CN101331245A - 镀覆树脂成型体 - Google Patents
镀覆树脂成型体 Download PDFInfo
- Publication number
- CN101331245A CN101331245A CNA2006800473545A CN200680047354A CN101331245A CN 101331245 A CN101331245 A CN 101331245A CN A2006800473545 A CNA2006800473545 A CN A2006800473545A CN 200680047354 A CN200680047354 A CN 200680047354A CN 101331245 A CN101331245 A CN 101331245A
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- molded body
- water
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Classifications
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
- C23C18/2073—Multistep pretreatment
- C23C18/2086—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- C—CHEMISTRY; METALLURGY
- 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
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
- C23C18/1641—Organic substrates, e.g. resin, plastic
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- C—CHEMISTRY; METALLURGY
- 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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
-
- C—CHEMISTRY; METALLURGY
- 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
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
- C25D5/56—Electroplating of non-metallic surfaces of plastics
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3445—Five-membered rings
-
- C—CHEMISTRY; METALLURGY
- 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
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31678—Of metal
- Y10T428/31681—Next to polyester, polyamide or polyimide [e.g., alkyd, glue, or nylon, etc.]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Chemically Coating (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Laminated Bodies (AREA)
Abstract
本发明提供镀覆粘着强度高、外观美的镀覆树脂成形体。具体而言,本发明的镀覆树脂成形体包括由树脂组合物制成的树脂成形体和位于该成型体表面的金属镀层,所述树脂组合物包含(A)合成树脂、(B)在水中的溶解度(25℃)为0.01g/100g~10g/100g的水溶性物质0.1~20质量份和(C)相容剂0~20质量份,并且相对于所述(A)、(B)及(C)成分合计量100质量份还包含(D)无机充填剂1~55质量份;其中,所述树脂成形体未经含铬及/或锰的酸刻蚀处理。
