CN1200495A - 具有层合双轴定向聚烯烃片层的复合照相材料 - Google Patents
具有层合双轴定向聚烯烃片层的复合照相材料 Download PDFInfo
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- CN1200495A CN1200495A CN98115424A CN98115424A CN1200495A CN 1200495 A CN1200495 A CN 1200495A CN 98115424 A CN98115424 A CN 98115424A CN 98115424 A CN98115424 A CN 98115424A CN 1200495 A CN1200495 A CN 1200495A
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- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C7/00—Multicolour photographic processes or agents therefor; Regeneration of such processing agents; Photosensitive materials for multicolour processes
- G03C7/30—Colour processes using colour-coupling substances; Materials therefor; Preparing or processing such materials
- G03C7/3029—Materials characterised by a specific arrangement of layers, e.g. unit layers, or layers having a specific function
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- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S430/00—Radiation imagery chemistry: process, composition, or product thereof
- Y10S430/131—Anticurl layer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
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Abstract
本发明涉及一种照相材料,包括一相纸基底,至少一感光卤化银层,和一位于所述相纸基底与所述卤化银层之间的微孔化双轴定向聚烯烃片层。
Description
本发明涉及照相材料。以优选的形式而言，它涉及用于照相彩色相纸的基底材料。
在形成彩色相纸中，已知基底相纸在其上面应用一层聚合物，通常为聚乙烯。此层起对相纸提供防水作用，以及提供一个在其上形成感光层的光滑表面。适宜的光滑表面的形成是困难的，它要求非常仔细且高费用以确保适合的沉积作用和聚乙烯层的冷却。当气泡被俘获于成型滚柱和将形成涂布感光材料的表面的聚乙烯之间时，造成了现有的生产技术的一个缺陷。此气泡将形成一个坑，该坑将导致一个在聚乙烯上形成的照相材料的照相性能的缺陷。若能以较少的成本形成一个较为可靠和改进的表面，是所希望的。
在彩色相纸中，需要提供具有提高的抗卷曲性能的彩色相纸。现有的彩色相纸在显影和贮藏期间会发生卷曲。此卷曲被认为是由彩色相纸各层在经历显影和干燥过程时的不同性能所造成的。在彩色相纸贮藏期间的湿度变化导致卷曲。彩色相纸当其经历长期高湿度贮藏时，例如大于50％的相对湿度，则存在特殊的问题。相对湿度小于20％的极低湿度还将致使相纸发生卷曲。
在相纸中，聚乙烯层还用作二氧化钛和其它增白物质以及着色材料的载体层。如果着色材料不分散于整个聚乙烯层而是能在此层的表面附近集中，在那里它们将在照相中更为有效，这是所希望的。
在美国专利5244861中已建议在用于热染料转印的接受片中使用双轴定向的聚丙烯。
在感光层和基底相纸之间仍然需要一个更为有效的层来更为有效地携带着色物质，并提供一个改善的光滑表面和更强的照相材料。
本发明的一个目的是提供改进的相纸。
另一个目的是提供一种用于感光影像的具有改进的表面光滑性的基底。
另一个目的是提供具有改进的卷曲性能的相纸。
本发明的这些以及其它目的通常通过照相材料来实现，该照相材料包括相纸基底，至少一感光卤化银层，和位于所述相纸基底和所述卤化银层之间的微孔化双轴定向聚烯烃片层。
本发明的另一具体实例通过一种形成照相材料的方法而实现，包括提供一制备好的双轴定向聚烯烃微孔片层，提供一基底相纸，将粘合剂加至所述基底相纸上，同时将所述微孔化片层加至所述粘合剂以使所述微孔层与所述基底相纸粘合。
本发明提供了用于涂布(casting)感光层的改进的基底，尤其提供了用于具有更大抗卷曲性和改进影像的彩色照相材料的改进的基底。
本发明比现有技术中的已有方法具有许多优点。本发明提供一种当暴露于极端的湿度下时具有非常小的卷曲趋势的照相材料。进一步，本发明提供了一种相纸，由于消除了形成聚乙烯的临界性，其成本低得多。由于本发明的双轴定向聚合物片层提供了一用于涂布感光层的高质表面，在形成聚乙烯层上的表面时不再需要难度大且花费高的涂布和冷却。由于彩色材料可被集中于双轴定向层的表面以达到最有效利用而几乎没有着色材料的浪费，所以改进了本发明照相材料的光学性能。本发明的使用微孔化片层的照相材料具有增强的抗扯性。由于微孔化片层在装配入照相材料之前，可对微孔化片层的质量进行筛选，因此本发明的照相材料的生产成本较低。使用现行的聚乙烯层，不能评价层的质量，直至与粘附的聚乙烯防水层完全形成基底相纸之后方可。因此，所有缺陷导致昂贵产品的高额废弃。由于水蒸气不能从乳剂通过双轴定向层透过，因此本发明使得照相纸乳剂更迅速地硬化。
