CN1147864A - 生产稳定光热敏材料的方法 - Google Patents
生产稳定光热敏材料的方法 Download PDFInfo
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- CN1147864A CN1147864A CN95192768A CN95192768A CN1147864A CN 1147864 A CN1147864 A CN 1147864A CN 95192768 A CN95192768 A CN 95192768A CN 95192768 A CN95192768 A CN 95192768A CN 1147864 A CN1147864 A CN 1147864A
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- Prior art keywords
- silver
- layer
- ground floor
- solvent
- acid
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- 238000004519 manufacturing process Methods 0.000 title abstract 2
- 229910052709 silver Inorganic materials 0.000 claims abstract description 77
- 239000004332 silver Substances 0.000 claims abstract description 77
- -1 silver halide Chemical class 0.000 claims abstract description 53
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 44
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229920002678 cellulose Polymers 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 19
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 59
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 230000002829 reductive effect Effects 0.000 claims description 18
- 239000007767 bonding agent Substances 0.000 claims description 13
- 229920000642 polymer Polymers 0.000 claims description 11
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- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
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- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 6
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Classifications
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- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/494—Silver salt compositions other than silver halide emulsions; Photothermographic systems ; Thermographic systems using noble metal compounds
- G03C1/498—Photothermographic systems, e.g. dry silver
- G03C1/49881—Photothermographic systems, e.g. dry silver characterised by the process or the apparatus
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/494—Silver salt compositions other than silver halide emulsions; Photothermographic systems ; Thermographic systems using noble metal compounds
- G03C1/498—Photothermographic systems, e.g. dry silver
- G03C1/49872—Aspects relating to non-photosensitive layers, e.g. intermediate protective layers
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/74—Applying photosensitive compositions to the base; Drying processes therefor
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/74—Applying photosensitive compositions to the base; Drying processes therefor
- G03C2001/7451—Drying conditions
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/76—Photosensitive materials characterised by the base or auxiliary layers
- G03C1/795—Photosensitive materials characterised by the base or auxiliary layers the base being of macromolecular substances
- G03C2001/7952—Cellulose ester
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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
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S430/00—Radiation imagery chemistry: process, composition, or product thereof
- Y10S430/136—Coating process making radiation sensitive element
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