Description
技术领域
本发明涉及镀覆强度高、外观优美的镀覆树脂成型体。
背景技术
出于汽车轻型化的目的,使用ABS树脂、聚酰胺树脂等的树脂成型体作为汽车部件,成为了赋予这些树脂成型体高级感、美感而镀覆铜、镍等。
传统上,对ABS树脂等的成型体实施镀覆时,为了提高树脂成型体与镀层的粘着强度,必须在脱脂步骤后进行刻蚀步骤,以使树脂成型体表面粗糙化。例如,对ABS树脂成型体、聚丙烯成型体进行镀覆时,必须在脱脂处理后用铬酸浴(三氧化铬及硫酸的混合液)进行65~70℃、10~15分钟的刻蚀处理,而废水中含有有毒的6价铬酸离子。因此,进行废水处理时的问题是:在将6价铬酸离子还原为3价离子后,必须进行中和沉淀处理。
考虑到这样的现场作业时的安全性、废水对环境的影响,希望不进行使用铬酸浴的刻蚀处理,但此时存在的问题时:无法提高镀层与由ABS树脂等得到的成型体之间的粘着强度。
在特开2003-82138号公报、特开2003-166067号公报和特开2004-2996号公报记载的发明中,为解决现有问题,不经过使用铬酸浴的刻蚀处理,获得了具有高粘着强度金属镀层的镀覆树脂成型体。
特开平6-99630号公报记载的发明在对聚酰胺成型品进行镀覆的步骤中,出于改善盐酸刻蚀表面粗化处理性和提高金属镀覆粘着强度的目的,大量地混合了大粒径的无机充填材料(实施例中混合了40重量%的平均粒径2.2μ~12μ的填充材料);而且为了抑制混合无机充填材料造成的冲击强度降低,混合了橡胶状物质。
发明内容
在特开2003-82138号公报、特开2003-166067号公报和特开2004-2996号公报记载的发明中,当采用注塑法作为镀覆前的树脂成型体的制造方法时,弹性模量低、固化速度也低,因此,在脱模性方面有待改善。在特开平6-99630号公报记载的发明中,因为混合了大量的无机充填材料,可以认为注塑时的脱模性良好。但存在的问题是:因为混合了大量的无机充填剂,所述无机充填剂在酸处理时溶解消失而形成凹凸,所以虽然镀覆后金属镀覆的粘着强度增大,但金属镀覆后的外观不佳。
本发明的技术问题是提供如下镀覆树脂成型体:其在对镀覆步骤前的树脂成型品进行注塑成型时的脱模性高、粘着强度高、外观优美。
本发明中,提供下述镀覆树脂成型体:其包括由树脂组合物制成的树脂成型体和位于该成型体表面的金属镀层,所述树脂组合物包含(A)合成树脂、(B)在水中的溶解度(25℃)为0.01g/100g~10g/100g的水溶性物质0.1~20质量份和(C)相容剂(compatibilizer,相溶化剤)0~20质量份,并且相对于所述(A)、(B)及(C)成分合计量100质量份还包含(D)无机充填剂1~55质量份;其中,所述树脂成型体未经采用含铬和/或锰的酸进行刻蚀处理。
对于本发明的镀覆树脂成型体而言,当采用注塑成型法作为镀覆处理前的树脂成型体的制造法时,脱模性好,因此可以改善生产性。此外,本发明的镀覆树脂成型体,镀覆的粘着强度高、在刚刚镀覆后及热循环测试后都保持优美的外观。
具体实施方式
<树脂组合物>
〔(A)成分〕
作为(A)成分合成树脂,优选选自(A-1)置于23℃水中、24hr后的吸水率(ISO62)为0.6%以上的树脂,和(A-2)置于23℃水中、24hr后的吸水率(ISO62)小于0.6%的树脂中的1种或2种以上。
(A-1)成分树脂的吸水率优选为0.6~11%,更优选为0.6~5%,特别优选为0.6~2.5%。(A-2)成分树脂的吸水率优选为0.4%以下。
本发明优选使用选自(A-1)成分树脂中的1种或2种以上树脂、与选自(A-2)成分树脂中的1种或2种以上树脂的组合。
作为(A-1)成分树脂,更优选为满足上述饱和吸水率的聚酰胺类树脂、丙烯酸盐类树脂、纤维素类树脂、乙烯醇类树脂、聚醚类树脂等,更优选为聚酰胺类树脂、聚醚类树脂,最优选为聚酰胺类树脂。