本发明的微孔化片层的另一优点是它们比现有产品的二氧化钛负载的聚乙烯更暗。它们获得这一阻光性有一部分是通过使用孔以及二氧化钛在片层表面的改进的集中。因为照相材料的反面上的定向聚合物片层比聚乙烯更易于抗划伤和其它损伤，所以本发明的照相材料更具有抗划伤性。这些以及其它优点从下面详细的说明中将会是显而易见的。
本文所用术语“顶部”，“上面”，“乳剂面”和“面对”指含有成像层的照相材料的一面。术语“底部”，“下面”和“背对”指照相材料与含有感光成像层或显影影像的一面相对的一面。
任何适宜的双轴定向聚烯烃片层可用作位于本发明层合基底的顶部层。优选微孔化复合双轴定向片层，容易通过将中心与表层一起复合挤压，接着双轴定向来生产，这样在中心层中所含的成孔材料周围形成孔。该复合片层公开在例如，美国专利号4377616，4758462和4632869中，本文引用其所公开内容作为参考。
优选的复合片层中心应为层整个厚度的15-95％，优选为整个厚度的30-85％。无孔表层因此应为层厚度的5-85％，优选为15-70％。
以术语“固体密度的百分数”表示的复合片层的密度(比重)如下计算：
固体密度百分数应为45％至100％之间，优选为67％至100％之间。当固体密度百分数变为小于67％时，由于抗拉强度下降，复合片层变得不易生产，并变得对物理损伤敏感。
复合片层的整个厚度可在12-100微米之间变化，优选20-70微米。在20微米以下时，微孔层不能足够厚，足以使载体中任何固有的平面度最小化，并更难于生产。在高于70微米的厚度时，几乎见不到在表面光滑度或机械性能方面的改进，从而使另外材料费用的进一步增加不具备理由。
本发明的双轴定向片层具有小于1.55×10-4g/mm2/天/大气压的水蒸汽渗透率。由于层合的本发明载体在将乳剂涂布在载体上的过程中未使水蒸汽从乳剂中透过，因而这允许在生产期间更迅速的乳剂硬化。透过率通过ASTM F1249测定。
虽然“孔”可能含有气体，在本文中“孔”被用来指缺乏加入的固体和液体材料。保留在最终组合层中心的产生孔的颗粒直径应为0.1-10微米，优选圆形，以产生所需形状和大小的孔。孔的大小还取决于在机器和横向上的定向程度。理想的，孔呈现出由两个相反且边缘相接的凹面盘所限定的形状。换句话说，孔趋向于具有透镜状或两面凸的形状。孔被定向，从而两个主要尺寸与机器和层的横向匹配。Z方向轴为较短的尺寸，大略为孔颗粒横向直径的大小。孔通常趋向于为封闭的孔，从而实质上没有从孔中心一边通向另一边的通道，其中通过该通道气体或液体可以穿过。
成孔材料可选自多种材料，并应以基于中心基质聚合物重量的约5-50％(重量计)的量存在，优选地，产生孔的材料包含聚合物材料。当采用聚合物材料时，它可以是与产生中心基质的聚合物混熔的聚合物，并且它能在悬浮体冷却时形成分散的球形颗粒。例子包括分散于聚丙烯中的尼龙，分散于聚丙烯中的聚对苯二甲酸丁二醇酯或分散于聚对苯二酸乙二醇酯中的聚丙烯。如果聚合物被预成型并掺入到基质聚合物中，重要的特征是颗粒的大小和形状。优选圆球形，且它们可为空的或固体。这些球体可由交联聚合物产生，其中聚合物选自具有通式Ar-C(R)＝CH2的链烯基芳香化合物，其中Ar代表芳香烃基团，或苯系的芳香卤代烃基团，R为氢或甲基；丙烯酸酯类型的单体包括式CH2＝C(R1)-C(O)(OR)单体，其中R选自氢和含有约1-12个碳原子的烷基，R1选自氢和甲基；乙烯基氯和1，1-二氯乙烯的共聚物、丙烯腈和乙烯基氯的共聚物、乙烯基溴、具有式CH2＝CH(O)COR的乙烯基酯，其中R为含有2-18个碳原子的烷基；丙烯酸、异丁烯酸、衣康酸、柠康酸、马来酸、富马酸、油酸、乙烯基苯甲酸；通过将对苯二酸和二烷基对苯二酸或其成酯衍生物与HO(CH2)nOH系列的1，2-亚乙基二醇反应制备的合成聚酯树脂，其中n为2-10的整数，并且在聚合物分子中具有活性烯键，上述聚酯在其中包含共聚的达20％(重量计)的具活性烯属不饱和键的第二种酸或其酯和其混合物，及选自二乙烯基苯、二甘醇二异丁烯酸酯、富马酸二烯丙基酯、邻苯二甲酸二烯丙基酯和其混合物的交联剂。
用于制备交联聚合物的常规单体的例子包括苯乙烯、丙烯酸丁酯、丙烯酰胺、丙烯腈、异丁烯酸甲酯、乙二醇二异丁烯酸酯、乙烯基吡啶、乙烯基乙酸酯、丙烯酸甲酯、乙烯基苄基氯、1，1-二氯乙烯、丙烯酸、二乙烯基苯、丙烯酰胺甲丙烷磺酸、乙烯基甲苯等。优选的交联聚合物为聚苯乙烯或聚(丙烯酸甲酯)。更优选，它为聚苯乙烯且交联剂为二乙烯基苯。
现有技术熟知的方法产生非均匀大小的颗粒，其特征为宽的颗粒大小分布。可通过筛选覆盖最初大小分布范围的珠来对所产生的珠进行分类。其它方法，如悬浮聚合法，有限聚结直接产生为极均匀的大小的颗粒。
可用制剂将成孔材料覆盖以易化成孔过程。适宜的制剂或润滑剂包括胶体硅石，胶体矾土和金属氧化物，如氧化锡和氧化铝。优选的制剂为胶体硅石和胶体矾土，更优选硅石。可通过本领域熟知的方法制备具有制剂涂层的交联聚合物。例如，优选常规的悬浮聚合法，其中将制剂加入悬浮物中。作为制剂，优选胶体硅石。