Abstract
一种生产光热敏材料的方法,包括步骤:a)提供一基材,b)在上述基材上涂布第一层,所述第一层包括有机聚合物粘合剂、卤化银、可还原银盐或银配合物和有机溶剂,c)所述第一层中70%的溶剂从所述第一层除去前,将包括溶剂和第二种聚合物粘合剂的第二层涂于所述第一层上,所述第二种聚合物粘合剂包括至少一种纤维素酯,所述第一层和所述第二层的至少一层含有银离子的还原剂。
Description
本发明涉及含光热敏卤化银的材料(element)和在多层涂布方法中生产这些材料的方法,由此这些材料显示改进的后期显影照片稳定性,特别是在取景盒(viewbox)中的稳定性。多层涂层体系与单层涂层相比,即使当在两个方法中使用相同的化学药品时,也显示改进的稳定性。
卤化银光热敏成像材料(因形成最终影像不需要液体显影常常称为“干式银”组合物),在本领域中已经知晓数年了。这些成像材料基本上包括对光不敏感的可还原银源、光敏材料(当光照射时生成银)和银源的还原剂。光敏材料一般为照相卤化银,它必须催化接近于对光不敏感的银源,催化接近是这两种材料的紧密物理联系,因此当通过照射照相卤化银或使照相卤化银曝光产生银斑点或银核时,这些银核可通过还原剂使银源催化还原。长期以来人们认为银是银离子还原的催化剂,同时可使产生银的光敏卤化银催化剂前体按多种不同方式与银源催化接近,所述方式的例子如银源与含卤源的部分复分解(例如,US 3,457,075)、卤化银和银源物质共沉淀(例如,US 3,839,049)和其它密切联系卤化银和银源的方法。
当Dmin区域暴露于来自取景盒的高强度光和热下时,光热敏乳液趋于损害后显影照片稳定性。惯用的光热敏材料具有不良照片稳定性。当样品处于光与热的组合趋于使本底密度变暗的取景盒上时最小密度区域变暗。造成照片稳定性困难的原因是显影剂、调色剂和银都包括于光热敏材料中,而在绝大多数卤化银照相体系中却不是这样的。来自取景盒的光和热也只是在片材成像中所用的光和热的延伸。因此,人们一直认为对改进照片稳定性的要求非常重要。
为改进光热敏材料的后显影照片稳定性,已进行了大量尝试。US4012260公开了通过加入羧酸2-氨基-2-噻唑啉(鎓)盐进行改进。US3877940采用封端硫酮和含卤稳定剂的前体混合物。US 3707377将三溴喹哪啶与六溴环己烷结合抑制背景褪色。在US 3839041中,采用加入包括5-乙酰基-4-甲基-2-(3-氧丁基-1硫代)噻唑的影像稳定剂前体。OrientalPhoto Ind.CO.Ltd.在JP 0288039中提出为生产稳定的片材,通过将三溴苯乙酮加到聚丙烯酸树脂基材上稳定热片材。
在US 4108665和US 4288536中公开了将四溴丁烷作为后显影照片稳定剂。使用酰胺化合物进行后处理稳定化描述于EP 473 351 AZ中。在EP480 568 AZ中用某些吖内酯强化卤化银光热敏乳液的后处理稳定性。在US5149620中,通过加入巯基三唑改进后处理稳定性。然而,并未发现这些化合物对于在取景盒中使用的光热敏材料产生足够的后显影照片稳定性。
已发现,将特定类型的树脂与特定涂布方法相结合对于改进光热敏卤化银材料,特别是薄膜材料上的后显影照片的稳定性是一个很有效的体系。当单层涂布时,纤维素酯树脂显示较差的照片稳定性。当这些树脂在光热敏材料中作为含湿银层上的罩面层或面漆涂层时,可制得具有改进的照片稳定性的光热敏片材。
在包括感光卤化银、有机银源(通常为银盐或银配合物)和银离子的还原剂的光热敏材料的Dmin区域中产生的晒像(print-out)可通过使用纤维素酯如乙酸纤维素、乙酸丁酸纤维素或乙酸丙酸纤维素与多层涂布方法相结合的方式降低。当在单层涂布方法中(在银释放(trip)层和罩面层或面漆涂层中)使用相同的树脂时,损害了照片的稳定性。多层涂布工艺涉及在湿状态下在各层上涂布第一层和第二层。单层涂布方法涉及涂布第一层,使该涂层干燥,然后涂布第二层并使此结构干燥。
在多层光热敏材料(特别是黑白光热敏材料)的一般涂布方法中,在将下一层例如罩面层涂于银释放层之前使银释放层(在有溶剂(通常为有机溶剂)的粘合剂中同时含有卤化银或其前体和可还原银源的层)干燥。干燥通常导致除去90%(重量)以上的载有粘合剂和银组分的有机溶剂(或含水溶剂)。在实施本发明中,将湿银释放层用纤维素酯层涂覆。在实施本发明中,“湿层”是基材上的那一层,初始涂布(即由窄缝涂布机、幕式淋涂机、刮板式涂布机等)时该层中含有至少30%(重量)的溶剂浓度(相对于粘合剂)。当将第二层(例如纤维素酯层)涂于第一下层上时,优选至少50%(重量),更优选至少70%(重量),最优选至少80%,90%,95%或100%的溶剂保留于第一下层中。纤维素酯层包括至少1%的纤维素酯粘合剂,这种粘合剂的浓度越高,结果越好。在第二下层中(面漆层或罩面层)中,至少50%(重量)的粘合剂包括纤维素酯是优选的。更优选地,罩面层包括至少75%,更优选至少90%,最优选至少100%的纤维素酯物质。尽管在银释放第一下层中可使用任何粘合剂,但对于该层优选的成膜有机聚合物粘合剂是聚乙烯醇缩醛,最优选聚乙烯醇缩丁醛。
本发明方法一般可描述为:a)提供一基材(优选透明聚合物薄膜),在所述基材上涂布第一层,第一层包括卤化银(或其前体)、可还原银源(例如银盐或银配合物)、有机聚合物粘合剂树脂和溶剂(通常为聚合物粘合剂的溶剂),b)在第一层干燥前(例如除去第一涂布层中的70%的溶剂之前)将第二层涂于所述第一层上,然后干燥该光热敏材料(例如总共除去两层中总溶剂的至少90%(重量))。两个涂布层中至少一层含有银离子的还原剂,这对于光热敏方法是必须的。
至少银释放层,相邻的纤维素酯层或与银释放层相邻的另一层必须含有光热敏材料所需的银离子的还原剂。所需的其它组分分布于这两层或其它层中。
本发明的光热敏乳液可在基材上构成两层或多层。虽然预计两层结构包括一个含有所有组分的乳液层和一个防护面漆层,但此两层结构必须在一个乳液层(通常为与基材相邻的层)中含有银源和卤化银,在第二层或这两层中含有其它组分。多色光热敏结构对每一种颜色可含有这些双层组,或如US 4,708,928中所述它们在一个单层中可含有所有组分。对于多层多色光热敏制品,如US 4,460,681中所述,一般通过在各种感光层之间使用官能或非官能阻挡层使各乳液层保持相互分离。
然而对于实施本发明则不必要,可便利地将汞(II)盐加入乳化层作为防灰雾剂。为此,优选的汞(II)盐是乙酸汞和溴化汞。
用于本发明的光敏卤化银一般可使用0.75至25mol%,优选2至20mol%的有机银盐。
卤化银可以是任何光敏卤化银如溴化盐、碘化银、氯化银、碘溴化银、碘氯溴化银、溴氯化银等。
卤化银可以为任何光敏性的形式,包括(但不限于)立方、正交、平片、四面体形状等,并可在其上取向生长晶体。
用于本发明的卤化银可不必改性而使用。然而,也可用化学增感剂如含硫、硒或铊等的化合物,含金、铂、钯、铑或铱等的化合物,还原剂如卤化锡等,或其混合物进行化学增感改性。这些方法详细描述于T.H.James“The Theory of the Photographic Process”,第四版,第5章,P149至169中。
卤化银可以任何方式加入乳液层中,使其催化接近银源。可将在粘合剂中分别形成或“预制”的卤化银或有机银盐在用于制备涂料溶液之前进行混合,但将其在球磨机中长时间共混也是有效的。此外,使用包括在制备的有机银盐中加入含卤化合物使有机银盐的银部分转化为卤化银的方法是有效的。
制备这些卤化银和有机银盐的方法和将其共混的方式在本领域是已知的并描述于Research Disclosure,1978年6月,17029条和US 3,700,458中。