作为聚酰胺类树脂,可以列举出尼龙66、聚癸二酰1,6-己二胺(尼龙6·10)、聚十二烷二酰1,6-己二胺(尼龙6·12)、聚十二烷二酰十二亚甲基二胺(尼龙1212)、聚己二酰间苯二甲胺(尼龙MXD6)、聚己二酰1,4-丁二胺(尼龙46)及它们的混合物或共聚物;尼龙6/66、6T成分为50摩尔%以下的尼龙66/6T(6T:聚对苯二甲酰1,6-己二胺)、6I成分为50摩尔%以下的尼龙66/6I(6I:聚间苯二甲酰1,6-己二胺)、尼龙6T/6I/66、尼龙6T/6I/610等共聚物;聚对苯二甲酰1,6-己二胺(尼龙6T)、聚间苯二甲酰1,6-己二胺(尼龙61)、聚对苯二甲酰(2-甲基1,5-戊二胺)(尼龙M5T)、聚间苯二甲酰(2-甲基1,5-戊二胺)(尼龙M5I)、尼龙6T/6I、尼龙6T/M5T等共聚物。除此之外,还可以是无定形尼龙等共聚尼龙,作为无定形尼龙,可以列举出对苯二甲酸与三甲基-1,6-己二胺的缩聚物等。
而且,还可以列举出:环状内酰胺的开环聚合物、氨基酸的缩聚物及由这些成分形成的共聚物,具体地有尼龙6、聚-ω-十一碳酰胺(尼龙11)、聚-ω-十二碳酰胺(尼龙12)等脂肪族聚酰胺树脂及它们的共聚物,与由二胺、二羧酸形成的聚酰胺的共聚物,具体地包括尼龙6T/6、尼龙6T/11、尼龙6T/12、尼龙6T/6I/12、尼龙6T/6I/610/12等及它们的混合物。
作为聚酰胺类树脂,在上述中优选PA(尼龙)6、PA(尼龙)66、PA(尼龙)6/66。
作为(A-2)成分树脂,可以列举出满足上述饱和吸水率的烯烃类树脂、苯乙烯类树脂、聚苯醚树脂、聚对苯二甲酸丁二醇酯树脂、聚对苯二甲酸乙二醇酯树脂等聚酯树脂,液晶聚合物、聚苯硫醚树脂、聚缩醛树脂、聚碳酸酯树脂等热塑性树脂,环氧树脂、不饱和聚酯树脂、酚醛树脂等热固化性树脂等。
烯烃类树脂是以碳原子数2~8的单烯烃为主要单体成分的聚合物,可以列举出选自低密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯、聚丙烯、乙烯-丙烯随机共聚物、乙烯-丙烯嵌段共聚物、聚甲基戊烯、聚1-丁烯及它们的衍生物等中的1种或2种以上,这其中,优选聚丙烯。
苯乙烯类树脂可以列举出苯乙烯及α取代、环取代苯乙烯等苯乙烯衍生物的聚合物。此外,还包括以这些单体为主的、由它们与丙烯腈、丙烯酸及甲基丙烯酸等乙烯基化合物及/或丁二烯、异戊二烯等共轭二烯化合物的单体构成的共聚物。可以列举出例如聚苯乙烯、高抗冲击性聚苯乙烯(HIPS)树脂、丙烯腈-丁二烯-苯乙烯共聚物(ABS)树脂、丙烯腈-苯乙烯共聚物(AS树脂)、苯乙烯-甲基丙烯酸共聚物(MS树脂)、苯乙烯-丁二烯共聚物(SBS树脂)等。
此外,作为聚苯乙烯类树脂,也包括共聚有含羧基不饱和化合物的苯乙烯类共聚物,所述含羧基不饱和化合物可以提高与聚酰胺类树脂的相容性、反应性。共聚有含羧基不饱和化合物的苯乙烯类共聚物是在橡胶质聚合物存在下,使含羧基不饱和化合物、与视需要而定的可与其共聚的其它单体聚合而成的共聚物。
对于成分具体示例的话,有:
1)在共聚了含羧基不饱和化合物的橡胶质聚合物存在下,使以芳香族乙烯基单体为必要成分的单体或以乙烯基类芳香族化合物(芳香族ビニル)和含羧基不饱和化合物为必要成分的单体进行聚合而得到的接枝聚合物;
2)在橡胶质聚合物存在下,使以乙烯基类芳香族化合物和含羧基不饱和化合物为必要成分的单体进行共聚而得的接枝共聚物;
3)使未共聚含羧基不饱和化合物的橡胶强化苯乙烯类树脂、与以含羧基不饱和化合物和乙烯基类芳香族化合物为必要成分的单体的共聚物的混合物;
4)上述1)、2)与以含羧基不饱和化合物和乙烯基类芳香族化合物为必要成分的共聚物的混合物;
5)上述1)~4)与以乙烯基类芳香族化合物为必要成分的共聚物的混合物。
在上述1)~5)中,作为乙烯基类芳香族化合物优选苯乙烯,此外作为与乙烯基类芳香族化合物共聚的单体优选丙烯腈。在苯乙烯类树脂中,含羧基不饱和化合物优选为0.1~8质量%,更优选为0.2~7质量%。
作为本发明的(A)成分,当组合使用(A-1)成分及(A-2)成分时,(A-1)成分的比例优选为10~90质量%,更优选20~80质量%,更优选30~70质量%,特别优选30~60质量%;(A-2)成分的比例优选10~90质量%,更优选20~80质量%,更优选30~70质量%,特别优选40~70质量%。
〔(B)成分〕
(B)成分水溶性物质在水中的溶解度(25℃)为0.01g/100g~10g/100g。