成孔颗粒也可为无机圆球体，包括固体或空心玻璃圆球，金属或陶瓷珠或无机颗粒，如粘土，滑石，硫酸钡，碳酸钙。重要的是这些材料不与中心基质聚合物发生化学反应。导致一种或多种下列问题：(a)基质聚合物的结晶动力学的改变，使其难以定向，(b)损坏中心基质聚合物，(c)损伤成孔颗粒，(d)成孔颗粒粘附至基质聚合物上，或(e)产生不希望的反应产物，如毒性或深色部分。成孔材料不应有照相活性或损伤照相材料的性能，其中在照相材料中使用了双轴定向的聚烯烃层。
对于面向乳剂顶部上的双轴定向层，用于双轴定向层的适宜类型的热塑聚合物及优选的复合片层的中心基质聚合物包含聚烯烃。
适宜的聚烯烃包括聚丙烯、聚乙烯、聚甲基戊烯、聚苯乙烯、聚丁烯和其混合物，也可采用聚烯烃共聚物，包括丙烯和乙烯，己烯、丁烯和辛烯的共聚物。优选聚丙烯，因为它的成本低并具有所希望的强度性能，
复合片层的无孔表层可用上述用于中心基质的相同的聚合材料制造。可制造复合片层具有与中心基质相同的聚合材料的表层，或它可具有与中心基质不同的聚合材料的表层。为了相容性，可用辅助层来促进表层与中心的粘附。
可向中心基质和/或表层加入附加物以改善这些层的白度。这包括本领域已知的任何方法，包括加入白色颜料，如二氧化钛，硫酸钡，粘土或硫酸钙。这还包括加入在紫外区吸收能量，在蓝光区发射大部分光的荧光剂，或改善层的物理性能或层的可制造性的任何添加剂。对于照相用途。优选具有浅蓝色调的白色基底。
可通过本领域已知的任何方法来进行这些复合片层的复合挤压，骤冷，定向和热硬化，如通过平层法或起泡法或管式法。平层法包括将混合物挤压通过缝模并迅速在一冷却的浇柱转鼓上骤冷被挤压片，这样片层的中心基质聚合物成分和表层成分在低于它们的玻璃固化温度时被骤冷。接着在高于玻璃化温度，低于基质聚合物的熔化温度时，通过相互垂直方向上的拉伸将骤冷片层双轴定向。可在一个方向，并接着在另一个方向上将片层拉伸，或可在两个方向上同时拉伸。在将片层拉伸后，通过加热至足以结晶或退火聚合物，同时在某种程度抑制片层在拉伸的两个方向上回缩的温度而将其热硬化。
所述的优选在每一侧具有至少三层微孔化中心和一表层的复合片层还可具有可起改变双轴定向层性能作用的附加层。不同的效果可通过附加层来实现。这些层可含有着色剂，抗静电材料或不同的成孔材料以产生具有独特性能的片层。可形成双轴定向层具有能提供改进的粘附性的，或指向载体和照相材料的表面层。如果需要获得一些特殊所需性能，可用多达10层来进行双轴定向挤压。
在复合挤压和定向方法之后，或在浇注和进行完全定向之间，可用任何数量的改善片层性能包括可印性的的涂层，将这些复合片层进行涂布或处理以提供蒸汽防护栅，使它们可被热密封，或改善与载体或感光层的粘附。实例为用于可印性的丙烯酸涂层，用于热密封性能的聚偏二氯乙烯涂层。其它实例包括火焰等离子或电晕放电处理以提高可印性或粘附。
由于在微孔中心具有至少一个无孔表层，片层的抗拉强度被增强并使得它变得更易制造。与用所有微孔化层制备片层相比，它允许以更宽的宽度和更高的拉伸比制造片层。复合挤压这些层进一步简化了生产过程。
本发明一般的双轴定向的微孔化片层结构如下：
固体表层
微孔化中心层
固体表层
在基底相纸与乳剂层相对的一侧的片层可为任何适宜的片层。此片层可为或可不为微孔型的。它可与相纸基材的顶部上的片层具有相同的组成。通常通过复合挤压可含有几层的片层，接着进行双轴定向来制造双轴定向片层。这些双轴定向片层公开在例如美国专利4764425中，其中的公开被本文引作参考。
优选的双轴定向片层为双轴定向聚烯烃片层，最优选为聚乙烯或聚丙烯片层。双轴定向层的厚度应为10-150微米。为15微米以下时，这些层不可能厚到足以将载体中的任何固有的非平面性减至最小，并更加难于生产。在大于70微米的厚度时，未见到表面光滑度或机械性能的改善，因此没有理由进一步增加另外材料的成本。
用于双轴定向层的适宜种类的热塑性聚合物包括聚烯烃、聚酯、聚酰胺、聚碳酸酯、纤维素酯、聚苯乙烯、聚乙烯树酯、聚磺酰胺、聚醚、聚酰亚胺、聚偏二氟乙烯、聚氨基甲酸乙酯、对聚苯硫、聚四氟乙烯、聚缩醛、多磺酸酯、聚酯离聚物和聚烯烃离聚物。这些聚合物的共聚物和/或混合物可被采用。
适宜的聚烯烃包括聚丙烯、聚乙烯、聚甲基戊烯和其混合物。聚烯烃共聚物，包括丙烯和乙烯、己烯、丁烯及辛烯的共聚物也是可采用的。由于共成本低并具有良好的强度和表面性能，所以优选聚丙烯。
适宜的聚酯包括从4-20个碳原子的芳香、脂族或环脂族二羧酸和具有2-24个碳原子的脂族或脂环二元醇制得的那些。适宜的二羧酸的例子包括对苯二酸、间苯二酸、苯二甲酸、萘二甲酸、琥珀酸、戊二酸、己二酸、壬二酸、癸二酸、富马酸、马来酸、衣康酸、1，4-环己烷二羧酸、钠代磺酸基间苯二酸和其混合物。适宜二元醇的例子包括1，2-亚乙基二醇、丙二醇、丁二醇、戊二醇、己二醇、1，4-环己烷二甲醇、二甘醇，其它聚乙二醇和其混合物。现有技术熟知这些聚酯，可通过熟知的方法制备，如美国专利号2465319和美国2901466中描述的那些。优选的连续基质聚酯为具有来自对苯二酸或萘二甲酸和至少一种选自1，2-亚乙基二醇、1，4-丁二醇和1，4-环己烷二甲醇的二元醇的重复单元的那些。尤其优选聚(对苯二酸乙二醇酯)，其中它可被少量其它单体改性。其它适宜的聚酯包括由适宜量的共酸成分，例如芪二羧酸的包含所形成的液晶共聚多酯。这些液晶共聚多酯的例子为公开在美国专利号4420607，4459402和4468510中的那些。
有用的聚酰胺包括尼龙6、尼龙66和其混合物。聚酰胺的共聚物也为适宜的连续相聚合物。有用的聚碳酸酯的例子为双酚A聚碳酸酯。适宜用作复合片层的连续相聚合物的纤维素酯包括硝酸纤维素、三乙酸纤维素、二乙酸纤维素、乙酸丙酸纤维素、乙酸丁酸纤维素，和其混合物或其共聚物。有用的聚乙烯树脂包括聚氯乙烯、聚(乙烯醇缩醛)和其混合物。也可使用乙烯基树脂的共聚物。