本发明使用的预制卤化银可以不洗涤或进行洗涤以除去可溶性盐。在后一情况下,可通过冷却凝固和沥滤除去可溶性盐或乳液可(例如)通过US 2,618,556;2,614,928;2,565,418;3,241,969和2,489,341中描述的方法洗涤凝结。卤化银颗粒可以是任何结晶形式,包括(但不限于)立方、四面体、正交、平片、薄片、片晶形状等。
有机银盐可以是含有可还原银离子源的任何有机物质。有机酸,特别是长链(10至30,优选15至28个碳原子)脂肪酸的银盐是优选的。有机或无机银盐的配合物(其中配位体具有的总稳定常数为4.0至10.0)也是合适的。
银源材料优选构成成像层的大约5至30%(重量)。
可用于本发明的有机银盐是对光较稳定的银盐,但当在曝光催化剂(如照相卤化银)和还原剂存在下加热至80℃或更高温度时,形成银影。
优选的有机银盐包括具有羧基基团的有机化合物的银盐。其非限制性的例子包括脂族羧酸的银盐和芳族羧酸的银盐。脂族羧酸的银盐的优选例子包括山萮酸银、硬脂酸银、油酸银、月桂酸银、己酸银、肉豆蔻酸银、棕榈酸银、马来酸银、富马酸银、酒石酸银、亚油酸银、丁酸银和樟脑酸银及其混合物等。在脂族羧酸上具有卤原子或羟基的银盐也可以有效地使用。芳族羧酸和其它含羧基的化合物的银盐包括苯甲酸银,取代苯甲酸银如3,5-二羟基苯甲酸银、邻甲基苯甲酸银、间甲基苯甲酸银、对甲基苯甲酸银、2,4-二氯苯甲酸银、乙酰氨基苯甲酸银、对苯基苯甲酸银等,棓酸银,单宁酸银,邻苯二甲酸银,对苯二甲酸银,水杨酸银,苯乙酸银,1,2,4,5-苯四酸银、公开于US 3,785,830中的3-羧甲基-4-甲基-4-噻唑啉-2-硫酮或其类似物的银盐和公开于US 3,330,663中的含硫醚基团的脂族羧酸的银盐等。
也可使用含巯基或硫酮基团的化合物或其衍生物的银盐。这些化合物的优选例子包括3-巯基-4-苯基-1,2,4-三唑的银盐,2-巯基苯并咪唑的银盐,2-巯基-5-氨基噻二唑的银盐,2-(乙基2-羟乙酰胺基)苯并噻唑的银盐,巯基乙酸的银盐如S-烷基(其中烷基具有12至22个碳原子)巯基乙酸的银盐,二硫代羧酸的银盐如二硫代乙酸的银盐,硫代酰胺的银盐,5-羧基-1-甲基-2-苯基-4-硫代吡啶的银盐,巯基三唑的银盐,2-巯基苯并噁唑的银盐,US 4,123,274中描述的银盐,例如1,2,4-巯基三唑衍生物的银盐如3-氨基-5-苄硫基-1,2,4-三唑的银盐,US 3,301,678中公开的硫酮化合物的银盐,例如3-(2-羧乙基)-4-甲基-4-噻唑啉-2-硫酮的银盐。
此外,可以使用含亚氨基基团的化合物的银盐。这些化合物优选的例子包括苯并三唑和其衍生物的银盐,例如苯并三唑的银盐如甲基苯并三唑银等,卤素取代苯并三唑的银盐例如5-氯苯并三唑银等,碳亚胺苯并三唑的银盐等,US 4,220,709中描述的1,2,4-三唑或1-H-四唑的银盐,咪唑或咪唑衍生物的银盐等。还可以使用各种银的乙炔化合物,如US 4,761,361和4,775,613中描述的。
还发现使用银半皂是合适的,其中由市售山萮酸的钠盐水溶液和分析约14.5%的银共沉淀制备的山萮酸银与山萮酸的等摩尔共混物代表一个优选的例子。施用于透明薄膜片基上的透明片材物质需要透明涂料,为此可以使用含不多于约4%或5%的游离羧酸和分析约25.2%的银的山萮酸银全皂
用于生产银皂分散体的方法是本领域公知的,该方法公开于ResearchDisclosure,1983年4月,22812条、Research Disclosure,1983年10月,23491条和US 3,985,565中。
光敏卤化银可有利地用已知的染料进行光谱增感,所述染料包括花青、部花青、苯乙烯、半花青、氧醇、半氧醇和呫吨染料。可用的花青染料包括那些具有碱性核如噻唑啉核、噁唑啉核、吡咯啉核、吡啶核、恶唑核、噻唑核、硒唑核和咪唑核的化合物。可用的优选部花青染料包括那些既具有上述碱性核又具有酸性核如乙内酰硫脲核、绕丹宁核、恶唑烷二酮核、噻唑烷二酮核、巴比土酸核、噻唑啉酮核、丙二腈核和吡唑啉酮核的化合物。在上述花青和部花青染料中,那些具有亚胺基团或羧基基团的化合物是特别有效的。实际上,用于本发明的光谱增感染料可以合适地选自已知的染料,例如US 3,761,279、3,719,495和3,877,943,GB1,466,201、1,469,117和1,422,057中公开的那些染料;并可按已知方法使其处于光致催化剂附近。光谱增感染料的用量对于每摩尔卤化银一般为l0-4mol至约1mol。
用于有机银盐的还原剂可以是能将银离子还原为金属银的任何物质,优选有机物质。常规照相显影剂如菲尼酮、氢醌和邻苯二酚是适用的,但优选受阻酚还原剂。还原剂的存在量应为成像层重量的1至10%。在多层结构中,若还原剂加入除乳化剂层外的层中,则约2至15%的稍高比例将更合适。
对于干式银体系,已公开了各种还原剂,包括偕胺肟例如苯基偕胺肟、2-噻吩基偕胺肟和对苯氧基苯基偕胺肟、吖嗪(例如4-羟基-3,5-二甲氧基苯甲醛吖嗪);脂族羧酸芳基酰肼与抗坏血酸的混合物,如2,2’-双(羟甲基)丙酰-B-苯基酰肼与抗坏血酸的混合物;多羟基苯与羟胺,还原酮和/或肼的混合物(例如氢醌与双(乙氧基乙基)羟胺,哌啶子基己糖还原酮或甲酰基-4-甲苯基肼的混合物);异羟肟酸,如苯基异羟肟酸,对羟苯基异羟肟酸和B-丙氨酸异羟肟酸;吖嗪与亚磺酰氨基苯酚的混合物(例如酚噻嗪与2,6-二氯-4-苯亚磺酰氨基苯酚的混合物);α-氰基苯乙酸衍生物,如α-氰基-2-甲苯乙酸乙酯,α-氰基苯乙酸乙酯;双-B-萘酚,如2,2’-二羟基-1-双萘基,6,6’-二溴-2,2’-二羟基-1,1’-双萘基和双(2-羟基-1-萘基)甲烷;双-B-萘酚与1,3-二羟基苯衍生物(例如2,4-二羟基二苯甲酮或2,4-二羟基苯乙酮)的混合物;5-吡唑啉酮如3-甲基-1-苯基-5-吡唑啉酮;还原酮例如二甲氨基己糖还原酮,脱水二氢氨基己糖还原酮和脱水二氢哌啶酮己糖还原酮;亚磺酰氨基-苯酚还原剂例如2,6-二氯-4-苯亚磺酰氨基苯酚和对苯亚磺酰氨基苯酚;2-苯基二氢化茚-1,3-二酮等;苯并二氢吡喃如2,2-二甲基-7-叔丁基-6-羟基苯并二氢吡喃;1,4-二氢吡啶如2,6-二甲氧基-3,5-二羰乙氧基-1,4-二氢吡啶;双酚(例如双(2-羟基-3-叔丁基-5-甲苯基)甲烷,2,2-双(4-羟基-3-甲苯基)丙烷,4,4-亚乙基双-(2-叔丁基-6-甲基苯酚),和2,2-双(3,5-二甲基-4-羟苯基)丙烷);抗坏血酸衍生物(例如1-抗坏血酸酰基棕榈酸酯,抗坏血酸酰基硬脂酸酯);不饱和醛和酮如苯偶酰和联乙酰;3-吡唑烷酮及某些二氢化茚-1,2-二酮。
除了上述组分外,包括改进影像的称为“调色剂”的添加剂将是有利的。调色剂物质的存在量可为(例如)所有含银组分重量的0.1至10%。调色剂是光热敏领域公知的物质,如US 3,080,254;3,847,612和4,123,282中给出的。
