞菁染料、甲染料或偶氮染料)，其光学特性可通过写入光束的作用可以改变，
·带有一个或多个羟基的酚、有利的是被取代的酚，作为稳定剂，其中有利地是酚以酚离子形式存在，酚替代部分常用的、有腐蚀作用的染料阴离子，
·骤冷剂或有利地用阴离子金属有机烯硫基配合物代替骤冷剂起骤冷剂作用，并代替染料阴离子中部分常用的、有腐蚀作用的阴离子，并因此对记录材料的稳定性作出贡献。
本发明的记录材料含有相对于染料的量来说一定量的酚离子，使得酚离子构成1-30％(摩尔百分比)的阴离子。还含有阴离子金属有机烯硫基配合物的本发明的记录材料含有相对于染料的量而言一定量的该配合物，使得其构成另外1-50％的阴离子。因为许多稳定剂阴离子对记录材料的光学特性有负面影响，较高比例的稳定剂离子是不利的。具有更高比例的金属有机烯硫基配合物离子，记录材料的溶解性变差。
本发明的记录材料中有利地被用作稳定剂的取代的酚或相应的酚盐为：2，6-二叔丁基-苯酚、2，6-二叔丁基-4-甲基-苯酚、2-叔丁基-4-甲基-苯酚、6-叔丁基-3-甲基-苯酚、α-甲基-苄基-苯酚、2，6-二叔丁基-4-甲氧基-苯酚、4-羟基-3，5-二叔丁基-苄醇、6-叔丁基-2-甲基-苯酚、β-(4-羟基-3，5-二叔丁基-苯基)丙酸酯、2，5-二叔丁基-对苯二酚、2，5-二叔戊基-对苯二酚、2，2’-亚甲基-双(6-叔丁基-4-甲基-苯酚)、2，2’-亚甲基-双(4，6-二甲基-苯酚)、2，2’-异亚丁基双(4，6-二甲基-苯酚)、2，2’-亚甲基-双(4-甲基-6-α-环己基-苯酚)、4，4-亚甲基-双(2，6-二叔丁基-苯酚)、4，4’-亚丁基-双(6-叔丁基-3-甲基-苯酚)、2，2’-硫代双(6-叔丁基-4-甲基-苯酚)、2，2’-硫代双(4-甲基-6-α-甲基-苄基-苯酚)、2，2’-硫代双(4，6-二-仲-戊基-苯酚)、4，4’-硫代双(6-叔丁基-2-甲基-苯酚)、4，4’-硫代双(6-叔丁基-3-甲基-苯酚)、双(4-羟基-3，5-二叔丁基-苄基)硫醚、1，1，3-三(5’-叔丁基-4’-羟基-2’-甲基-苯基)丁烷、2，4，6-三(4’-羟基-3’，5’-二叔丁基-苄基)、2，4-二羟基-二苯酮，4-烷氧基-2-羟基-二苯酮、2-羟基-4-甲氧基-二苯酮、或两种或两种以上的所述酚或酚盐的混合物。
观察到的、由稳定剂离子引起的染料光学特性的变化使人们怀疑其中生成了离子配合物，它不仅靠静电力而且靠配位力结合在一起。
适用于本发明的记录材料的、具有骤冷剂作用的阴离子烯硫基金属配合物为，例如，下式的二-烯硫基-金属配合物：
其中M＝Ni、Co、Fe、Cu、Sn、Zn、Al、Ti、Cr、V、Pt或Pd；和
其中-R＝-H、-Cl、-Br、-I、-F、-NO2、-CSN、-CN、-OCH3、-OCnH(2n+1)，其中n＝1-20，或-COOR，其中R＝OCnH(2n+1)。
有利的用于生产本发明记录材料的离子替代物可以这样得到：使用酚离子例如苯酚钾形式的酚，将染料和酚盐溶于有机溶剂(如二甲基甲酰胺或丙酮)，在升高的温度(如70-120°)下，将溶液搅拌较长的时间(如2-12小时)。随后，例如，通过用水洗涤分离构成水溶性盐的替代离子。然后将得到的物质干燥，需要配制生产记录层的溶液时，将其溶于例如双丙酮醇与甲氧基乙醇混合物、双丙酮醇与丁醇混合物、双丙酮醇与异丙醇混合物或溶于另一种适宜的有机溶剂或溶剂混合物中。
具体实施方式
实施例1
将Fuji Photo Film Co.Ltd生产的带有5个次甲基的花青染料Dye OM 57、Nippon Kayako Co.Ltd生产的骤冷剂IRG 23和作稳定剂的2，2’-硫代双(6-叔丁基-4-甲基-苯酚)按下列重量比混合：Dye∶骤冷剂＝10∶1，染料∶稳定剂＝10∶3。通过在室温下搅拌至少24小时，将混合物以浓度3％(重量百分比)溶于双丙酮醇和异丙醇(10∶1)中。然后在氮气存在下，将溶液通过RC58型过滤器(Schleicher &Schuell)加压过滤。此法生产的染料溶液在连续搅拌下用于生产记录层。
