CN1701135A - 无电镀用催化剂前体组合物和用该组合物制备透明的电磁干扰屏蔽材料的方法 - Google Patents
无电镀用催化剂前体组合物和用该组合物制备透明的电磁干扰屏蔽材料的方法 Download PDFInfo
- Publication number
- CN1701135A CN1701135A CNA2004800009320A CN200480000932A CN1701135A CN 1701135 A CN1701135 A CN 1701135A CN A2004800009320 A CNA2004800009320 A CN A2004800009320A CN 200480000932 A CN200480000932 A CN 200480000932A CN 1701135 A CN1701135 A CN 1701135A
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- Prior art keywords
- catalyst precursor
- precursor composition
- electroless plating
- acrylate
- base material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000012018 catalyst precursor Substances 0.000 title claims abstract description 94
- 239000000203 mixture Substances 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 78
- 238000007772 electroless plating Methods 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 21
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 12
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 8
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- 238000000034 method Methods 0.000 claims description 34
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- JHPBZFOKBAGZBL-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylprop-2-enoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)=C JHPBZFOKBAGZBL-UHFFFAOYSA-N 0.000 claims description 5
- 125000000524 functional group Chemical group 0.000 claims description 5
- HCLJOFJIQIJXHS-UHFFFAOYSA-N 2-[2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOCCOC(=O)C=C HCLJOFJIQIJXHS-UHFFFAOYSA-N 0.000 claims description 4
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 4
- -1 phenyl glyoxylic acid ester Chemical class 0.000 claims description 4
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 3
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 3