调色剂的例子包括苯邻二甲酰亚胺和N-羟基苯邻二甲酰亚胺;环酰亚胺例如琥珀酰亚胺、吡唑啉-5-酮和喹唑啉酮,3-苯基-2-吡唑啉-5-酮,1-苯基脲唑,喹唑啉和2,4-噻唑烷二酮;萘酰亚胺(例如N-羟基-1,8-萘酰亚胺);钴配合物(例如三氟乙酸六氨合高钴);硫醇,例如3-巯基-1,2,4-三唑,2,4-二巯基嘧啶,3-巯基-4,5-二苯基-1,2,4-三唑和2,5-二巯基-1,3,4-噻二唑;N-(氨甲基)芳碳二酰亚胺(例如(N,N-二甲氨基甲基)苯邻二甲酰亚胺,和(N,N-二甲氨基甲基)萘-2,3-二碳酰亚胺);及封端吡唑、异硫脲鎓盐衍生物和某些光致漂白剂(例如N,N’-六亚甲基双(1-氨基甲酰基-3,5-二甲基吡唑),1,8-(3,6-重氮基辛烷)双(三氟乙酸异硫脲鎓)和2-(三溴甲基磺酰基)苯并噻唑的混合物);和部花青染料如3-乙基-5[(3-乙基-2-苯并噻唑啉亚基)-1-甲基亚乙基]-2-硫代-2,4-噁唑烷二酮;2,3-二氮杂萘酮,6-氯-2,3-二氮杂萘酮,5,7-二甲氧基-2,3-二氮杂萘酮和2,3-二氢-2,3-二氮杂萘-1,4-二酮;2,3-二氮杂萘酮与亚磺酸衍生物(例如邻苯二甲酸、4-甲基邻苯二甲酸、4-硝基邻苯二甲酸和四氯邻苯二甲酸酐)的混合物;喹唑啉二酮、苯并噁嗪或吩噁嗪的衍生物;不仅作为色泽改性剂,而且作为现场形成卤化银的卤素离子源的铑配合物,例如六氯合铑(III)酸铵、溴化铑、硝酸铑和六氯合铑(III)酸钾;无机过氧化物和过硫酸盐(例如过硫酸铵和过氧化氢);苯并噁嗪-2,4-二酮如1,3-苯并噁嗪-2,4-二酮、8-甲基-1,3-苯并噁嗪-2,4-二酮和6-硝基-1,3-苯并噁嗪-2,4-二酮;嘧啶和不对称三嗪(例如2,4-二羟基嘧啶、2-羟基-4-氨基嘧啶),氮杂脲嘧啶和四氮杂并环戊二烯衍生物(例如3,6-二巯基-1,4-二苯基-1H,4H-2,3a,5,6a-四氮杂并环戊二烯和1,4-二(邻氯苯基)-3,6-二巯基-1H,4H-2,3a,5,6a-四氮杂并环戊二烯)。
对于用干式银体系获得彩色影像,本领域已经知道多种方法,这些方法包括:苯并三唑银、公知的品红、黄和蓝绿成色剂、氨基苯酚显影剂、碱释放剂如三氯乙酸鈲和在聚(乙烯醇缩丁醛)中的溴化银的混合物,如US4,847,188和5,064,742中公开的;预制染料释放体系,如US 4,678,739中描述的;碘溴化银、亚磺酰氨基苯酚还原剂、山萮酸银、聚(乙烯醇缩丁醛)、胺如正十八胺和2当量或4当量品红、黄或蓝绿成色剂的混合物;氧化形成染料影像的无色染料母体(例如孔雀绿、结晶紫和对蔷薇苯胺);卤化银、山萮酸银、3-甲基-1-苯基吡唑啉酮和氢氯化N,N’-二甲基对苯二胺的现场混合物;掺入酚类无色染料还原剂如2(3,5-二(叔丁基)-4-羟苯基)-4,5-二苯基咪唑和双(3,5-二(叔丁基)-4-羟苯基)苯基甲烷,掺入偶氮甲碱染料或偶氮染料还原剂;银染料漂白方法(例如,可将包括山萮酸银、山萮酸、聚(乙烯醇缩丁醛)、聚(乙烯醇缩丁醛)胶溶碘溴化银乳液、2,6-二氯-4-苯磺酰氨基苯酚、1,8-(3,6-重氮基辛烷)双(对甲苯磺酸异硫脲鎓)和偶氮染料的材料曝光并进行热处理以制得具有均匀染料分布的负银影,然后层压至包括聚丙烯酸、硫脲和对苯磺酸的酸活化剂片材上并加热得到良好清晰度的正染料影像);及与掺入的还原剂例如2,6-二氯-4-苯磺酰氨基苯酚的氧化形式反应形成染料影像的胺如氨基N-乙酰苯胺(形成黄色染料),3,3’-二甲氧基联苯胺(形成蓝色染料)或N-磺酰苯胺(形成品红染料)。通过加入胺如山萮酰胺和对茴香胺可得到中性染料影像。
在这些卤化银体系中用于成色的无色染料氧化公开于US 4,021,240;4,374,821;4,460,681和4,883,747中。
本发明的乳液可含有增塑剂和润滑剂如多醇(例如甘油和US 2,960,404中描述的各种二醇);脂肪酸或酯,如US 2,588,765和US 3,121,060中描述的;有机硅树脂,例如GB 955,061中描述的。
本发明的乳液还可含有光热敏领域已知的稳定剂和防灰雾剂。它们可以是初始稳定剂和防灰雾剂或后处理稳定剂。其中,优选的防灰雾剂是具有三卤代,特别是三溴甲基基团的有机化合物。它们常常是芳核,所述芳核具有直接与芳核连接或通过桥基团(例如磺酰基)与芳核连接的卤代基团。
本发明的光热敏材料可包括影像染料稳定剂,这些影像染料稳定剂的例子为GB1,326,889,US 3,432,330、3,698,909、3,574,627、3,572,050、3,764,337和4,042,394中描述的那些稳定剂。
本发明含乳液层的光热敏材料可在含吸光物质和滤光染料(例如US3,253,921、2,274,782、2,527,583和2,956,879中描述的)的照相材料中使用,如需要,可将这些染料进行媒染(例如US 3,282,699中描述的)。
这里所述含乳液层的光热敏材料可含有消光剂,例如淀粉、二氧化钛、氧化锌、二氧化硅、聚合物珠粒(包括US 2,992,101和US 2,701,245中描述的珠粒类型)。
根据本发明,可将乳液用于含抗静电或导电层的光热敏材料中,所述层的例子是包括可溶性盐(例如氯化物、硝酸盐等)、蒸发金属层、离子聚合物(如US 2,861,056和3,206,312中描述的)或不溶无机盐(例如US3,428,451中描述的)的层。
粘合剂可选自公知的天然或合成树脂,例如明胶、聚乙烯醇缩醛、聚氯乙烯、聚乙酸乙烯酯、乙酸纤维素、聚烯烃、聚酯、聚苯乙烯、聚丙烯腈、聚碳酸酯等。当然这些定义中也包括共聚物和三元聚合物。优选的含光热敏银的聚合物是聚乙烯醇缩丁醛和纤维素酯。
非必要地,这些聚合物可以其两种或多种的混合物使用。聚合物的用量应足以载带分散于其中的组分,换言之应在起到粘合剂作用的有效范围内。该有效范围可由本领域熟练技术人员合适地确定。原则上对于载带至少一种银盐情况,一般认为粘合剂与有机银盐的优选比例范围为15∶1至1∶2,特别优选8∶1至1∶1。
根据本发明,可将含稳定剂的光热敏乳液涂于各种基材上。典型的基材包括聚酯薄膜、底层聚酯薄膜、聚(对苯二甲酸乙二醇酯)薄膜、硝酸纤维素薄膜、纤维素酯薄膜、聚(乙烯醇缩醛)薄膜、聚碳酸酯薄膜和有关的或树脂材料以及玻璃、纸、金属等。一般使用柔韧基材,尤其是可部分乙酰化或用氧化钡和/或α-烯烃聚合物,特别是含有2至10个碳原子的α-烯烃聚合物如聚乙烯、聚丙烯、乙烯-丁烯共聚物等涂布的纸基材。这些基材可以是透明的或不透明的。
具有背面耐热层的基材也可用于光热敏成像体系中,如US 4,460,681和4,374,921中给出的。
本发明的光热敏乳液可通过各种涂布方法进行涂布包括幕式淋涂、滑动涂布、窄缝涂布或使用描述于US 2,681,294中的料斗的挤出涂布。
其它层可包括于本发明的光热敏制品中,这些层的例子如光热敏领域公知的接受流动染料影像的染料接受层、不透明层(当需要反射光照片时)、防护面漆层和底漆层。此外,在某些情况下,特别是当需要隔离出不同乳液层的成像化学药品时,需要将不同乳液层涂布到透明基材的两个表面上。
本发明将在下列实施例中详细描述,但本发明的实施方案不限制本发明。
实施例1
通过US 3,839,049中公开的方法制备卤化银-山萮酸银干性皂。卤化银共占总银的9%,而山萮银占总银的91%。卤化银为具有2%碘的0.055微米碘溴化银乳液。
通过将300g上述卤化银-山萮酸银干性皂与525g甲苯、1675g 2-丁酮和50g聚(乙烯醇缩丁醛)(B-79,Monsanto)均化制备光热敏乳液。
将均化的光热敏乳液534g和27.5g 2-丁酮在搅拌下冷却至55°F。加入0.65g在5gm MeOH中的氢溴化吡啶鎓过溴化物并搅拌2小时。加入4.75ml溴化钙溶液(1g CaBr2和10ml甲醇),接着搅拌30分钟。再加入聚(乙烯醇缩丁醛)(110g B-79)并搅拌60分钟。将温度保持在55°F下接着在搅拌下在15分钟内加入下列增量物:预混料I:甲醇中的4.32g2-(4-氯苯甲酰基)苯甲酸、染料:0.0803g 3,31二己酸-2,21-硫代三碳菁、超增感剂:0.382g甲基硫醇苯并咪唑(MMBI)、22g甲醇。16.73g 1,1-双(2-羟基-3,5-二甲苯基)-3,5,5-三甲基己烷。2.5g 2-三溴甲基磺酰喹哪啶。异氰酸酯溶液:在6g丁酮中的1.02g Desmodur N3300。
用下列组分制备活性防护面漆溶液:
81.2g 2-丁酮
9.59g甲醇
7.7g乙酸丁酸纤维素,Eastman Kodak(CAB171-15S)
0.53g 2,3-二氮杂萘(PhZ)
0.26g 4-甲基邻苯二甲酸(4-MPA)