为了生产记录层，通过旋转沉积法(spin-on deposition)将记录材料溶液涂布于由槽结构化的聚碳酸酯载体一侧，层的厚度约180-220nm。然后将涂敷载体于80℃干燥。用本身已知的方法将厚度约为60-90nm的一层银通过喷镀施于干燥的记录层上。随后用旋转沉积法涂上保护清漆层，并在紫外光下硬化。
弃掉的记录材料溶液可以制备用于循环，其中混合需要量的骤冷剂和溶剂。由于分解的骤冷剂量在不断增加，所以再循环能力是有限的。
为了检测数据存储介质的耐用性，将装置在温度80℃、相对环境湿度85％的条件下老化72小时。然后用PCRW 404型Philips激光记录器将试验资料记录到数据存储介质上，用已校对的CD-CATS测试仪测定BLER值(填充错误率)以及坑和平面的抖动值，并与写入的未老化的数据存储介质的对应的测量值进行比较。
实施例2
在10％(重量百分比)染料OM 57(如实施例1中)溶于二甲基甲酰胺的溶液中，加入20％(摩尔百分比，相对于染料)2，2’-硫代双(6-叔丁基-4-甲基-苯酚)的钾盐。将溶液于70℃搅拌2小时。然后将溶液倾到冷水中，此时有机组分沉淀出来，水溶性盐溶进溶液中。滤除有机组分，用二甲基甲酰胺和乙醇(4∶1)溶液重结晶，然后干燥。
收率：95％
为了生产记录层，然后将染料和稳定剂的离子化合物与骤冷剂IRG23混合(染料与骤冷剂的数量比＝10∶1)，然后按实施例1所述方法将其溶解、使用。此步中，旋转沉积施加的记录材料层的厚度可减至150-180nm。
实施例3
在10％(重量百分比)的染料OM 57(如实施例1中)溶于二甲基甲酰胺的溶液中，加入20％(摩尔百分比，相对于染料)2，2’-硫代双(6-叔丁基-4-甲基-苯酚)的钾盐以及10％(摩尔百分比，相对于染料)的式1的烯硫基配合物的四丁基铵盐，式中M＝Co，-R＝-OCH3。将混合物按实施例2中所述方法进一步进行处理。
在不加任何骤冷剂的情况下，将以此方式制成的染料、稳定剂和烯硫基配合物的离子化合物溶解以制备记录层和按实施例1的方法使用。本例中，旋转沉积施加的记录材料的层厚度可减至130-150nm。对于循环使用弃掉的记录材料溶液，不必检测骤冷剂含量和添加骤冷剂。
下表含有按实施例1-3生产的光学数据存储介质的检测结果，并与记录层中只含有染料OM 57和骤冷剂IRG 23(重量比10∶1)的数据存储介质(已知技术)进行比较。
                               测试老化前/后百分比变化[％]
                                BLER    坑抖动    平面抖动
对照数据存储介质(已知技术)      30      24        26
实施例1的数据存储介质           12      10        12
实施例2的数据存储介质           5       2         3
实施例3的数据存储介质           1       0         1

Claims (15)

1.光学数据存储介质用记录材料，该记录材料包含具有可被写入光束改变的光学特性的阳离子染料或阳离子染料混合物，还包含至少一种具有骤冷剂作用的物质和一种用作稳定剂的带有一个或多个羟基的酚或取代酚，其特征在于所述酚或取代酚在记录材料中以酚离子形式存在，并且构成用于染料阳离子的一部分阴离子。