可使用相同聚合物材料的层合来制备层合基底背面上的双轴定向片层，或可使用不同聚合物组成的片层来制备它，为了相容性，可使用辅助层来提高各层的粘附。
可向双轴定向的背面片层加入附加物来提高这些片层的白度。这包括现有技术已知的任何方法，包括加入白色颜料，如二氧化钛、硫酸钡、粘土或硅酸钙。这还包括加入在紫外区吸收能量，在蓝光区发射大部分光的荧光剂，或其它将改善片层的物理性能或片层的可制造性的添加剂。
可通过现有技术中已知的用于生产定向片层的任何方法来进行这些双轴定向片层的复合挤压、骤冷、定向和热硬化，例如通过平层法或起泡法或管式法。平层法包括将混合物挤压或复合挤压通过缝模并迅速在一冷却的浇注转鼓上骤冷被挤压或被复合挤压片，这样片层的聚合物成分在低于它们的固化温度下被骤冷。接着在高于聚合物玻璃化温度下，通过相互垂直方向上的拉伸将骤冷片层双轴定向。可在一个方向，并接着在另一个方向将片层拉伸，或可在两个方向上同时拉伸。在将片层拉伸后，通过加热至足以结晶聚合物，同时在某种程度抑制片层在拉伸的两个方向上回缩的温度而将其热硬化。
所述的优选具有至少一层的层合基底的背面上的双轴定向片层也可被提供具有可起改变双轴定向片层性能作用的另外的层。不同的效果可通过附加层来实现，这些层可含有着色剂抗静电材料或滑润剂以产生具有独特性能的片层。可形成双轴定向片层具有提供改进的粘附性的或指向载体和照相材料的表层。如果需要获得一些特殊的所需性能，可用多达10层来进行双轴定向挤压。
在复合挤压和定向方法之后，或在浇注和完全定向之间，可用任何数量的可被用来提高片层性能包括可印性的涂层，对这些双轴定向片层进行涂布或处理以提供蒸汽阻挡层，使它们成为热密封，或改善与载体或感光层的粘附。实例为用于可印性的丙烯酸涂层，用于热密封性能的聚偏二氯乙烯涂层。其它实例包括火焰，等离子或电晕放电处理以提高可印性或粘附。
本发明一般的双轴定向片层的结构如下：
被处理的表层
固体中心层
载体可为聚合、合成相纸、布、织物聚合纤维或纤维素纤维相纸载体或其层压物，其中，微孔复合片层和双轴定向片层被层压至其上用作感光卤化银层的层合载体。基底还可为微孔聚乙烯对苯二甲酸酯，例如公开在美国专利号4912333；4994312和5055371中的那些，其所公开的被本文引作参考。
优选的载体为照相级纤维素纤维相纸。当使用纤维素纤维相纸载体时，优选使用聚烯烃树脂将微孔复合片层挤压层合至基底相纸上。通过在其中应用粘附剂，将本发明的双轴定向片层和基底相纸组合在一起，接着将它们在一个辊隙，如两个辊之间压制来进行挤压层合。在它们被放置到辊隙中之前，可将粘附剂加入到双轴定向片层或基底相纸。在一个优选形式中，粘附剂与双轴定向片层和基底相纸同时放入辊隙中。粘附剂可为任何对照相材料无有害作用的适宜材料。优选的材料为聚乙烯，它在被放入到相纸和双轴定向片层之间的辊隙时熔化。
在层压法期间，为了将产生的层合载体的卷曲减小到最小程度，需要维持对双轴定向片层强度的控制。对于高湿度度应用(＞50％RH)和低湿度应用(＜20％RH)，需要对前面和后面膜均进行层压以将卷曲保持至最小限度。
在一个优选具体实例中，为了生产具有所需照相外观和质感的照相材料，优选使用相对厚的相纸载体(例如至少120μm厚，优选120-250μm厚)和相对薄的微孔复合片层(如小于50μm厚，优选20-50μm厚，较优选30-50μm厚)。
照相材料可为单色材料或多色材料。多色材料含有对光谱的三个主要区均敏感的影像染料形成单元。每一单元可包含对光谱给定区域敏感的单一乳剂层或多个乳剂层。材料的各层，包括成像单元的层，可按现有技术中已知的各种顺序排列。在另一种方式中，对光谱的三个主要区均敏感的乳剂可被安排作为单一分开的层。
用于本发明的照相乳剂通常通过使用现有技术常规方法将卤化银晶体沉淀于胶体基质中来制备。胶体通常为亲水性的成膜试剂，如明胶，藻酸或其衍生物。
洗涤沉淀步骤中形成的晶体，接着通过加入光谱敏感染料和化学增感剂，并提供一加热步骤，其中在此期间提高乳剂温度，通常为40℃-70℃，并保持一段时间来进行化学和光谱增感。在制备本发明采用的乳剂中使用的沉淀和光谱及化学增感法可为现有技术中已知的那些方法。
乳剂的化学增感一般采用增感剂，如含硫化合物，如异硫氰酸烯丙酯、硫代硫酸钠和烯丙基脲；还原剂，如聚胺和亚锡盐；贵金属化合物，如金，铂；和聚合物试剂，如聚亚烷基氧化物。如所描述的，采用热处理来完成化学增感作用。光谱增感作用借助于染料的混合来完成，其中染料被设计为在可见光或红外线光谱中具有感光趣的波长范围，业已知在热处理之前和之后加入这些染料。
在光谱增感作用之后，乳剂被涂覆于载体上。各种涂覆技术包括浸涂，空气刮涂法，幕涂和挤压贴胶。
用于本发明的卤化银乳剂可包括任何卤化物类型。因此，它们可包括氯化银、碘氯化银、溴化银、氯溴化银、溴氯化银、氯碘化银、溴碘化银、氯溴化银、溴碘氯化银、氯溴碘化银和溴氯碘化银。然而，优选乳剂主要为氯化银乳剂。主要为氯化银，指多于约50％摩尔乳剂晶粒为氯化银。优选地，它们为大于约90％摩尔的氯化银；和最佳为大于约95％摩尔的氯化银。
该卤化银乳剂可含有任何大小和形状的晶粒。因此，晶粒可呈立方体，八面体，立方体一八面体，或任何其它天然形成的立方体晶格类型的卤化银晶粒的形状。而且，晶粒可为不规则的，如球形晶粒或平片状晶粒。具有平片状或立方体形状的晶粒为优选的。
本发明的照相材料可采用如照相过程原理(The Theory of thePhotographic process)第4版，T.H.James，Macmillan Publishing CompanyInc.，1977，P.151-152中描述的乳剂。业已知还原增感作用提高卤化银乳剂的照相敏感性。虽然还原增感的卤化银乳剂通常呈现出良好的照相速度，但它们通常导致不需要的灰雾和不良的贮存稳定性。