作为(B)成分水溶性物质,可以列举出满足上述溶解度条件的淀粉、糊精、支链淀粉、透明质酸、羧甲基纤维素、甲基纤维素、乙基纤维素或它们的盐等多糖类;丙二醇、乙二醇、二甘醇、新戊二醇、丁二醇、戊二醇、聚氧乙二醇(polyoxyethylene glycol)、聚氧丙二醇(polyoxypropylene glycol)、三羟甲基丙烷、季戊四醇、二季戊四醇、丙三醇等多元醇;聚乙烯醇、聚丙烯酸、聚马来酸、聚丙烯酰胺、聚乙烯基吡咯烷酮、聚环氧乙烷、丙烯酸-马来酸酐共聚物、马来酸酐-二异丁烯共聚物、马来酸酐-乙酸乙烯酯共聚物、萘磺酸盐福尔马林缩合物及它们的盐等。
作为(B)成分,优选季戊四醇(溶解度7.2g/100g)、二季戊四醇(水中溶解度(20℃)为0.22g/100g)。
(B)成分的含量相对于(A)成分100质量份为0.1~20质量份,优选0.1~10质量份,更优选0.5~5质量份。
〔(C)成分〕
(C)成分相容剂是视需要含有的成分,当选择彼此相溶性低的2种以上树脂作为(A)成分树脂时,优选根据使用的树脂选择公知的相容剂。
(C)成分的含量相对于(A)成分100质量份为0~20质量份,优选1~15质量份,更优选1~10质量份。
〔(D)成分〕
作为(D)成分无机充填材料,可以使用粒状或粉状充填材料或纤维状充填材料。(D)成分无机充填材料是用于改善对镀覆对象即树脂成型体进行注塑时的脱模性的成分,而不是起改善镀覆后的镀覆粘着强度作用的成分。
作为粒状或粉状充填材料,可以列举出滑石、炭黑、石墨、二氧化钛、二氧化硅、云母、硫酸钙、碳酸钙(重质碳酸钙、沉降碳酸钙)、碳酸钡、碳酸镁、硫酸镁、硫酸钡、过硫酸盐(オキシサルフエ一ト)、氧化锡、氧化铝、高岭土、碳化硅、金属粉末、玻璃粉、玻璃片、玻璃珠等。
粒状或粉状充填材料的平均粒径优选100μm以下,更优选50μm以下,更优选10μm以下,特别优选5μm以下。(D)成分的平均粒径在所述范围内,不仅可以改善注塑时的脱模性,还可以美化镀覆后的外观。平均粒径采用沉降天平法测定,以50%粒度中值表示。
作为纤维状充填材料,可以列举出硅灰石、玻璃纤维、玻璃纤维的缩绒纤维(ミルドフアイバ一)、碳纤维、碳纤维的缩绒纤维、钛酸钾晶须、硼酸铝晶须、氧化锌晶须、绿坡缕石等。
(D)成分中,作为纤维状充填材料优选硅灰石,粒状或粉状充填材料优选滑石、碳酸钙(特别是平均粒径小的沉降碳酸钙)、高岭土等。当使用碳酸钙时,平均粒径优选为2μm以下,更优选为1.5μm以下、1.0μm以下、0.5μm以下、0.1μm以下。
(D)成分含量相对(A)、(B)及(C)成分合计量100质量份为1~55质量份,优选1~40质量份、更优选1~35质量份、特别优选5~25质量份。(D)成分的含量在所述范围内,不仅可以改善注塑时的脱模性,还可以美化镀覆后的外观。
〔其它成分〕
本发明中,还可以混合表面活性剂及/或凝固剂。当采用乳液聚合制造(A)成分时,表面活性剂可以是残留在树脂中的表面活性剂(乳化剂);当采用本体聚合等不使用乳化剂的制造方法时,可以通过其它途径向(A)成分中添加表面活性剂。
表面活性剂、凝固剂可以是用于树脂的乳液聚合的制品,也可以是其它制品。表面活性剂优选阴离子型表面活性剂、阳离子型表面活性剂、非离子型表面活性剂、两性表面活性剂。
作为表面活性剂可以列举出选自:脂肪酸盐、松香酸盐、烷基硫酸盐、烷基苯磺酸盐、烷基二苯醚磺酸盐、聚氧乙烯烷基醚硫酸盐、磺基丁二酸二酯盐、α-烯烃硫酸酯盐、α-烯烃磺酸盐等阴离子表面活性剂;单或二烷基胺或其聚氧乙烯加合物、单或二长链烷基季铵盐等阳离子表面活性剂;烷基糖苷、聚氧乙烯烷基醚、聚氧乙烯烷基苯基醚、蔗糖脂肪酸酯、山梨聚糖脂肪酸酯、聚氧乙烯山梨聚糖脂肪酸酯、聚氧乙烯脂肪酸酯、聚氧乙烯丙烯嵌段共聚物、脂肪酸单甘油酯、氧化胺等非离子表面活性剂;羧基甜菜碱(カルボベタイン)、磺基甜菜碱(スルホベタイン)、羟基磺基甜菜碱(ヒドロキシスルホベタイン)等两性表面活性剂中的1种或2种以上。
树脂组合物中表面活性剂的含量相对于(A)成分100质量份优选为0.01~10质量份,更优选0.01~5质量份,更优选0.01~2质量份。
本发明中,还可以混合选自下列的1种或2种以上的含磷化合物。
磷酸三苯酯、磷酸三甲苯酯、磷酸三(二甲苯酯)、磷酸三(异丙基苯酯)、磷酸三(邻-或对-苯基苯酯)、磷酸三萘酯、磷酸甲苯基二苯基酯、二甲苯基二苯基磷酸酯、二苯基(2-乙基己基)磷酸酯、二(异丙基苯基)苯基磷酸酯、邻-苯基苯基二甲苯基磷酸酯、三(2,6-二甲基苯基)磷酸酯、间苯撑二磷酸四苯酯、对苯撑二磷酸四苯酯、苯基间二苯酚·聚磷酸酯、双酚A-双(二苯基磷酸酯)、双酚A·聚苯基磷酸酯、二焦儿茶酚次二磷酸酯(ジピロカテコ一ルハイポジホスフエ一ト)等缩合类磷酸酯;