2.权利要求1的记录材料，特征在于稳定剂包括下列酚的阴离子或所述酚离子的混合物：2，6-二叔丁基苯酚、2，6-二叔丁基-4-甲基-苯酚、2-叔丁基-4-甲基-苯酚、6-叔丁基-3-甲基-苯酚、α-甲基-苄基-苯酚、2，6-二叔丁基-4-甲氧基-苯酚、4-羟基-3，5-二叔丁基-苄醇、6-叔丁基-2-甲基-苯酚、β-(4-羟基-3，5-二叔丁基-苯基)丙酸酯、2，5-二叔丁基-对苯二酚、2，5-二叔戊基-对苯二酚、2，2’-亚甲基-双(6-叔丁基-4-甲基-苯酚)、2，2’-亚甲基-双(4，6-二甲基-苯酚)、2，2’-异亚丁基-双(4，6-二甲基-苯酚)、2，2’-亚甲基-双(4-甲基-6-α-环己基-苯酚)、4，4-亚甲基-双(2，6-二叔丁基-苯酚)、4，4’-亚丁基-双(6-叔丁基-3-甲基-苯酚)、2，2’-硫代双(6-叔丁基-4-甲基-苯酚)、2，2’-硫代双(4-甲基-6-α-甲基-苄基-苯酚)、2，2’-硫代双(4，6-二-仲戊基-苯酚)、4，4’-硫代双(6-叔丁基-2-甲基-苯酚)、4，4’-硫代双(6-叔丁基-3-甲基-苯酚)、双(4-羟基-3，5-二叔丁基-苄基)硫醚、1，1，3-三(5’-叔丁基-4’-羟基-2’-甲基-苯基)丁烷、2，4，6-三(4’-羟基-3’，5’-二叔丁基-苄基)、2，4-二羟基-二苯酮，4-烷氧基-2-羟基-二苯酮、2-羟基-4-甲氧基-二苯酮。
3.权利要求1的记录材料，特征在于，作为具有骤冷剂作用的物质它包含有一种阴离子金属有机烯硫基配合物，其构成用于染料阳离子的一部分阴离子。
4.权利要求3的记录材料，特征在于阴离子金属有机配合物是下列结构的二烯硫基配合物，
Figure C008071240003C1
其中M＝Ni、Co、Fe、Cu、Sn、Zn、Al、Ti、Cr、V、Pt或Pd，以及其中-R＝-H、-Cl、-Br、-I、-F、-NO2、-CSN、-CN、-OCH3、-OCnH(2n+1)，其中，n＝1-20，或-COOR，其中，R＝OCnH(2n+1)。
5.权利要求1至4之任一项的记录材料，特征在于它包含摩尔比为100∶1至100∶30的染料和稳定剂。
6.权利要求1至4之任一项的记录材料，特征在于它包含摩尔比为100∶1至100∶50的染料和阴离子金属有机烯硫基配合物。
7.权利要求1至4之任一项的记录材料，特征在于它溶于一种有机溶剂或有机溶剂混合物中。
8.权利要求1至7之任一项的记录材料用于制备光学数据存储介质记录层和光学数据存储介质的应用。
9.制备权利要求1至7之任一项的记录材料的方法，特征在于将染料和稳定剂溶于一种有机溶剂，在70-120℃温度下搅拌该溶液，以及在进一步的步骤中，将水溶性盐从溶液中最大程度地分离出来。
10.权利要求9的方法，特征在于将阴离子金属有机烯硫基配合物与染料和稳定剂一起溶解。
11.权利要求9或10的方法，特征在于为了分离水溶性盐，用水洗涤搅拌的溶液。
12.光学数据存储介质，其具有载体，载体上是记录层并且由权利要求1至7之任一项的记录材料组成，记录层上面是反射层，反射层上面是保护清漆层。
13.权利要求12的光学数据存储介质，特征在于反射层由银、金或铝组成。
14.生产具有载体、载体上面有记录层、记录层上面有反射层、反射层上面有保护清漆层的光学数据存储介质的方法，其中，载体是用注模法生产的，记录层是通过旋转沉积法将溶于溶剂中的记录材料涂布于载体上随后通过旋转沉积将溶剂从记录材料中除去而形成，用喷镀法将金属层涂布于记录层上作为反射层，以及将金属层用保护清漆覆盖，所述方法的特征在于溶解的记录材料是权利要求1至7之任一项的记录材料。
15.权利要求14的方法，特征在于金属层由金、银或铝组成。
CNB008071241A 1999-03-05 2000-03-06 光学数据存储介质用记录材料,生产所述记录材料的方法和带有相应记录层的光学数据存储介质 Expired - Fee Related CN1214378C (zh)

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