可通过加入还原增感剂，将银离子还原形成金属银原子的化学物质，或通过提供一还原环境，如高pH(过量的氢氧根离子)和/或低PAg(过量银离子)来有目的地进行还原增感作用。在卤化银乳剂的沉淀过程中，当例如迅速加入硝酸银或碱性溶液或混合不匀而形成乳剂晶粒时，可发生无意识的还原增感作用。而且，在存在催熟剂(晶粒生长改良剂)，如硫醚、硒醚，硫脲或氨时卤化银乳剂的沉淀具有易化还原增感作用的趋势。
为还原增感乳剂可在沉淀或光谱/化学增感作用期间使用的还原增感剂及条件的例子包括抗坏血酸衍生物；锡化合物；聚胺化合物；和描述于美国专利2487850；2512925和英国专利789823中的硫脲二氧化物基化合物。在S.Collier照相科学和工艺(Photographic Science andEngineering)23，113(1979)中讨论了还原增感剂或条件的具体例子，如二甲基氨基甲硼烷，氯化亚锡、肼、高pH(pH8-11)和低pAg(pAg1-7)成熟剂。在EP0348934(Yamashita)，EP0369491A1(Yamashita)，EP0371388(Ohashi)，EP0396424A1(Takada)，EP0404142A1(Yamada)和EP0435355A1(Makino)中描述了用于有目的地制备还原性增感的卤化银乳剂的方法的实例。
如研究公开(Research Disclosure)1996年9月，项38957，第I章，Kenneth Mason Publications Ltd.出版，Dudley Annex，12a North Street，Emsworth，Hampshire P010 7DQ，英国中所描述的，本发明的照相材料可使用添加有VIII族金属，如铱，铑，锇和铁的乳剂。此外，在Carroll，“铱增感作用：文献综述”，照相科学和工艺，Vol.24，No.6，1980中包含铱在卤化银乳剂增感作用中的应用的综述。美国专利4693965描述在铱盐和照相光谱增感染料存在时，通过化学增感乳剂制备卤化银乳剂的方法。在一些情况下，当添加这些掺入物时，当用如英国照相年刊杂志(The British Journal of Photography Annual)1982，P.201-203中所描述的E-6回色法处理时，乳剂呈现出增多的新灰雾和较低的对比感光曲线。
本发明一般的多色彩照相材料包含本发明的层合载体，该层合载体具有氰基染料成像单元包含至少一个与至少一个氰基染料形成成色剂相关联的红色感光卤化银乳剂层；品红成像单元包含至少一个与至少一个品红染料形成成色剂相关联的绿色感光卤化银乳剂层；和黄色染料成像单元，包含至少一个与至少一个黄色染料形成成色剂相关联的兰色感光卤化银乳剂层。该材料可含有另外的层，如滤光层，中间层，保护涂层，下层等。本发明的载体还可用作黑白照相印相材料。
如美国专利4279945和4302523所描述的，照相材料还可包含透明磁记录层，如在透明载体的底面含有磁性颗粒的层。通常，该材料具有的约5-约30微米的总厚度(排除载体)。
在下表中，参考(1)研究公开，1978年12月，项17643，(2)研究公开，1989年12月，项308119，和(3)研究公开，1996年9月项38957，均由Kenneth Mason Publication，Ltd.出版，Dudley Annex，12a North.Street，Emsworth，Hampshire P010 7DQ，英国。认为该表及表中所引参考文献描述了适用于本发明材料的具体成分。此表及所引参考文献也描述了制备，曝光，冲洗加工和操作该照相材料及其中所包含的影像的方法。
| 参考文献 | 章节 | 主题 |
| 123 | I，III，II，IX，XXI，XII，XIV，XVI，II，III，IXA&B | 晶粒组合物，形态学和制备。乳剂制备，其中包括硬化，涂覆过程，附加物等。 |
| 123 | III，IVIII，IVIV，V | 化学增感作用和光谱增感作用/减感的作用。 |
| 123 | VVVI | 紫外染料，荧光增白剂，发光染料 |
| 123 | VIVIVII | 防灰雾剂和稳定剂 |
| 123 | VIIIVIII，XIII，XVIVIII，IX C&D | 吸收剂和分散剂；抗静电层；无光泽剂。 |
| 123 | VIIVIIX | 像成色剂和像调节成色剂，染料稳定剂和色彩调节剂。 |
| 123 | XVIIXVIIXV | 载体 |
| 3 | XI | 具体的层排列 |
| 3 | XII，XIII | 底片工作乳剂；直接正片乳剂 |
| 23 | XVIIIXVI | 曝光 |
| 123 | XIX，XXXIX，XX，XXIIXVIII，XIX，XX | 化学冲洗加工；显影剂 |
| 3 | XIV | 扫描和数字处理方法 |
可用各种形式能量对照相材料曝光，其包括紫外线，可见光和电磁光谱的红外区以及电子束，β射线，γ射线，X-射线，α粒子，中子射线，和其它形式的颗粒和由激光产生的非相干(无规则相)形式或相干(规则相)形式的波样辐射能量。当照相材料被打算曝光于X-射线时，它们可包含在常规放射线照相材料中可找到的特征。
优选将照相材料曝光于光化辐射线中，通常在光谱的可见光区域以形成潜像，接着冲洗加工形成可见像，优选不通过热处理。优选用已知的RA-ATM(Eastman Kodak Company)方法或其它适宜于显影高氯乳剂的冲洗加工体系来进行冲洗加工过程。