- VFZKVQVQOMDJEG-UHFFFAOYSA-N 2-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(=O)C=C VFZKVQVQOMDJEG-UHFFFAOYSA-N 0.000 claims description 3
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 3
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 3
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- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 claims description 2
- PUGOMSLRUSTQGV-UHFFFAOYSA-N 2,3-di(prop-2-enoyloxy)propyl prop-2-enoate Chemical compound C=CC(=O)OCC(OC(=O)C=C)COC(=O)C=C PUGOMSLRUSTQGV-UHFFFAOYSA-N 0.000 claims description 2
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 claims description 2
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 2
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- MHCLJIVVJQQNKQ-UHFFFAOYSA-N ethyl carbamate;2-methylprop-2-enoic acid Chemical compound CCOC(N)=O.CC(=C)C(O)=O MHCLJIVVJQQNKQ-UHFFFAOYSA-N 0.000 claims description 2
- JZMPIUODFXBXSC-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.CCOC(N)=O JZMPIUODFXBXSC-UHFFFAOYSA-N 0.000 claims description 2
- WGOQVOGFDLVJAW-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCOC(N)=O WGOQVOGFDLVJAW-UHFFFAOYSA-N 0.000 claims description 2
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- PBDBXAQKXCXZCJ-UHFFFAOYSA-L palladium(2+);2,2,2-trifluoroacetate Chemical compound [Pd+2].[O-]C(=O)C(F)(F)F.[O-]C(=O)C(F)(F)F PBDBXAQKXCXZCJ-UHFFFAOYSA-L 0.000 claims description 2
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 2
- 125000002769 thiazolinyl group Chemical group 0.000 claims 1
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0094—Shielding materials being light-transmitting, e.g. transparent, translucent
- H05K9/0096—Shielding materials being light-transmitting, e.g. transparent, translucent for television displays, e.g. plasma display panel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
- C08F290/06—Polymers provided for in subclass C08G