二苯基(2-乙基己基)磷酸酯、二苯基-2-丙烯酰氧基乙基磷酸酯、二苯基-2-甲基丙烯酰氧基乙基磷酸酯、二苯基新戊基磷酸酯、季戊四醇二苯基二磷酸酯、乙基焦儿茶酚磷酸酯等正磷酸酯等脂肪酸·芳香族磷酸酯。
聚磷酸密胺、三聚磷酸、焦磷酸、正磷酸、六偏磷酸等的碱金属盐、肌醇六磷酸等含磷化合物或它们的碱金属盐或烷醇胺盐等。
而且,作为上述以外的含磷化合物,可以使用公知的用作树脂用阻燃剂及抗氧化剂的磷酸类化合物。
树脂组合物中含磷化合物的含量,相对于(A)成分100质量份优选为0.1~30质量份,更优选0.1~20质量份,更优选0.1~10质量份。
本发明的树脂组合物中,根据树脂成型体的用途,可以混合公知的各种添加剂。
<镀覆树脂成型体>
本发明的镀覆树脂成型体是在使用上述树脂组合物,采用注塑、挤出成型等公知的成型方法,获得适于其用途的希望形状的树脂成型体后,按下述步骤进行镀覆。但是,本发明的镀覆树脂成型体在其镀覆步骤中,对于镀覆对象即树脂成型体不使用含铬及/或锰的酸进行刻蚀处理。
镀覆方法可以采用在特开2003-82138号公报、特开2003-166067号公报和特开2004-2996号公报记载的发明的实施例中记载的方法(I)(包括无电解镀覆步骤的镀覆方法),及包括直接镀覆步骤的镀覆方法(II)。不论采用何种镀覆方法,均不对镀覆对象即树脂成型体的表面使用含铬及/或锰的酸进行刻蚀处理。
(I)在特开2003-82138号公报、特开2003-166067号公报和特开2004-2996号公报记载的发明中的实施例中记载的方法(包括无电解镀覆步骤的镀覆方法)
(1)脱脂步骤
(2)用酸进行接触处理的步骤
(3)添加催化剂步骤
(4)第1活化步骤
(5)第2活化步骤
(6)镍的无电解镀覆步骤
(7)酸活化步骤
(8)铜的电镀步骤
(II)包括直接镀覆步骤的镀覆方法
(1)脱脂步骤
(2)用酸进行接触处理的步骤(刻蚀步骤)
(3)添加催化剂步骤
(4)直接镀覆步骤
(5)铜的电镀步骤
镀覆方法(II)中,脱脂步骤、用酸进行接触处理的步骤、添加催化剂的步骤及铜的电镀步骤与在特开2003-82138号公报、特开2003-166067号公报和特开2004-2996号公报记载的发明的实施例中记载的方法相同。但,与镀覆方法(I)的“(2)用酸进行接触处理的步骤”相比,镀覆方法(II)的“(2)用酸进行接触处理的步骤”中,使用浓度更高的酸。
在镀覆方法(II)的“(2)用酸进行接触处理的步骤”中,作为酸,除了盐酸、磷酸、硫酸外,还可以使用有机酸等,例如乙酸、柠檬酸、甲酸等。
当使用盐酸时,优选1.5~3.5当量的盐酸,更优选1.8~3.5当量的盐酸,更优选2~3当量的盐酸。
该步骤的处理可以采用例如:将树脂成型体浸渍在酸中的方法,可以采用在液温10~80℃的酸中浸渍0.5~20分钟的方法。使用1.5~3.5当量的盐酸时,可以采用在所述浓度范围的盐酸水溶液中于20~60℃浸渍1~10分钟的方法。
包括直接镀覆步骤的镀覆方法(II)是公知的,其公开于特开平5-239660号公报、WO98/45505(专利第3208410号公报)、特开2002-338636号公报(第5段)等。
直接镀覆步骤中,使用称作选择液的含有金属化合物、还原性化合物及金属氢氧化物的镀覆液,与通过以往常用的化学镀覆形成的镀层(导电层)相比,可形成极薄的导电层。
作为金属化合物,优选铜化合物,可以列举出例如硫酸铜、氯化铜、碳酸铜、氧化铜、氢氧化铜。铜化合物的含量以铜计优选为0.1~5g/L,更优选为0.8~1.2g/L。
还原性化合物中不含有诸如公知的在无电解镀覆(化学镀覆)中常用的福尔马林、次磷酸那样的还原力强的物质,可以列举出例如下述比它们还原力弱的物质:
可以列举出:氯化亚锡、硼氢化钠、二甲胺硼烷、三甲胺硼烷、甲酸或其盐类、甲醇、乙醇、丙醇、乙二醇、丙三醇等醇及其盐;
可以列举出:还原性糖类,例如,葡萄糖、葡萄糖(グルコ一ス)、山梨糖醇、纤维素、蔗糖、甘露糖、葡糖酸内酯。糖类的含量优选3~50g/L,更优选10~20g/L。
作为金属氢氧化物,可以列举出氢氧化钠、氢氧化钾、氢氧化锂等。金属氢氧化物的含量优选10~80g/L,更优选30~50g/L。