0.17g四氯邻苯二甲酸(TCPA)
0.26g MRA-1(用作Mottle Reducing Agent的表面活性剂)
MRA-1是由N-乙基全氟辛烷磺酰基氨乙基甲基丙烯酸酯/甲基丙烯酸羟乙酯/丙烯酸按比例70/20/10制备的三元聚合物。
将所得组合物分为两个20g部分。面漆的每一20g部分刚好足以涂布35g前述银配料等分样品。
第一涂层通过将此银配料用刮刀涂布机涂于3密耳厚的聚酯薄膜上制得,基材上的涂层厚度设定为4.2密耳。将涂层在170°F下干燥3分钟并在刮刀涂布机中在3.5密耳缝隙下于1.95g/ft2的干燥银层上重新设置。第二层或面漆层同样在相同的条件下干燥。将这种顺序的涂布、干燥、涂布、干燥的方法称为单层涂布工艺。
将来自实施例1的第二等分银和面漆进行多层涂布,即将刮刀涂布机设置两个间隔6英寸的同时涂布的棒或刀。使用相同的基材。将后一个棒设置为4.2密耳并在湿银层上将前一个棒设置为5.6密耳或1.4密耳。通过将银乳液在后一个刮刀之前倒入薄膜上并将面漆在前一个棒之前倒入薄膜上对银和面漆进行多层涂布。然后将薄膜向前拉伸,这样两层同时涂布,导致单道多层方法。干燥条件不变。干燥温度为170°F,时间为3分钟。
接着将涂布物质用包括811nm二极管的激光感光仪曝光,曝光后将此薄膜条在250°F下处理15秒。将制得的影像用密度计进行评价。感光测定的结果包括Dmin,DHi(密度在Dmin+0.20以上1.4Log E处测量),速度(Spd 2=在Dmin以上密度1.05处的相对速度)和平均反差(AC-1,对Dmin以上连接0.25和2.0密度点的直线的斜率的测量)。感光度在涂布之后不久进行评价。
将选定的样品同样按类似方式曝光并在260°F下处理15秒。如此用附加的能量使样品显影以对Dmin或灰雾进行涂布方法研究。然后对处理的样品进行后显影照片稳定性测试。这种测试要将样品放入使用荧光灯、温度113°F、相对湿度20%的具有1200英尺荧光的控制看片灯箱(lightbox)中。将样品显影乳液边面向排灯放在看片灯箱中24小时。在MacbethTD 528密度计中用中性和蓝色滤光片测量Dmin。记录ΔDmin(DminαT24-DminαT0)。用设定125°F表面温度的Maxant看片灯箱进行第二次测试以测定在此高温下的ΔDmin。结果汇集于表I中,证明多层涂布工艺不但通过在显影条件下保持低的灰雾量的方式改进了显影宽容度,而且意想不到地改进了在看片灯箱中的照片稳定性。
表1
树脂 | 涂布方法 | 811nm15秒-250°F感光度 | 未处理的雾度 | 处理的雾度 | |||
Dmin | DHi | Spd2 | AC-1 | ||||
CAB171-15S | 双层 | .09 | 3.44 | 1.60 | 3.9 | 14.5 | 13.5 |
CAB171-15S | 单层 | .10 | 3.19 | 1.66 | 3.5 | 16.5 | 17.3 |
15秒-260°F | |||||||
CAB171-15S | 双层 | .11 | 3.13 | 1.71 | 3.5 | ||
CAB171-15S | 单层 | .15 | 3.15 | 1.74 | 3.1 |
在15秒/250°F下处理的样品的照片稳定性
树脂 | 涂布方法 | ΔDmin可见滤光片113°F24小时 | ΔDmin蓝色滤光片113°F24小时 | Δ Dmin可见滤光片125°F24小时 | Δ Dmin蓝色滤光片125°F24小时 |
CAB171-15S | 双 层 | .16 | .24 | .37 | .37 |
CAB171-15S | 单 层 | .57 | .54 | .82 | .77 |
实施例II
当按多层或双层方式涂布时,其它乙酸纤维素酯也显示改进的照片稳定性和显影宽容度。银层与实施例I相同。调节树脂的百分数以调节粘度。用各种树脂制备面漆。
IIA 面漆配方
MEK | 81.22 |
MeOH | 9.59 |
乙酸丙酸纤维素-482-20 | 6.0 |
4 MPA | 0.259 |
TCPA | 0.173 |
PhZ | 0.527 |
MRA-1(16%固体) | 0.256 |
IIB 面漆配方
MEK | 81.22 |
MeOH | 9.59 |
乙酸丙酸纤维素-482-0.5 | 20.0 |
4 MPA | 0.259 |
TCPA | 0.173 |
PhZ | 0.527 |
MRA-1(16%固体) | 0.256 |
IIC 面漆配方
MEK | 81.22 |
MeOH | 9.59 |
乙酸丙酸纤维素-504-.2 | 20.0 |
4 MPA | 0.259 |
TCPA | 0.173 |
PhZ | 0.527 |
MRA-1(16%固体) | 0.256 |
IID 面漆配方
MEK | 81.22 |
MeOH | 9.59 |
乙酸纤维素-394-60 | 6.0 |
4 MPA | 0.259 |
TCPA | 0.173 |
PhZ | 0.527 |
MRA-1(16%固体) | 0.256 |
IIE 面漆配方
MEK | 81.22 |
MeOH | 9.59 |
乙酸纤维素-398-6 | 20.0 |
4 MPA | 0.259 |
TCPA | 0.173 |
PhZ | 0.527 |
MRA-1(16%固体) | 0.256 |
IIF 面漆配方
MEK | 81.22 |
MeOH | 9.59 |
乙酸丁酸纤维素-381-20 | 8.0 |
4 MPA | 0.259 |
TCPA | 0.173 |
PhZ | 0.527 |
MRA-1(16%固体) | 0.256 |
IIG 面漆配方
MEK | 81.22 |
MeOH | 9.59 |
乙酸丁酸纤维素-171-155 | 8.0 |
Gelva V-7(Monsanto) | 8.0 |
4 MPA | 0.259 |
TCPA | 0.173 |
PhZ | 0.527 |
MRA-1(16%固体) | 0.256 |
各实施例按单层和多层方式与实施例I完全相同地涂布。按与实施例1相同的方式进行所有测试。表II中为感光度和照片稳定性数据。
表II
实施例 | 树脂 | 涂布方法 | 811nm15秒-250°F感光度 | |||
Dmin | DHi | Spd2 | AC-1 | |||
IIAIIA | CAP482-20CAP482-20 | 双 层单 层 | .10.11 | 3.963.23 | 1.491.61 | 3.73.7 |
IIBIIB | CAP482-.5CAP482-.5 | 双 层单 层 | .10.09 | 3.633.26 | 1.541.46 | 3.12.9 |
IICIIC | CAP504-.2CAP504-.2 | 双 层单 层 | .10.10 | 3.613.41 | 1.451.52 | 2.83.2 |
IIDIID | CA-396-60CA-396-60 | 双 层单 层 | .11.13 | 3.243.41 | 1.651.77 | 3.13.6 |
IIEIIE | CA-398-6CA-398-6 | 双 层单 层 | .12.16 | 3.384.05 | 1.731.80 | 3.93.4 |
IIFIIF | CAB381-20CAB381-20 | 双 层单 层 | .09.08 | 3.423.46 | 1.731.72 | 3.63.9 |
IIGIIG | CAB171+Gelva V7CAB171+Gelva V7 | 双 层单 层 | .09.10 | 3.403.44 | 1.781.88 | 3.73.7 |