本发明的层合底物可具有复制限制特征，例如1996年2月8日递交的美国专利申请号08/598785同用一天递交的申请号08/598778中公开所包括的。这些申请公开了通过向文件中埋入不可见的网点(microdots)来维持文件复印的限制性。然而，这些网点可被数字文件复印机的电光扫描仪检测到。网点图案可包含于整个文件。该文件还可具有彩色边缘或在背面具有不可见的网点以使得使用者或机器能阅读和识别存储介质。该介质可呈能显示影像的片层的形式，通常的这些材料为照相纸和软片材料，由聚乙烯树脂涂覆的相纸、聚酯、(聚)乙烯萘酸酯和三乙酸纤维基材料构成。
网点可为任何规则或不规则形状，其大小小于各网点被察觉到足以降低影像的有效性的最大大小，并且最小水平由扫描仪的检测水平来限定。网点可以中心至中心的控制间距规则或不规则地分布以避免文件密度的增加。网点可为任何色调，明暗度和不导致随意观察足以检测出的饱和度，但优选为至少人眼可分辨的色调，还有适宜地与用于最佳检测的文件扫描仪的敏感性一致。
在一个具体实例中，携带信息的文件由载体，涂覆在载体上的成像层及定位于载体和成像层之间以提供复制限制性介质的网点图案所组成，可在产生原始文件之前或之后，通过各种印片技术实现将网点图案掺入文件介质中。网点可由任何有色物质组成，虽然取决于文件的性质，但着色剂可为半透明，透明或不透明的。在应用保护层之前，优选将网点图案定位在载体层，除非保护层含有光散射颜料。接着网点应位于这些层之上，优选被保护层涂覆。网点可由选自照相技术中已知的影像染料和过滤染料的着色剂组成，并分散于用于印刷墨或光敏感介质的粘合剂或载体中。
在一个优选的具体实例中，可通过将感光材料对电磁照射的可见或不可见波长进行瞬时、立体和光谱曝光产生作为潜像的网点图案。通过采用标准的照相化学冲洗加工，可使得潜像网点图案可被检测。该网点尤其可用作彩色和黑白成像照相介质，虽然通常照相介质含有至少三个卤化银照敏感层，但该照相介质一般含有至少一个卤化银照射敏感层。该介质还可含有多个对照射的相同区域敏感的层。如公开在研究公开37038，1995年2月中所述层的排列可采取现有技术中技术人员已知的任何形式。
下面实施例说明本发明的实践。它们不被认为穷尽了本发明所有可能的变化。除非另有说明，份和百分数按重量计。商业级相纸的实施例
通过将50％漂白的硬木牛皮纸，25％漂白的硬木亚硫酸盐纸浆和25％漂白的软木亚硫酸盐纸浆的精制纸浆配料通过一双盘匀浆机，接着通过Jordan锥形匀浆机匀浆和匀浆至200cc的加拿大标准打浆度。向产生的纸浆配料中加入基于干重的0.2％烷基乙烯酮二聚体，1.0％阳离子玉米淀粉，0.5％聚酰胺表氯醇，0.26阴离子聚丙烯酰胺和5.0％ TiO2。在长网造纸机上生产出约46.5Lbs/1000sq.ft.(Ksf)的无水干重的基底相纸，湿压至42％的固体，使用蒸气加热干燥器干燥至10％的湿度，得到160Sheffield单元的Sheffield孔隙度和0.70g/cc的表观密度。用10％羟乙基化的玉米淀粉溶液，使用垂直上胶挤压将相纸基底进行表面上胶以获得3.3％(重量计)的淀粉上胶。表面上胶载体被砑光为1.04gm/cc的表观密度。实施例实施例1
通过挤压层合下面的片层至照相级纤维素相纸载体的两面制备下面的层合照相基底：顶部片层：(乳剂侧)Oppalyte 350TW(Mobil Chemical Co.)
复合片层(38μm厚)(d＝0.62g/cc)由具微孔和定向的聚丙烯中心(整个片层厚度的约73％)组成，在各面具有二氧化钛着色的无微孔定向的聚丙烯层；成孔材料为聚(对苯二甲酸丁二醇酯)。底部片层：(背侧)BICOR 70 MLT(Mobil Chemical Co.)
一面无光光洁度，一面经处理的聚丙烯片层(18μm厚度)(d＝0.9g/cc)由固体定向聚丙烯中心组成。
上面顶部和底部片层一起被用纯聚烯烃(25g/m2)挤压层合至照相级纤维素相纸载体上。
接着将该层合载体用彩色感光卤化银层涂覆。
为了评价上面照相材料的卷曲，使用柯达卷曲试验(Kodak CurlTest)。
该试验测量抛物线形变样品中的卷曲量。将8.5cm直径的复合物的圆形样品在试验湿度下贮存21天。所需时间的长短取决于被施加在湿度敏感相纸基底上的叠层的蒸汽阻挡层性能，并应根据需要进行调节，确定在测试湿度中使样品重量平衡的时间。卷曲读数以ANSI卷曲单位表示，具体地即100除以曲率半径(英寸)。
通过目视将卷曲的形状，沿卷曲轴的可视度与背景中标准曲线比较确定曲率半径。试验的标准偏差为2个卷曲单位。卷曲可为正向的反向的，并且对于照相产品，通常情况是正向面向感光层卷曲。
实施例1的卷曲结果示于下表1中。
表I
卷曲单位100/r
％湿度 对照 实施例I
5 22 12
20 6 4
50 -7 -1
85 -18 2
上面数据表明当在两面与双轴定向片层一起挤压层合时，与用作相关现有技术的基底的照相基底相比，照相级纤维素相纸在照相纸卷曲方面是最佳的。实施例2
通过在两面挤压层合下面片层至照相级纤维素相纸载体两面来制备下面层合的照相基底：顶部片层(乳剂侧)PF1.OPPalyte 350TW(Mobil Chemical Co.)
复合片层(38μm厚度)(d＝0.50g/cc)由微孔化和定向的聚丙烯中心(整个片层厚度的约73％)组成，在各面具有二氧化钛着色的无微孔定向的聚丙烯层；成孔材料为聚(对苯二甲酸丁二醇酯)。PF2.OPPalyte 350TW(Mobil Chemical Co.)
复合层(38μm厚度)(d＝0.70g/cc)由微孔化和定向的聚丙烯中心(整个片层厚度的约73％)组成，在各面具有二氧化钛着色的无微孔定向的聚丙烯层；成孔材料为聚(对苯二甲酸丁二醇酯)。PF3.OPPalyte 350 TW(Mobil Chemical Co.)