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
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- C23C18/2066—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
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Abstract
本发明涉及无电镀用催化剂前体组合物,更具体来说,本发明提供了包含(a)活性低聚体;(b)活性单体;(c)光引发剂;(d)无电镀用催化剂前体;和(e)溶剂的催化剂前体组合物以及用该组合物制备EMI屏蔽材料的方法。本发明通过使用含有对基材具有良好粘附性的UV固化树脂的催化剂前体组合物提供了制备EMI屏蔽材料的简易方法,从而无需在无电镀前用接受层对基材进行预处理。
Description
发明背景
(a)发明领域
本发明涉及无电镀用催化剂前体组合物和用该组合物制备透明的电磁干扰屏蔽材料(下文称之为“EMI”屏蔽材料)的方法。更具体来说,本发明涉及包含对基材具有良好粘附性的UV(紫外)固化树脂的催化剂前体组合物,从而在制备EMI屏蔽材料时无需额外预处理。这样,本发明就提供了易于制备EMI屏蔽材料的催化剂前体组合物和用该组合物制备EMI屏蔽材料的方法。
(b)相关技术描述
等离子体显示面板(下文称之为“PDP”)具有为面板前部玻璃的整个表面提供信号和电源的电极,因而在运行时与其它显示设备相比产生更多的电磁辐射。
因此,PDP需要装备过滤器以屏蔽PDP运行时产生的有害电磁波。该过滤器由层积在玻璃上的若干膜组成,例如防反射膜(下文称之为“AR膜”)、近红外线屏蔽膜(下文称之为“NIR膜”)、Neon-cut膜、EMI屏蔽膜等。
优选具有良好透明度的EMI屏蔽膜以确保可见光的透过。可通过将诸如铜、银和镍的导电材料粘附在格栅图案中的透明基材上制备EMI屏蔽膜。可将导电金属粘附在基底上的方法分为包含溅射法和真空沉积法的干法和包含无电镀等的湿法。由于干法需要昂贵的制造装置,因此便宜的湿法是最广泛应用的。
在无电镀法中,通过使镀液与催化剂接触引发镀反应,于是使金属仅仅镀在催化剂上。将催化剂印刷在格栅图案中的透明基底上,然后进行无电镀从而得到透明的EMI屏蔽材料。
通常,由于在水中制备无电镀用催化剂,因此催化剂不易于粘附在光滑且疏水的基材上。所以必须通过蚀刻等对基材进行预处理以提高其表面粗糙度和亲水性。然而该预处理使基材表面的均匀性和可见度降低。
日本公开No.2000-311527号公报公开了一种通过在基材上印刷含无电镀用催化剂的树脂组合物以形成图案,然后通过无电镀法在图案上形成导电金属层来制备透明导电膜的方法。然而,其化学催化剂必须通过复杂的工艺获得,而且必须在无电镀发生前在基材表面上形成树脂组合物的接受层。
日本公开No.2001-177292号公报公开了一种通过在基材上涂覆含无电镀用催化剂的疏水性透明树脂,然后进行无电镀制备透明导电膜的方法。通过在树脂层上涂覆耐镀性化合物之后进行无电镀或者首先通过在无电镀表面上涂覆光致抗蚀剂化合物,然后通过光掩模辐照光,再进行蚀刻得到透明金属图案。在多数情况下,使用疏水性树脂以粘附在疏水性基材上,但该方法存在的问题是由于低的附着性不能得到具有高耐久性的透明导电膜。此外,使金属图案成形的工艺复杂,需要诸如光掩模的昂贵设备,而且使用无水镀液,因此提高了生产成本。
日本公开No.2002-185184号公报公开了一种通过在格栅图案中的基材上印刷含无电镀催化剂的树脂组合物,然后进行无电镀来制备透明EMI屏蔽材料的方法。在这种情况下,透明图案是通过印刷方法来制备的,因此不需要诸如光掩蔽机械的昂贵设备,但在镀膜前必须用接受层或固定层对基材进行预处理以使树脂组合物易于粘附在基材上。具体来说,需要约3天时间去固化用两组分溶液涂覆的固定层,因此难以实用。
发明概述
本发明的动机在于解决上述问题和其它问题。本发明的目的之一在于提供一种包含对基材具有良好粘附性的UV(紫外)固化树脂的无电镀用催化剂前体组合物,以易于制备EMI屏蔽材料而无需基材的额外预处理。
本发明的另一目的在于提供一种使用该催化剂前体组合物制备EMI屏蔽材料的方法。
本发明的另一目的在于提供一种根据本发明方法制备的EMI屏蔽材料。