实施例 | 树脂 | 涂布方法 | 15秒-260°F感光度 | |||
Dmin | DHi | Spd 2 | AC-1 | |||
IIAIIA | CAP482-20CAP482-20 | 双 层单 层 | .13.19 | 3.523.14 | 1.571.68 | 3.83.2 |
IIBIIB | CAP482-.5CAP482-.5 | 双 层单 层 | .12.12 | 3.463.21 | 1.531.59 | 2.72.9 |
IICIIC | CAP504-.2CAP504-.2 | 双 层单 层 | .17.13 | 3.483.26 | 1.611.52 | 3.42.6 |
照片稳定性
15秒-250°F处理
实施例 | 树脂 | 涂布方法 | ΔDmin可见滤光片24小时 | ΔDmin蓝色滤光片24小时 | ΔDmin可见滤光片24小时 | ΔDmin蓝色滤光片24小时 |
113°F | 113°F | 125°F | 125°F | |||
IIAIIA | CAP482-20CAP482-20 | 双层单层 | .13.28 | .28.34 | .26.59 | .29.56 |
IIBIIB | CAP482-.5CAP482-.5 | 双层单层 | .05.08 | .12.16 | .17.22 | .21.23 |
IICIIC | CAP504-.2CAP504-.2 | 双层单层 | .O1.09 | .06.15 | .12.20 | .14.23 |
IIDIID | CA-396-60CA-396-60 | 双层单层 | .20.39 | .31.49 | .11.34 | .09.34 |
IIEIIE | CA-398-6CA-398-6 | 双层单层 | .11.28 | .23.49 | .09.25 | .06.34 |
IIF | CAB381-20 | 双层 | .22 | .37 | .22 | .39 |
IIF | CAB381-20 | 单层 | .40 | .53 | .55 | .74 |
IIGIIG | CAB171+Gelva V7CAB171+Gelva V7 | 双层单层 | .40.76 | .70.87 | .861.14 | .961.26 |
树脂 | 涂布方法 | ΔDmin可见滤光片24小时看片灯箱113°F | ΔDmin蓝色滤光片24小时看片灯箱113°F |
CAP482-20CAP482-20 | 双层单层 | .23.45 | .40.59 |
CAP482-.5CAP482-.5 | 双层单层 | .11.20 | .21.28 |
CAP504-.2CAP504-.2 | 双层单层 | .06.14 | .14.22 |
实施例III
将另一些化合物用于检验本发明的范围。银配料与实施例I相同。面漆由树脂和调色剂制备。对每一由树脂和溶剂组成的面漆制备预混料。调节预混料的固体百分数以使粘度在10-200cp范围内。列出预混料配方和粘度。涂布前一天,将0.55g PHZ,0.27g 4-MPA和0.18g TCPA加入100g树脂预混料中并混合至溶解。
将实施例III的这些样品用多层涂布工艺涂布,用811nm激光曝光进行感光度测试并在与实施例I和II中相同的加工机械上在250°F下处理15秒。照片稳定性测试在与实施例I和II所述相同的看片灯箱中进行。下列实施例中所述光稳定性使用标记:24hr/V=在密度计上使用可见滤光片在看片灯箱中24小时。给出了ΔDmin。24hr/B=在用蓝色滤光片测量的看片灯箱中24小时。初始感光测量值Dmin、Dmax、Spd Pt=SPD2、ContC=AC-1。SPD2和AC-1采用上述值。
树脂 | 树脂预混料组合物 | 初始值 | 光稳定性 | ||
硝化纤维素RS1/2sec.(Hercules) | 5%树脂84%MEK10%EtOH+2%MRA-1 | DminDmaxSpd Pt | 0.201.00*** | 24小时/V24小时/B | 0.80n.m. |
硝化纤维素FM200(Daicel) | 5%树脂84%MEK10%EtOH | DminDmaxSpd Pt | 0.181.440.75 | 24小时/V24小时/B | 0.96n.m. |
硝化纤维素FM200(Daicel) | 5%树脂84%MEK10%EtOH+2%MRA-1 | DminDmaxSpd Pt | 0.161.820.95 | 24小时/V24小时/B | 0.67n.m. |
VYNS-390%PVC10%PVAc(Union Carbide) | 12%树脂78%MEK10%EtOH | DminDmaxSpd PtCont C | 0.263.832.034.14 | 24小时/V24小时/B | 1.952.03 |
VYHD86%PVC14%PVAc(Union Carbide) | 20%树脂70%MEK10%EtOH | DminDmaxSpd PtCont C | 0.243.462.063.90 | 24小时/V24小时/B | 1.371.52 |
VMCH86%PVC13%PVAc1%马来酸(Union Carbide) | 20%树脂70%MEK10%EtOH | DminDmaxSpd PtCont C | 0.213.352.403.85 | 24小时/V24小时/B | 1.872.06 |
VMCA | 25%树脂 | Dmin | 0.12 | 24小时/V | 1.36 |
81%PVC17%PVAc2%马来酸(Union Carbide) | 65%MEK10%EtOH | DmaxSpd PtCont C | 3.241.712.65 | 24小时/B | 1.63 |
VAGH90%PVC4%PVAc6%PVAl(Union Carbide) | 15%树脂75%MEK10%EtOH | DminDmaxSpd PtCont C | 0.133.331.803.24 | 24小时/V24小时/B | 1.031.20 |
树脂 | 树脂预混料组合物 | 初始值 | 光稳定性 | ||
VROH81%PVC4%PVAc15%HO-R-丙烯酸酯(Union Carbide) | 25%树脂65%MEK10%EtOH | DminDmaxSpd PtCont C | 0.143.461.843.49 | 24小时/V24小时/B | 1.401.54 |
VYES67%PVC11%PVAc22%HO-R-丙烯酸酯(Union Carbide) | 25%树脂65%MEK10%EtOH | DminDmaxSpd PtCont C | 0.163.061.591.95 | 24小时/V24小时/B | 1.081.32 |
硝化纤维素RS1/2秒作为接受的(Hercules) | 12%树脂78%MEK10%EtOH | DminDmaxSpd PtCont C | 0.751.22****** | 24小时/V24小时/B | 0.771.22 |
Versamid 940聚酰胺 | 15%树脂28%MEK | DminDmax | 0.143.22 | 24小时/V24小时/B | 0.520.79 |
总Mill | 28%甲苯28%EtOH | Spd PtCont C | 1.813.61 | ||
Versalon 1164聚酰胺总Mill | 15%树脂42%甲苯42%EtOH | DminDmaxSpd PtCont C | 0.112.841.682.18 | 24小时/V24小时/B | 0.490.84 |