选择液中,视需要可以含有络合剂(錯化剤)。作为络合剂,可以列举出:乙内酰脲类、有机羧酸类等。作为乙内酰脲类,可以列举出乙内酰脲、1-甲基乙内酰脲、1,3-二甲基乙内酰脲、5,5-二甲基乙内酰脲、尿囊素等;作为有机羧酸类,可以列举出柠檬酸、酒石酸、琥珀酸及它们的盐等。选择液中螯合剂的含量优选2~50g/L,更优选10~40g/L。
选择液的pH优选在10.0~14.0的范围,更优选在11.5~13.5的范围。
作为选择液的具体例子,可以使用特开平5-239660号公报实验例1的(c)(第31段)记载的镀覆浴、WO98/45505(专利第3208410号公报)实施例记载的本发明浴1~8,视需要可以添加其它公知成分。
直接镀覆步骤处理可以采用下述方法:将选择液的液温调整为优选20~70℃、更优选35~50℃,然后浸渍树脂成型体30秒~20分钟左右、优选3~5分钟左右。
通过直接镀覆步骤处理,在树脂成型体的表面形成膜厚非常薄的导电层,因此可以在接下来的步骤中,进行直接电镀。
本发明的镀覆树脂成型体优选在经历下述热循环测试后,通过肉眼观察不能发现其外观变化。
(热循环测试1)
使用长100mm、宽50mm、厚3mm的镀覆树脂成型体作为测试片,以-30℃保持60分钟、室温(20℃)保持30分钟、90℃保持60分钟、室温(20℃)保持30分钟为1个循环,进行共计3个循环的热循环测试。
(热循环测试2)
使用长100mm、宽50mm、厚3mm的镀覆树脂成型体作为测试片,以
-30℃保持60分钟、室温(20℃)保持30分钟、100℃保持60分钟、室温(20℃)保持30分钟为1个循环,进行共计3个循环的热循环测试。
本发明的镀覆树脂成型体的形状、镀层种类、厚度等,可以根据各种用途适宜选择,特别适合于作为减震器(バンパ一)、标志、轮盖、内装部件、外装部件等汽车部件使用。
实施例
(树脂组合物)
(A)成分
(A-1-1):聚酰胺(聚酰胺6,宇部兴产株式会社制,UBE尼龙61013B,吸水率1.8%)
(A-1-2):聚酰胺(聚酰胺66,宇部兴产株式会社制,UBE尼龙662020B,吸水率1.3%)
(A-2-1):AS树脂(苯乙烯量75质量%、丙烯腈25质量%)
(A-2-2):ABS树脂(苯乙烯量45质量%、丙烯腈15质量%、橡胶量40质量%)
(A-2-3):聚丙烯树脂(J713M、Grandpolymer公司制)
(B)成分
(B-1):二季戊四醇(广荣化学工业公司制)
(C)成分
(C-1):酸改性ABS树脂(苯乙烯量42质量%、丙烯腈16质量%、橡胶量40质量%、甲基丙烯酸量2质量%)
(C-2):酸改性ABS树脂(苯乙烯量40质量%、丙烯腈14质量%、橡胶量40质量%、甲基丙烯酸量6质量%)
(C-3):酸改性聚丙烯树脂(E109H、Grandpolymer(株))
(D)成分
(D-1):硅灰石(PH330、JFE矿物(株)制、平均粒径3.2μm)
(D-2):滑石(5000S、林化成(株)制、平均粒径2.8μm)
(D-3):碳酸钙(Calfine200、丸尾钙(株)制、平均粒径0.07μm)
(D-4):碳酸钙(SL-2200、竹原化学工业(株)、平均粒径1.3μm)
(D-5):烧结高岭土(NeoGen 2000、竹原化学工业(株)制、平均粒径0.7μm)
实施例及比较例
用V型转鼓(タンブラ一)混合表1记载的各成分,然后用双螺杆挤出机(日本制钢制,TEX30,料筒温度230℃)进行熔融混炼,得到了粒料。然后,通过注塑成型机(料筒温度240℃、模具温度60℃)得到了100×50×3mm的树脂成型体。
以得到的树脂成型体作为测试片,进行(I)包括无电解镀覆步骤的镀覆或(II)包括直接镀覆步骤的镀覆,得到了镀覆树脂成型体。这些镀覆树脂成型体的热循环测试结果如表1所示。
(I)包括无电解镀覆步骤的镀覆
(1)脱脂步骤
将测试片在Catalyst A-220(奥野制药工业(株)制)50g/L水溶液(液温40℃)中浸渍20分钟。
(2)用酸进行接触处理的步骤
在1.0当量的盐酸100ml(液温40℃)中浸渍5分钟。
(3)添加与催化剂的步骤
在35质量%盐酸150ml/L,与Catalyst C(奥野制药工业(株)制)40ml/L水溶液的混合水溶液(液温25℃)中浸渍3分钟。
(4)第1活化步骤
将测试片在100ml/L的98质量%硫酸水溶液(液温40℃)中浸渍3分钟。
(5)第2活化步骤