本发明的另一目的在于提供一种含EMI屏蔽材料的PDP过滤器。
本发明的另一目的在于提供一种含PDP过滤器的PDP。
附图简要说明
本发明通过参照附图和以下对实施方案的详细描述将会变得更加清楚,其中:
图1是根据本发明实施方案的PDP的平面图;和
图2是图1所示PDP的PDP过滤器的放大剖面图。
优选实施方案的详细描述
本发明涉及一种包含(a)活性低聚体;(b)活性单体;(c)光引发剂;(d)无电镀用催化剂前体;和(e)溶剂的催化剂前体组合物。
本发明涉及一种通过在格栅图案中的透明基材上印刷催化剂前体组合物,用UV(紫外)辐照固化该前体组合物,和在固化表面上进行无电镀来制备透明EMI屏蔽材料的方法。
本发明涉及一种根据本发明方法制备的透明EMI屏蔽材料。
下面更详细描述本发明。
本发明人进行研究以开发对基材具有高的粘附性而无需进行基材预处理的催化剂前体组合物,从而提供一种EMI屏蔽材料的简易生产方法;并降低了生产成本。
在研究过程中,本发明人通过将包含VIIIB族或IB族金属的有机化合物或无机化合物作为催化剂前体溶解在溶剂中,然后在基材上印刷具有优良粘附性的UV固化树脂,发现了一种无电镀用催化剂前体组合物。此外,本发明人还发现了用该催化剂前体组合物制备的透明EMI屏蔽材料,其中由于对基材具有高粘附性的UV固化树脂的加入从而避免了对基材进行预处理的需要。
无电镀用催化剂前体组合物包括(a)活性低聚体;(b)活性单体;(c)光引发剂;(d)无电镀用催化剂前体;和(e)溶剂。
通过在格栅图案中的基材上印刷该催化剂前体组合物、干燥、用UV辐照固化,然后进行无电镀,制备透明导电膜。在该方法中,通过由UV辐照引发的反应将溶解在组合物中的催化剂前体转变为适于无电镀的催化剂。
组合物中的催化剂前体是以离子形式存在的,因此也称为“催化剂前体离子(Mn+)”。催化剂的实例包括Co,Rh,Ir,Ni,Pd,Pt,Cu,Ag,和Au。通过用UV辐照催化剂前体将光引发剂转变为自由基,然后将催化剂前体还原为适于无电镀的金属元素(M0)。
此外,本发明的优点在于该催化剂前体组合物含有对基材具有良好粘附性的UV固化树脂,从而避免了在无电镀前用接受层对基材进行预处理的需要。
下面将描述催化剂前体组合物中的各个组分。
在本发明的催化剂前体组合物中,(a)活性低聚体决定了催化剂前体组合物的基本物化特征,例如反应性、粘度、表面光泽度、粘附性和对化学品和污染物的抗性。
在本发明的催化剂前体组合物中,活性低聚体优选使用具有丙烯酸酯和甲基丙烯酸酯作为官能团的材料。例如,活性低聚体包括聚氨酯丙烯酸酯、聚氨酯二丙烯酸酯、聚氨酯三丙烯酸酯、聚氨酯甲基丙烯酸酯、环氧丙烯酸酯、环氧二丙烯酸酯、聚酯丙烯酸酯、丙烯酸丙烯酸酯、或其混合物,但并不限于此。
活性低聚体优选具有500-5000的分子量。活性低聚体的量取决于印刷方法。对于催化剂前体组合物的总重量而言,活性低聚体含量为5-50重量%,优选20-45重量%。
本发明的催化剂前体组合物中含有(b)活性单体从而通过降低活性低聚体的粘度使其易于使用。此外,通过参与交联反应,活性单体成为固化材料的一部分。
活性单体使用具有丙烯酸酯和甲基丙烯酸酯作为官能团的材料,例如丙烯酸异冰片酯、丙烯酸辛酯,丙烯酸癸酯、1,6-己二醇二丙烯酸酯、二丙二醇二丙烯酸酯、三丙二醇二丙烯酸酯、三乙二醇二丙烯酸酯、四乙二醇二丙烯酸酯、乙氧基化新戊二醇二丙烯酸酯、丙氧基化新戊二醇二丙烯酸酯、丙烯酸2-苯氧乙酯、丙氧基化甘油三丙烯酸酯、乙氧基化三羟甲基丙烷三丙烯酸酯、季戊四醇三丙烯酸酯、和其混合物。
活性单体优选具有100-600的分子量。活性单体的量取决于印刷方法。对于催化剂前体组合物的总量而言,活性单体的含量为10-55重量%,更优选25-45重量%。
在本发明中,使用具有丙烯酸酯和甲基丙烯酸酯作为官能团的活性低聚体和活性单体可加速从催化剂前体离子(Mn+)到催化剂前体元素(M0)的还原反应(R.L Jackson,J.Electrochem.Soc.1990,137(1),95.;Y.Nakao,J.Colloid Interface Sci.1995,171,386)。
此外,本发明的催化剂前体组合物含有(c)光引发剂,该光引发剂通过UV辐照离解成自由基并引发UV固化树脂的交联反应。
光引发剂除了该基本功能外,本发明中的光引发剂还能将催化剂前体组合物中的催化剂前体离子(Mn+)还原为用作无电镀反应催化剂的催化剂前体元素(M0)。