Emerez 1532聚酰胺Emery | 15%树脂42%甲苯42%EtOH | DminDmaxSpd PtCont C | 0.133.051.853.09 | 24小时/V24小时/B | 0.590.86 |
PKHH苯氧基树脂Union Carbide | 15%树脂38%MEK38%甲苯10%EtOH | DminDmaxSpd PtCont C | 0.212.271.79*** | 24小时/V24小时/B | 0.360.60 |
Styron 685D聚苯乙烯Dow Chemical | 15%树脂85%MEK | DminDmaxSpd PtCont C | 0.223.492.032.74 | 24小时/V24小时/B | 1.301.71 |
聚(4-叔丁基苯乙烯)Aldrich Chemical | 15%树脂85%MEK | DminDmaxSpd PtCont C | 0.183.952.103.30 | 24小时/V24小时/B | 0.640.79 |
树脂 | 树脂预混料组合物 | 初始值 | 光稳定性 | ||
Tyril 880苯乙烯-丙烯氰Dow Chemical | 15%树脂85%MEK | DminDmaxSpd PtCont C | 0.302.802.051.48 | 24小时/V24小时/B | 2.002.29 |
乙基纤维素N-20048%羟基Hercules | 4%树脂43%MEK43%甲苯10%EtOH | DminDmaxSpd PtCont C | 0.463.942.043.26 | 24小时/V24小时/B | 0.350.52 |
Scripset 520苯乙烯-马来酸酐共聚物,酸酐形式(Monsanto) | 15%树脂75%MEK10%EtOH | DminDmaxSpd PtCont C | 0.080.22****** | 24小时/V24小时/B | 1.662.45 |
Scripset 540苯乙烯-马来酸酐共聚物,酯/酸形式(Monsanto) | 18%树脂74%MEK8%EtOH | DminDmaxSpd PtCont C | 0.103.111.622.83 | 24小时/V24小时/B | 1.221.58 |
Estane 5706聚氨酯(Goodrich) | 15%树脂75%MEK10%EtOH | DminDmaxSpd PtCont C | 0.242.841.992.86 | 24小时/V24小时/B | 0.370.58 |
Estane 5715聚氨酯(Goodrich) | 15%树脂75%MEK10%EtOH | DminDmaxSpd PtCont C | 0.182.681.992.34 | 24小时/V24小时/B | 0.150.27 |
VitelPE 200(vitel 2200)聚酯(Goodyear) | 20%树脂80%MEK | DminDmaxSpd PtCont C | 0.191.180.49*** | 24小时/V24小时/B | 0.190.33 |
Parlon S-10氯化橡胶Hercules | 15%树脂75%MEK10%EtOH | DminDmaxSpd PtCont C | 0.143.251.603.05 | 24小时/V24小时/B | 0.490.74 |
实施例III的树脂说明当考虑感光度和照片稳定性时,选择面漆树脂是困难的。同时,在双层模式中,银与面漆溶液的相容性很重要。当考虑多层结构时,纤维素酯类在所有方面清楚地说明了本发明的最佳方式。
Claims (19)
1.一种生产光热敏材料的方法,包括步骤:a)提供一基材,b)在上述基材上涂布第一层,所述第一层包括有机聚合物粘合剂、卤化银、可还原银盐或银配合物和有机溶剂,c)所述第一层中70%的溶剂从所述第一层除去前,将包括溶剂和第二种聚合物粘合剂的第二层涂于所述第一层上,所述第二种聚合物粘合剂包括至少一种纤维素酯,所述第一层和所述第二层的至少一层含有银离子的还原剂。
2.权利要求1的方法,其中所述纤维素酯选择乙酸纤维素、乙酸丁酸纤维素和乙酸丙酸纤维素。
3.权利要求1的方法,其中所述纤维素酯包括至少50%(重量)的第二种聚合物粘合剂。
4.权利要求2的方法,其中所述纤维素酯包括至少50%(重量)的第二种聚合物粘合剂。
5.权利要求1的方法,其中所述纤维素酯包括至少75%(重量)的第二种聚合物粘合剂。
6.权利要求2的方法,其中所述纤维素酯包括至少75%(重量)的所述第二种粘合剂。
7.权利要求1的方法,其中所述纤维素酯包括至少90%(重量)的所述第二种粘合剂。
8.权利要求2的方法,其中所述纤维素酯包括至少90%(重量)的所述第二种粘合剂。
9.权利要求1的方法,其中所述第一层中50%的溶剂除去之前将所述第二层涂于所述第一层上。
10.权利要求2的方法,其中所述第一层中50%(重量)的溶剂除去之前将所述第二层涂于所述第一层上。
11.权利要求4的方法,其中所述第一层中50%的溶剂除去之前将所述第二层涂于所述第一层上。
12.权利要求6的方法,其中所述第一层中50%的溶剂除去之前将所述第二层涂于所述第一层上。
13.权利要求8的方法,其中所述第一层中50%(重量)的溶剂除去之前将所述第二层涂于所述第一层上。
14.权利要求1的方法,其中所述第一层中30%的溶剂除去之前将所述第二层涂于所述第一层上。
15.权利要求8的方法,其中所述第一层中30%(重量)的溶剂除去之前将所述第二层涂于所述第一层上。
16.权利要求1的方法,其中所述基材为透明聚合物薄膜。
17.权利要求2的方法,其中所述基材为透明聚合物薄膜。
18.权利要求8的方法,其中所述基材为透明聚合物薄膜。
19.权利要求15的方法,其中所述基材为透明聚合物薄膜。
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US08/233,695 US5405740A (en) | 1994-04-26 | 1994-04-26 | Process for manufacturing stable photothermographic elements |
US08/233,695 | 1994-04-26 |
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CN1147864A true CN1147864A (zh) | 1997-04-16 |
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US (1) | US5405740A (zh) |
EP (1) | EP0759187B1 (zh) |
JP (1) | JP3535169B2 (zh) |
CN (1) | CN1147864A (zh) |
AU (1) | AU1984095A (zh) |
BR (1) | BR9507528A (zh) |
CA (1) | CA2187456A1 (zh) |
DE (1) | DE69505520T2 (zh) |
WO (1) | WO1995029429A1 (zh) |
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CN107077061A (zh) * | 2014-11-04 | 2017-08-18 | 卡尔斯特里姆保健公司 | 成像材料、制剂和组合物 |