将测试片在15g/L的氢氧化钠水溶液(液温40℃)中浸渍2分钟。
(6)镍的无电解镀覆步骤
将测试片在150ml/L化学镍HR-TA(奥野制药工业(株)制)、与150ml/L化学镍HR-TB(奥野制药工业(株)制)的混合水溶液(液温40℃)中浸渍5分钟。
(7)酸活化步骤
将测试片在TOP SUN(奥野制药工业(株)制)的100g/L水溶液(液温25℃)中浸渍1分钟。
(8)铜的电镀步骤
将测试片浸渍在与实施例1相同的镀覆浴(液温25℃)中,进行120分钟电镀。
(II)包括直接镀覆步骤的镀覆
(1)脱脂步骤
将树脂成型体在Catalyst A-220(奥野制药工业(株)制)的50g/L水溶液(液温40℃)中浸渍5分钟。
(2)刻蚀步骤(用酸进行接触处理的步骤)
将树脂成型体在35质量%盐酸200ml/L(2.3当量)水溶液(液温40℃)中浸渍5分钟。
(3)添加催化剂的步骤
在150ml/L的35质量%盐酸水溶液、与40ml/L的Catalyst C(奥野制药工业(株)制)水溶液的混合水溶液(液温25℃)中浸渍3分钟。
(4)直接镀覆步骤
将树脂成型体在下述组成的选择液(45℃,pH为12)中浸渍3分钟,使树脂成型体表面形成导电层。
硫酸铜 3g/L
氢氧化钠 30g/L
葡萄糖 10g/L
乙内酰脲 10g/L
(5)铜的电镀步骤
将树脂成型体浸渍在下述组成的镀覆浴(液温25℃)中,进行120分钟电镀。
(镀覆浴的组成)
硫酸铜(CuSO4·5H2O) 200g/L
硫酸(98%) 50g/L
氯离子(Cl-) 5ml/L
脱普鲁奇那(トツプルチナ)2000MU(奥野制药工业(株)制)5ml/L
镀铜后,用肉眼对刚刚镀覆后的外观进行评价。获得光滑表面的为良好,存在粗糙面的为不良。而且,不良制品不再进行热循环测试。
表1的热循环测试中,良好表示通过肉眼观察完全未见或基本上未见刚刚镀覆后和热循环后的外观变化;膨胀表示发现镀层出现了从树脂成型体上隆起的部分。
在实施例1中,注塑成型后用于脱模的必要冷却时间为20s;在不含无机充填材料的比较例1中,冷却时间为60s。从10s开始每次5s地增加冷却时间,将不损伤成型品地进行脱模的时间作为冷却时间。
比较例2~5的镀覆树脂成型体,在刚刚镀覆后,其镀覆表面的光滑性明显劣于实施例1~18的镀覆树脂成型体。从这些结果可以认为:与实施例相比,比较例2~5中使用的无机充填材料的粒径大、混合量多,因此在用盐酸接触的步骤中,无机充填材料溶解,导致树脂成型体的表面粗糙。
另一方面,可以认为:与比较例相比,实施例1~18中使用的无机充填剂粒径小、混合量少,因此在用盐酸接触的步骤中,树脂成型体的表面没有变粗糙。特别是,与其它实施例相比,使用小粒径的(D-3)碳酸钙的实施例3和实施例8的外观优美。
Claims (4)
1.一种镀覆树脂成型体,其包括由树脂组合物制成的树脂成型体和位于该树脂成型体表面的金属镀层,
所述树脂组合物包含:(A)合成树脂、(B)0.1~20质量份在水中的溶解度(25℃)为0.01g/100g~10g/100g的水溶性物质和(C)0~20质量份相容剂,并且以所述(A)、(B)及(C)成分总质量100质量份计,该树脂组合物还包含(D)1~55质量份的无机充填材料;
其中,所述树脂成型体未经含铬和/或锰的酸进行刻蚀处理。
2.权利要求1的镀覆树脂成型体,其中,所述(A)成分合成树脂包括:
(A-1)置于23℃的水中,24hr后的吸水率(ISO62)为0.6%以上的树脂10~90质量%,和
(A-2)置于23℃的水中,24hr后的吸水率(ISO62)小于0.6%的树脂10~90质量%。
3.权利要求1或2的镀覆树脂成型体,其中,所述(D)成分无机充填材料选自滑石、碳酸钙、硅灰石、高岭土。
4.权利要求1~3任一项的镀覆树脂成型体,该镀覆树脂成型体在经历下述热循环测试后,通过肉眼观察不能发现其外观变化:
热循环测试1
使用长100mm、宽50mm、厚3mm的镀覆树脂成型体作为测试片,以在-30℃保持60分钟、室温(20℃)保持30分钟、90℃保持60分钟、室温(20℃)保持30分钟为1个循环,进行共计3个循环的热循环测试;
热循环测试2
使用长100mm、宽50mm、厚3mm的镀覆树脂成型体作为测试片,以-30℃保持60分钟、室温(20℃)保持30分钟、100℃保持60分钟、室温(20℃)保持30分钟为1个循环,进行共计3个循环的热循环测试。