复合片层(38μm厚度)(d＝0.90g/cc)由固体定向的聚丙烯片层组成。底部片层：BICOR 70 MLT(Mobil Chemical Co.)
一面无光光洁度一面被处理的聚丙烯片层(18μm厚度)(d＝0.9g/cc)由固体定向的聚丙烯中心组成。
通过用纯的聚烯烃(25g/m2)挤压层合至照相级纤维素相纸载体上制备下面三种样品：
载体A：PF1顶部片层和70MLT底部片层
载体B：PF2顶部片层和70MLT底部片层
载体C：PF3顶部片层和70MLT底部片层
为了评价上面照相材料的不透明度，用Hunter分光光度计CIE体系D65来进行标准的不透明度试验。在此试验中，由标准的彩色相纸组成的对照样品被用来比较结果。该不透明度试验使用大小为25×106cm的样品段并测定样品的不透明度。如下计算不透明度的百分比：其中样品的不透明度等于所测得载体样品的不透明度，对照的不透明度等于标准彩色照相载体的不透明度。结果示于下表II中：
表II
不透明度改善数据表
| 载体 | ％不透明度 |
| 载体A | 103.40％ |
| 载体B | 100.50％ |
| 载体C | 98.20％ |
| 对照 | 100％ |
上面的数据表明，通过将微孔双轴定向片层(载体A和载体B情况中)挤压层合至标准的纤维素照相纸，照相载体的不透明度比相关现有技术中使用的照相载体优越。无微孔的载体C具有较小的不透明度。这表明当与对照比较时，微孔载体A和B优异的不透明度。在不透明度不是第一重要的情况时，如当它被二氧化钛涂覆，但仍获得增加的抗卷曲性和改善的影像质量时，使用载体C也会是满意的。实施例3
通过挤压层合下面的片层至照相级纤维素相纸载体的两面制备下面的层合照相基底。顶部片层OPPalyte 350TW(Mobil Chemical Co.)
复合层(38μm厚度)(d＝0.75g/cc)由微孔化和定向聚丙烯中心(整个片层厚度的约73％)组成具有一面为二氧化钛着色系统(包括所需的色彩调节)的无微孔定向的聚丙烯层和纯无微孔定向聚丙烯层面；成孔材料为聚(对苯二甲酸丁二醇酯)。底部片层：BICOR 70 MLT(Mobil Chemical Co.)
一面无光光洁度，一面经处理的聚丙烯片层(18μm厚度)(d＝0.9g/cc)由固体定向的聚丙烯中心组成。
上面顶部和底部片层均被用纯聚烯烃(25g/m2)挤压层合至照相级纤维素相纸载体上。
由于在加入其它感光层以前测定了白度，所以不需用彩色感光卤化银层涂覆该层合载体。
为了评价上面照相材料的白度，采用HUNTER分光光度计CIE系统D65方法来测定L Star UVO(紫外光滤出)。在此试验中，采用由标准的彩色相纸组成的对照样品来比较结果。92.95的L Star UVO值被认为正常。实施例的结果为93.49，在所需方向上有显著变化。
上面数据表明，当在两面与双轴定向片层一起挤压层合时，与相关现有技术所用的照相基底相比，照相级纤维素相纸在照相白度方面是最佳的。实施例4
通过挤压层合下面的片层至照相级纤维素相纸载体的两面制备下面的层合照相基底。顶部片层：OPPalyte 350 TW(Mobil Chemical Co.)
复合层(38μm厚度)(d＝0.62g/cc)由微孔化和定向聚丙烯中心(整个片层厚度的约73％)组成，在各面具有二氧化钛着色的无微孔定向的聚丙烯层；成孔材料为聚(对苯二甲酸丁二醇酯)底部片层：BLCOR 70 MLT(Mobil Chemical CO.)
一面无光光洁度，一面经处理的聚丙烯片层(18μm厚度)(d＝0.9g/cc)由固体定向的聚丙烯中心组成。
组装的结构表明了具有比其它用聚乙烯或其它聚烯烃涂覆的相纸基底结构更为优秀的抗撕裂性。
为了评价抗撕裂性，使用TAPPI法414，通过埃尔曼多夫扯裂试验测试上面的结构及标准的彩色载体的对照样品。结果示于下表III中。
表III
| 通过相对挤压涂层聚乙烯层压BOPP进行的埃尔曼多夫扯裂的改进 | |||
| 对照 | Lam.w BOPP | ％变化 | |
| 机械方向 | 99 | 122 | 23 |
| 横向 | 110 | 151 | 37 |
*BOPP为双轴定向聚丙烯
上面数据表明当在两面与双轴定向片层一起挤压层合时，与用作相关现有技术的基底的照相基底相比，照相级纤维素相纸在照相基底抗撕裂性方面是最佳的。实施例5
通过将约等摩尔的硝酸银和氯化钠溶液加入至含明胶胶溶剂和硫醚催熟剂的搅拌均匀的反应器中来制备黄色乳剂YE1。加入制备形成过程的1-70％的戊氯亚硝酰基锇酸盐和制备形成过程的93％的碘化钾以形成磺化银晶粒的带。得到的乳剂含有边长大小为0.60μm的立方体形状的晶粒。通过加入戊二酰二氨基苯基硫化物，接着加入硫化亚金的胶体悬浮物并倾斜加热至60℃来将该乳剂进行最佳增感，其中在此期间加入定时兰色感光染料，Dyel，六氯铱酸钾(potassium hexachloroiridate)，Lippmann溴和1-(3-乙酰氨基苯基)-5-巯基四唑。
通过将约等摩尔硝酸银和氯化钠溶液加入至含有明胶胶溶剂和硫醚催熟剂的搅拌均匀的反应器中来沉淀品红乳剂ME1。所得乳剂含有边长大小为0.30μm的立方体形状的晶粒。通过加入硫化亚金的胶体悬浮物并加热至55℃将该乳剂进行最佳增感。接着加入下面成分：六氯铱酸钾，Lippmann溴和绿色感光染料，Dye2。接着将最终乳剂冷却，并在冷却开始后几秒钟加入1-(3-乙酰氨基苯基)-5-巯基四唑。
通过将约等摩尔的硝酸银和氯化钠溶液加入至含有明胶胶溶剂和硫醚催熟剂的搅拌均匀的反应器中来沉淀氰基乳剂CE1。此外，在此制备中加入汞。所得乳剂包含边长大小为0.40μm的立方体形晶粒。通过加入双(1，4，5-三甲基-1，2，4-三唑 -3-硫醇)氟硼酸金(I)和硫代硫酸钠，并接着在65℃加热浸煮来将该乳剂进行最佳增感。接着加入下面成分：1-(3-乙酰氨基苯基)-5-巯基四唑，六氯铱酸钾和溴化钾。将乳剂冷却至40℃，加入红色感光染料Dye3。
通过现有技术已知方法将乳剂YE1，ME1和CE1与携带成色剂的分散剂混合，并涂施于根据表格1中所示结构的实施例1的分层基底上以制备具有低卷曲和优异的强度性能的照相材料。
表格1
项目说明 沉淀作用
(Laydown mg/ft2)层1 兰色感光层
明胶 122