例如,光引发剂为α-羟基酮、苯基乙醛酸酯、苯偶酰二甲缩酮、α-氨基酮、单酰基膦、二酰基膦、和其混合物。
将催化剂前体离子(Mn+)还原为元素(M0)的反应速率取决于所用光引发剂的类型。通常,α-羟基酮具有最高的还原速率,尽管该速率会随着活性低聚体和活性单体类型的不同而稍有差别。
对于除溶剂外的催化剂前体组合物而言,催化剂前体组合物中光引发剂的量为1.5-6.0重量%,更优选2.5-4.0重量%。
此外,(d)无电镀用催化剂前体是VIIIB族元素或IB族元素的有机化合物或无机化合物。
鉴于催化剂前体在溶剂中的溶解度,优选使用有机化合物,最优选使用包含Pd2+的含羰基或烯基有机化合物的盐,例如乙酸钯,三氟乙酸钯、草酸钯、乙酰丙酮钯等。
在一定的范围内,无电镀的反应速率与催化剂的量成正比。VIIIB族金属或IB族金属的有机或无机化合物非常昂贵,因此最优化该化合物的量是很重要的。具体来说,尽管该化合物的量会随无电镀类型的不同而稍有差别,但对除溶剂外的催化剂前体组合物而言,催化剂前体的含量优选为0.2-6.0重量%,更优选0.4-3.0重量%。
此外,对于催化剂前体组合物中的溶剂没有特别的限制,可以是工业领域通常使用的溶剂。溶剂优选是在交联反应中不沉淀并在室温和1大气压下以液相存在的有机化合物。对于溶剂的粘度和表面张力没有特别的限制。然而,溶剂需要对催化剂前体和光引发剂具有良好的溶解度,应与活性低聚物和活性单体混合均匀,而且在1大气压下沸点为60-85℃。虽然可以使用沸点低于60℃的溶剂,但其存在安全问题。
满足要求的溶剂实例包括氯仿、乙腈、甲乙酮、乙酸乙酯、和其混合物。
对于催化剂前体组合物的总重量而言,溶剂的量为20-45重量%,优选30-40重量%。
用上述催化剂前体组合物制备EMI屏蔽材料的方法可概括有以下步骤:在光栅图案中印刷催化剂前体组合物、加热、用UV辐照、然后无电镀。下面作进一步详细描述。
通过将包括VIIIB族或IB族金属的有机或无机化合物与光引发剂溶解在溶剂中得到溶液,然后在搅拌同时将所得溶液与活性单体和活性低聚物混合以得到催化剂前体组合物。优选混合催化剂前体组合物的各组分的容器为由耐热玻璃如Pyrex玻璃(耐火玻璃)制成的三口圆底烧瓶。由于金属搅拌器会被催化剂前体腐蚀,因此优选特氟隆(聚四氟乙烯)搅拌器。
在制备完催化剂前体组合物之后,用适当方法将该组合物印刷在基材上。印刷方法没有特别限制,但优选喷墨印刷、凹版印刷、柔性版印刷、和丝网印刷等。基于催化剂前体组合物的粘度,可以选择最佳印刷方法。在25℃时,已知具有1-100cps粘度的印刷油墨适用于喷墨印刷,30-300cpa粘度的印刷油墨适用于凹版印刷,50-500cps粘度的印刷油墨适用于柔性版印刷,而1000-5000cps粘度的印刷油墨适用于丝网印刷。
基材可以是对可见光具有足够透光度且表面易于用催化剂前体组合物印刷的材料,但是并没有特别的限制。基材的形状可以是平面或具有曲面。基材的厚度也没有特别的限制。基材的实例包括玻璃、聚酯、聚苯乙烯、聚甲基丙烯酸甲酯、聚碳酸酯、聚丙烯和聚砜。由于在印刷催化剂前体组合物之后需对基材进行加热并无电镀,因此基材应具有良好的耐热性和低吸湿性。故优选聚酯。
在印刷的同时或印刷完之后立即通过加热基材蒸发掉催化剂前体组合物中的溶剂。在蒸发过程中,溶解在溶剂中的催化剂前体离子(Mn+)大量转移到组合物的表层。
在加热催化剂前体组合物时或加热完后用UV辐照基材。UV辐照使光引发剂离解成自由基,该自由基可引发活性单体或活性低聚物的交联反应。在交联反应的同时,催化剂前体离子(Mn+)被还原为催化剂金属(M0),该催化剂金属(M0)可用作无电镀的催化剂。尽管UV辐照时间长短取决于催化剂前体组合物的组成,但此处UV辐照1-3分钟。在这种情况下,UV的能量密度为1500-4500J/cm2。
当将催化剂前体离子(Mn+)还原成元素态(M0)时,VIIIB族或IB族金属在基材表面显示出其独特的颜色。钯显示银灰色。
在UV辐照后,将基材浸在无电镀溶液中。通过一般的无电镀法进行无电镀,但优选镍无电镀和铜无电镀。在本发明的优选实施方案中,镍无电镀的溶液优选含有16.5-18.5g/L的NiSO4、29-31g/L的NaC6H5O7、8.9-9.1g/L的NaC2H3O2、87-89g/L的NaH2PO2和3.7-3.9g/L的KOH。铜镀液优选含有4.5-5.5g/L的CuSO4、7-8g/L的NaOH、2-3.5g/L的HCHO、和30-36g/L的EDTA。