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CA2189325A1 (en) * | 1995-03-10 | 1996-09-19 | Youichi Ohara | Flame-retardant polyethylene terephthalate resin compositions |
JP3362754B2 (ja) * | 1995-07-28 | 2003-01-07 | 出光石油化学株式会社 | メッキ成形体の製造方法及びその方法で得られたメッキ成形体 |
EP0810298A4 (en) * | 1995-12-19 | 1998-04-01 | Polyplastics Co | THERMOPLASTIC RESIN MOLDING HAVING A METAL LAYER ON ITS SURFACE |
JP3620614B2 (ja) * | 1996-08-01 | 2005-02-16 | 出光興産株式会社 | メッキ用樹脂組成物 |
JP4284808B2 (ja) * | 1999-03-30 | 2009-06-24 | 宇部興産株式会社 | 射出溶着用材料 |
KR100448115B1 (ko) * | 2000-11-30 | 2004-09-10 | 현대자동차주식회사 | 폴리아미드 수지 조성물 |
JP4030754B2 (ja) * | 2001-11-28 | 2008-01-09 | ダイセルポリマー株式会社 | メッキ樹脂成形体 |
JP4619625B2 (ja) * | 2002-04-03 | 2011-01-26 | ダイセルポリマー株式会社 | メッキ樹脂成形体の製造方法 |
JP4290509B2 (ja) * | 2002-08-23 | 2009-07-08 | 株式会社プライムポリマー | 金型内被覆成形体およびその製造方法 |
JP4220770B2 (ja) * | 2002-12-11 | 2009-02-04 | 三菱樹脂株式会社 | 印刷層を有する成形体、および、その製造方法 |
JP4276555B2 (ja) * | 2004-02-20 | 2009-06-10 | ダイセルポリマー株式会社 | メッキ樹脂成形体 |
JP2005232338A (ja) * | 2004-02-20 | 2005-09-02 | Daicel Polymer Ltd | メッキ樹脂成形体 |
-
2005
- 2005-12-15 JP JP2005361186A patent/JP4468295B2/ja active Active
-
2006
- 2006-12-13 EP EP06834978.6A patent/EP1961839B1/en not_active Ceased
- 2006-12-13 CN CN2006800473545A patent/CN101331245B/zh not_active Expired - Fee Related
- 2006-12-13 WO PCT/JP2006/325308 patent/WO2007069769A1/ja active Application Filing
- 2006-12-13 US US12/086,271 patent/US20090169850A1/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
JP4468295B2 (ja) | 2010-05-26 |
EP1961839A1 (en) | 2008-08-27 |
EP1961839A4 (en) | 2015-05-27 |
CN101331245B (zh) | 2012-06-13 |
US20090169850A1 (en) | 2009-07-02 |
WO2007069769A1 (ja) | 2007-06-21 |
JP2007162084A (ja) | 2007-06-28 |
EP1961839B1 (en) | 2017-10-18 |
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