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US6685367B1 (en) | 2000-06-13 | 2004-02-03 | Eastman Kodak Company | Image processing apparatus and method for thermally processed films |
JP2002006445A (ja) * | 2000-06-27 | 2002-01-09 | Konica Corp | 熱現像感光材料 |
US7157736B2 (en) | 2003-12-23 | 2007-01-02 | Eastman Kodak Company | Multi-layer compensation film including stretchable barrier layers |
US7468241B1 (en) | 2007-09-21 | 2008-12-23 | Carestream Health, Inc. | Processing latitude stabilizers for photothermographic materials |
US7524621B2 (en) * | 2007-09-21 | 2009-04-28 | Carestream Health, Inc. | Method of preparing silver carboxylate soaps |
US7622247B2 (en) * | 2008-01-14 | 2009-11-24 | Carestream Health, Inc. | Protective overcoats for thermally developable materials |
WO2017123444A1 (en) | 2016-01-15 | 2017-07-20 | Carestream Health, Inc. | Method of preparing silver carboxylate soaps |
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JPS5411694B2 (zh) * | 1972-05-09 | 1979-05-17 | ||
US4055432A (en) * | 1973-01-18 | 1977-10-25 | Fuji Photo Film Co., Ltd. | Thermodevelopable photographic material |
JPS5333615A (en) * | 1976-09-09 | 1978-03-29 | Fuji Photo Film Co Ltd | Thermal development sensitive materials |
JPS592895B2 (ja) * | 1980-07-04 | 1984-01-21 | 旭化成株式会社 | 熱現像型乾式銀塩シ−トの製造方法 |
US4395484A (en) * | 1982-06-25 | 1983-07-26 | Minnesota Mining And Manufacturing Company | Roomlight-stable ultraviolet-response photothermographic imaging material |
IT1228313B (it) * | 1989-02-09 | 1991-06-11 | Minnesota Mining & Mfg | Procedimento per la stesa simultanea di piu' strati di composizioni acquose colloidali idrofile su un supporto idrofobo e materiale fotografico a piu' strati |
US5028523A (en) * | 1990-06-04 | 1991-07-02 | Minnesota Mining And Manufacturing Company | Photothermographic elements |
US5196301A (en) * | 1990-07-30 | 1993-03-23 | Minnesota Mining And Manufacturing Company | Post-processing stabilization of photothermographic emulsions |
US5028518A (en) * | 1990-09-24 | 1991-07-02 | Minnesota Mining And Manufacturing Company | Radiographic thermographic imaging film |
-
1994
- 1994-04-26 US US08/233,695 patent/US5405740A/en not_active Expired - Lifetime
-
1995
- 1995-03-02 JP JP52762795A patent/JP3535169B2/ja not_active Expired - Fee Related
- 1995-03-02 WO PCT/US1995/002889 patent/WO1995029429A1/en active IP Right Grant
- 1995-03-02 DE DE69505520T patent/DE69505520T2/de not_active Expired - Fee Related
- 1995-03-02 AU AU19840/95A patent/AU1984095A/en not_active Abandoned
- 1995-03-02 BR BR9507528A patent/BR9507528A/pt not_active Application Discontinuation
- 1995-03-02 CN CN95192768A patent/CN1147864A/zh active Pending
- 1995-03-02 EP EP95912797A patent/EP0759187B1/en not_active Expired - Lifetime
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CN107077061A (zh) * | 2014-11-04 | 2017-08-18 | 卡尔斯特里姆保健公司 | 成像材料、制剂和组合物 |
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EP0759187A1 (en) | 1997-02-26 |
JP3535169B2 (ja) | 2004-06-07 |
JPH09512350A (ja) | 1997-12-09 |
CA2187456A1 (en) | 1995-11-02 |
US5405740A (en) | 1995-04-11 |
AU1984095A (en) | 1995-11-16 |
DE69505520T2 (de) | 1999-04-08 |
WO1995029429A1 (en) | 1995-11-02 |
EP0759187B1 (en) | 1998-10-21 |
DE69505520D1 (de) | 1998-11-26 |
BR9507528A (pt) | 1997-09-02 |
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