尽管起始反应会随镀液类型的不同而稍有差别,但一般在浸渍2-5分钟之后开始无电镀反应。基材在化学镀液中浸渍约30分钟后会在格栅图案上产生微米级的金属镀层。由于无电镀反应仅仅发生在催化剂上,因此通过无电镀得到的金属层仅仅在印刷部分上。金属层呈格栅图案,并因此具有透明度和导电性。
本发明的EMI屏蔽材料具有层状结构的基材、UV固化层和由下至上的镀层。通常,基材优选是透明材料,例如在等离子体显示过滤器中广泛应用的玻璃。
如上所述,催化剂前体组合物含有对基材具有优良粘附性的UV固化树脂,因此无需对基材进行预处理的步骤,从而提供了EMI屏蔽材料的简易制备方法。
此外,本发明提供了包含本发明得到的EMI屏蔽膜、近红外线屏蔽膜(NIR膜)、防反射涂膜(AR膜)、Neon-cut层、校色层和黑层的PDP过滤器。
本发明也提供了含等离子体显示过滤器的等离子体显示面板。
图1是根据本发明实施方案的等离子体显示面板的图。现参照图1更详细描述本发明的等离子体显示面板。该等离子显示面板装有显示图象用显示屏11,在显示屏11后面装有运行面板用电子元件的运行电路基底12,显示红、绿和蓝的面板组件13,装在面板组件13前面的等离子体显示过滤器14,容纳等离子体显示屏11、运行电路基底12、面板组件13以及等离子体显示过滤器14的罩15。
图2是图1中所示等离子体显示过滤器的放大剖面图。该等离子显示过滤器在透明基材上具有层状结构的几个功能膜。参见图2,等离子体显示过滤器14在透明基材140上具有层状结构的校色膜142,EMI屏蔽膜144,近红外线屏蔽膜146和防反射膜148。
在PDP过滤器14中,近红外线屏蔽膜146包括近红外线吸收膜,其中将与近红外线吸收染料混合的聚合物涂覆在透明基材140上。
本发明的PDP包括EMI屏蔽过滤器,该过滤器在图2所示的面板组件上部具有EMI屏蔽材料。因此,本发明能降低PDP的生产成本。
下面通过实施例来更详细描述本发明。然而,以下实施例仅仅用于理解本发明,而不应限制本发明的范围。
实施例
实施例1
A.催化剂前体组合物的制备
通过将15g乙酸钯和35g Irgacure 184(Ciba)溶解在400g甲乙酮中得到溶液。在搅拌该溶液的同时,加入300g三丙二醇二丙烯酸酯和100g季戊四醇三丙烯酸酯作为活性单体。将该溶液匀化后,向该混合溶液中加入600g脂族聚氨酯丙烯酸酯(Ebecyl 264,SK-ucb)作为活性低聚物,然后搅拌使其成为均匀溶液,从而得到室温下粘度为298cps的催化剂前体组合物。
B.催化剂前体组合物的印刷
根据凹版印刷法,在格栅的线宽为30μm和间距为300μm的矩形格栅图案中将催化剂前体组合物印刷在聚酯基材(SH34,SKC)上。将溶剂在80℃干燥1分钟后立即用UV灯照射基材。约2分钟后,催化剂前体溶液固化成为具有钯的银灰色的固相。
C.无电镀
将用UV辐照的基材浸渍在50℃的镍镀液中。约5分钟后,在印刷图案表面产生氢气,这表示化学镍还原反应的开始。约30多分钟后,在图案表面选择性形成6μm厚的镍层。Nichiban胶带测试结果表明,化学镍层对基材的粘附度为99/100。所制造的透明EMI屏蔽材料具有120Ω/sq.的表面电阻和78%的透光度。
实施例2
A.催化剂前体组合物的制备
通过将20g乙酰丙酮钯、30g Irgacure 184(Ciba)和5g Irgacure TPO(Ciba)溶解在400g氯仿中得到溶液。在搅拌该溶液的同时,加入200g1,6-己二醇二丙烯酸酯、250g二丙二醇二丙烯酸酯、150g三乙二醇二丙烯酸酯和300g丙烯酸辛酯/癸酯作为活性单体。将该溶液匀化后,向该混合溶液中加入100g聚酯丙烯酸酯(CN2200,Sartomer)作为活性低聚物,然后搅拌使其成为均匀溶液,从而得到室温下粘度为4.1cps的催化剂前体组合物。
B.催化剂前体组合物的印刷
将该催化剂前体组合物注入到空的喷墨印刷用墨盒中,然后将该墨盒装在喷墨打印机上。该打印机和墨盒是分别是由Epson制造的Stylus 980型打印机和T003型墨盒。利用美国电脑软件公司(Autodesk)的AutoCAD 2002软件使用计算机制造线宽40μm和线距400μm的矩形格栅图案,通过使计算机与打印机相连将催化剂前体组合物印刷在格栅图案中的聚酯基材上。将溶剂在65℃经1分钟干燥后立即用UV灯辐照基材。使用光纤进行UV辐照。约1分钟后,催化剂前体溶液固化成为具有钯的银灰色的固相。