黄色乳剂YE1(如Ag) 20
Y-1 45
ST-1 45
S-1 20层2 中间层
明胶 70
SC-1 6
S-1 17层3 绿色感光层
明胶 117
品红乳剂(如Ag) 7
M-1 29
S-1 8
S-2 3
ST-2 2
ST-3 17.7
ST-4 57
PMT 10层4 紫外中间层
明胶 68.44
UV-1 3
UV-2 17
SC-1 5.13
S-1 3
S-2 3层5 红色感光层
明胶 126
氰基乳剂CE1 17
C-1 39
S-1 39
UV-2 25
S-2 3
SC-1 0.3层6 紫外涂层
明胶 48
UV-1 2
UV-2 12
SC-1 4
S-1 2
S-3 2层7 SOC
明胶 60
SC-1 2
ST-1＝N-叔丁基丙烯酰胺/正丁基丙烯酸酯共聚物(50∶50)
S-1＝二丁基邻苯二甲酸酯
S-2＝二十一烷基邻苯二甲酸酯
PMT＝1-苯基-5-巯基四唑
S-3＝1，4-环己基二亚甲基双(2-乙基己酸酯)
S-4＝乙酸2-(2-丁氧基乙氧基)乙酯
已具体参考其优选实例对本发明进行了详细描述，但是应理解可在本发明的实质和范围内进行变化和修改。
Claims (19)
1、一种照相材料，包括一相纸基底，至少一个感光卤化银层以及所述相纸基底和所述至少一个卤化银层之间的微孔化双轴定向聚烯烃片层。
2、权利要求1的照相材料，其中所述材料进一步包括在所述基底相纸的所述感光卤化银层反面的双轴定向聚烯烃片层。
3、权利要求1的照相材料，其中所述微孔聚烯烃片层包括固体百分密度为约77％至约100％的片层。
4、权利要求1的照相材料，其中所述微孔聚烯烃片层包括固体百分密度为80％至87％的片层。
5、权利要求1的照相材料，其中所述微孔化聚烯烃片层包括无微孔材料的表层。
6、权利要求1的照相材料，其中所述微孔聚烯烃片层包括位于各表面上的表层。
7、权利要求1的照相材料，其中所述微孔聚烯烃片层具有约13-65微米的厚度。
8、权利要求1的照相材料，其中所述微孔聚烯烃片层包括含二氧化钛的层。
9、权利要求1的照相材料，进一步包括位于所述微孔片层和所述相纸基底之间的聚乙烯层。
10、权利要求1的照相材料，其中所述微孔片层具有约689MPa至5516Mpa之间的杨氏模量。
11、权利要求1的材料，其中所述双轴定向片层是微孔化的。
12、权利要求1的材料，其中所述片层具有小于1.55×10-4g/mm2天/大气压的水蒸气传递速率。
13、一种形成照相材料的方法，包括提供一制备好的双轴定向聚烯烃片层，提供一基底相纸，将粘合剂加至所述基底相纸上，并同时将所述微孔片层放至所述粘合剂上以使所述微孔片层与所述基底相纸粘合在一起。
14、权利要求13的方法，其中所述双轴定向片层是微孔化的。
15、权利要求13的方法，其中所述粘合剂包括聚烯烃。
16、权利要求13的方法，其中所述粘合剂包括挤压至所述基底相纸上的聚乙烯。
17、权利要求13的方法，其中所述粘合剂包括粘合剂聚合物。
18、权利要求13的方法，其中所述方法进一步包括将粘合剂加至与所述相纸基底相反的一面上并将双轴定向片层放到所述相纸基底的与微孔片层相反的一面上。
19、权利要求1的材料，进一步包括定位于所述至少一个卤化银层与所述双轴定向聚烯烃片层之间的网点的复制限性性结构。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US862,708 | 1992-04-03 | ||
| US08/862,708 US5866282A (en) | 1997-05-23 | 1997-05-23 | Composite photographic material with laminated biaxially oriented polyolefin sheets |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1200495A true CN1200495A (zh) | 1998-12-02 |
Family
ID=25339115
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98115424A Pending CN1200495A (zh) | 1997-05-23 | 1998-05-23 | 具有层合双轴定向聚烯烃片层的复合照相材料 |
Country Status (4)
| Country | Link |
|---|---|
| US (2) | US5866282A (zh) |
| EP (1) | EP0880068A1 (zh) |
| JP (1) | JPH10333277A (zh) |
| CN (1) | CN1200495A (zh) |
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-
1997
- 1997-05-23 US US08/862,708 patent/US5866282A/en not_active Expired - Fee Related
-
1998
- 1998-05-11 EP EP98201534A patent/EP0880068A1/en not_active Withdrawn
- 1998-05-22 JP JP10140991A patent/JPH10333277A/ja active Pending
- 1998-05-23 CN CN98115424A patent/CN1200495A/zh active Pending
- 1998-12-10 US US09/208,673 patent/US6043009A/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10333277A (ja) | 1998-12-18 |
| EP0880068A1 (en) | 1998-11-25 |
| US5866282A (en) | 1999-02-02 |
| US6043009A (en) | 2000-03-28 |
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