C.无电镀
将用UV辐照的聚酯基材浸渍在46℃的铜镀液中。约5分钟后,在图案表面开始镀反应。约30多分钟后,约1.5μm厚的铜层选择性粘附在图案表面。Nichiban胶带的试验结果表明,化学铜层对基材的粘附度为99/100。所制造的透明EMI屏蔽材料具有15Ω/sq.的表面电阻和78%的透光度。
测量
用Brookfield制造的DV-II+粘度计测量催化剂前体组合物的粘度。分别用Guardian制造的Guardian 232-1000表面电阻率计和Murakami Color Research Laboratory制造的HR-100透射率反射率计测量表面电阻和透光度。通过根据JIS D0202进行的Nichiban胶带试验测量无电镀金属层对基材的粘附度。
化学镀液
在实施例中制备了镍化学镀液,而铜化学镀液购自Cuposit 250TM(Shipley)。化学镀液具有以下组成和状态。
镍化学镀液:
16.5-18.5g/L的NiSO4;29-31g/L的NaC6H5O7;8.9-9.1g/L的NaC2H3O2;87-89g/L的NaH2PO2;3.7-3.9g/L的KOH。温度:47-53℃。
铜化学镀液(Cuposit 250TM)
4.5-5.5g/L的CuSO4;7-8g/L的NaOH;2-3.5g/L的HCHO;30-36g/L的EDTA。温度:43-49℃。
根据将本发明的催化剂前体组合物印刷在基材上以得到图案、将该图案干燥、U.V.辐照、然后在其上进行无电镀的实施例,本发明提供了将金属如镍和铜仅仅电镀在图案上的图案而无需对基材进行额外的预处理,从而易于制备EMI屏蔽材料。而且,该EMI屏蔽材料具有良好的表面电阻和透光度。
Claims (13)
1.无电镀用催化剂前体组合物,包括:
(a)活性低聚体;
(b)活性单体;
(c)光引发剂;
(d)无电镀用催化剂前体;和
(e)溶剂。
2.根据权利要求1的催化剂前体组合物,其中(a)活性低聚体具有丙烯酸酯或甲基丙烯酸酯作为官能团,且分子量为500-5000。
3.根据权利要求2的催化剂前体组合物,其中(a)活性低聚体选自以下之一:聚氨酯丙烯酸酯、聚氨酯二丙烯酸酯、聚氨酯三丙烯酸酯、聚氨酯甲基丙烯酸酯、环氧丙烯酸酯、环氧二丙烯酸酯、聚酯丙烯酸酯、丙烯酸丙烯酸酯、和其混合物。
4.根据权利要求1的催化剂前体组合物,其中(b)活性单体具有丙烯酸酯或甲基丙烯酸酯作为官能团,且分子量为100-600。
5.根据权利要求4的催化剂前体组合物,其中(b)活性单体选自以下之一:丙烯酸异冰片酯、丙烯酸辛酯,丙烯酸癸酯、1,6-己二醇二丙烯酸酯、二丙二醇二丙烯酸酯、三丙二醇二丙烯酸酯、三乙二醇二丙烯酸酯、四乙二醇二丙烯酸酯、乙氧基化新戊二醇二丙烯酸酯、丙氧基化新戊二醇二丙烯酸酯、丙烯酸2-苯氧乙酯、丙氧基化甘油三丙烯酸酯、乙氧基化三羟甲基丙烷三丙烯酸酯、季戊四醇三丙烯酸酯、和其混合物。
6.根据权利要求1的催化剂前体组合物,其中(c)光引发剂选自以下之一:α-羟基酮、苯基乙醛酸酯、苯偶酰二甲缩酮、α-氨基酮、单酰基膦、二酰基膦、和其混合物。
7.根据权利要求1的催化剂前体组合物,其中(d)无电镀用催化剂前体是包括VIIIB族金属或IB族金属的有机化合物或无机化合物。
8.根据权利要求7的催化剂前体组合物,其中(d)无电镀用催化剂前体是包含羰基或烯基的有机化合物和Pd2+的盐。
9.根据权利要求8的催化剂前体组合物,其中有机化合物的盐为选自以下之一:乙酸钯,三氟乙酸钯、草酸钯、乙酰丙酮钯、和其混合物。
10.根据权利要求1的催化剂前体组合物,其中(e)溶剂选自以下之一:氯仿、乙腈、甲乙酮、乙酸乙酯、和其混合物。
11.制备透明电磁干扰屏蔽材料的方法,包括:
用包含(a)活性低聚体,(b)活性单体,(c)光引发剂,(d)无电镀用催化剂前体和(e)溶剂的催化剂前体组合物在透明基材上印刷格栅图案的步骤;
通过UV(紫外)线辐照固化的步骤;和
在基材的固化表面上进行无电镀的步骤。
12.通过权利要求11的方法制备的透明电磁干扰屏蔽材料。
13.根据权利要求12的透明电磁干扰屏蔽材料,包括基材、UV固化层和自下至上层积的无电镀层。
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- 2004-07-23 JP JP2005518227A patent/JP4160598B2/ja not_active Expired - Lifetime
- 2004-07-27 TW TW93122464A patent/TWI267531B/zh active
- 2004-07-28 US US10/900,622 patent/US7378478B2/en not_active Expired - Lifetime
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CN101925540B (zh) * | 2007-12-21 | 2012-09-05 | 3M创新有限公司 | 液体过滤系统 |
WO2014063636A1 (en) * | 2012-10-26 | 2014-05-01 | Shenzhen Byd Auto R&D Company Limited | Coating composition, composite prepared by using the coating composition and method for preparing the same |
CN103773143A (zh) * | 2012-10-26 | 2014-05-07 | 比亚迪股份有限公司 | 白色涂料组合物、绝缘基材表面选择性金属化的方法及复合制品 |
CN103773143B (zh) * | 2012-10-26 | 2017-02-22 | 比亚迪股份有限公司 | 白色涂料组合物、绝缘基材表面选择性金属化的方法及复合制品 |
CN106519740A (zh) * | 2012-10-26 | 2017-03-22 | 比亚迪股份有限公司 | 白色涂料组合物、绝缘基材表面选择性金属化的方法及复合制品 |
US10085351B2 (en) | 2012-10-26 | 2018-09-25 | Byd Company Limited | Coating composition, composite prepared by using the coating composition and method for preparing the same |
CN106519740B (zh) * | 2012-10-26 | 2019-01-11 | 比亚迪股份有限公司 | 白色涂料组合物、绝缘基材表面选择性金属化的方法及复合制品 |
CN105828587A (zh) * | 2015-01-06 | 2016-08-03 | 富葵精密组件(深圳)有限公司 | 感光油墨及应用其的电磁屏蔽结构、电路板、电子装置 |
CN115992354A (zh) * | 2022-11-16 | 2023-04-21 | 浙江鑫柔科技有限公司 | 一种柔性基板上形成金属膜的方法 |
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TW200505977A (en) | 2005-02-16 |
EP1649077A1 (en) | 2006-04-26 |
US8053540B2 (en) | 2011-11-08 |
EP1649077B1 (en) | 2008-10-15 |
US20080213506A1 (en) | 2008-09-04 |
ATE411412T1 (de) | 2008-10-15 |
JP4160598B2 (ja) | 2008-10-01 |
KR100529371B1 (ko) | 2005-11-21 |
TWI267531B (en) | 2006-12-01 |
JP2006510809A (ja) | 2006-03-30 |
US7378478B2 (en) | 2008-05-27 |
DE602004017183D1 (de) | 2008-11-27 |
CN100427643C (zh) | 2008-10-22 |
US20050022692A1 (en) | 2005-02-03 |
KR20050013842A (ko) | 2005-02-05 |
WO2005010234A1 (en) | 2005-02-03 |
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