CN114231874A - 一种碳钢表面的复合镀方法 - Google Patents
一种碳钢表面的复合镀方法 Download PDFInfo
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C22/68—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous solutions with pH between 6 and 8
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/027—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal matrix material comprising a mixture of at least two metals or metal phases or metal matrix composites, e.g. metal matrix with embedded inorganic hard particles, CERMET, MMC.
Abstract
一种碳钢表面的复合镀方法,包括热镀锌处理和化学复合镀处理;化学复合镀的镀液包括20~28份NiSO4·6H2O、12~20份NiCl2·6H2O、20~33份NaH2PO2·H2O、9~15份H3BO4、10~16份柠檬酸三铵、6~11份CH4N2S、2~4.5份C2H10BN、1.5~2.5份C12H25SO4Na、0.5~1.5份仲烷基磺酸钠、38~56份炭黑分散液、70~95份去离子水;本发明制备的镀件在硫酸溶液中的腐蚀速率1.27~1.88g/m2•h,氢氧化钠溶液中的腐蚀速率3.1×10‑5~4.3×10‑5g/m2•h,中性盐雾试验1069~1236小时后出现肉眼可见锈点。
Description
技术领域
本发明涉及一种碳钢表面的复合镀方法,属于金属表面处理技术领域。
背景技术
碳钢是各行各业广泛应用的基础材料,但碳钢本身普遍存在的不耐腐蚀问题,给人们的生产生活带来经济上的浪费和诸多不便,甚至危及到结构件的安全可靠性,造成生命财产方面不可挽回的巨大损失。防腐技术是有效遏制和减缓金属腐蚀的有效手段,世界各国都投入了大量物力财力开发金属耐腐蚀技术。
金属耐腐蚀防护方法非常多,常见的有表面涂层法、金属本身合金化法、特殊热处理法、电化学保护法以及表面镀层法等,其中表面镀层法因具有镀层组成材料可选范围广,镀层功能可设计性强,镀覆方法多种多样,镀层结合力强等优点而得到普遍应用。
中国专利CN101255554A公开了一种镁合金表面纳米化学复合镀溶液及其制备工艺和应用,该专利将纳米氧化物以纳米浓缩浆形式加入到镀液中的,此浆分散性好,固含量高,稳定性好,可以存放半年以上,得到的镀层仅能耐受中性盐溶液的腐蚀,对酸碱腐蚀耐受性差。
中国专利CN105603399A公开了一种低碳钢表面化学镀Ni-Zn-P/纳米SiO2复合镀层的制备工艺。该专利得到的复合镀层盐雾试验仅能耐受120小时,耐腐蚀性比较差。
以上可以看到,镀层防腐技术方面仍存在镀层耐腐蚀性能差,防护作用不持久等问题,因此开发高耐蚀镀层的制备方法对降低金属腐蚀引起的损失有着十分重要的作用。
发明内容
针对上述现有技术存在的不足,本发明提供一种碳钢表面的复合镀方法,实现以下发明目的:开发制备耐腐蚀镀层的化学复合镀方法,利用该方法制备出结合力强,耐腐蚀性能优异且防护作用持久的复合镀层。
为实现上述发明目的,本发明采取以下技术方案:
一种碳钢表面的复合镀方法,包括热镀锌处理和化学复合镀处理,其中化学复合镀处理包括化学复合镀的镀液配制和施镀。所述化学复合镀的镀液,以重量份计,包括20~28份NiSO4·6H2O、12~20份NiCl2·6H2O、20~33份NaH2PO2·H2O、9~15份H3BO4、10~16份 柠檬酸三铵、6~11 份CH4N2S、2~4.5份C2H10BN、1.5~2.5份C12H25SO4Na、0.5~1.5份仲烷基磺酸钠、38~56份炭黑分散液、70~95份去离子水;所述炭黑分散液的制备方法为将1,2,4-丁三醇、异辛醇磷酸酯钾盐、月桂基磺化琥珀酸单酯二钠溶解于去离子水中,加入改性炭黑后,4500~6500转/分下搅拌1~2小时后,超声分散15~40分钟得到;所述改性炭黑的制备方法为强力搅拌下将炭黑加入强氧化剂溶液中,超声分散均匀后,加热搅拌反应完成后离心分离,得到的沉淀用去离子水洗涤三遍,然后烘干得到改性炭黑。
以下是对上述技术方案的进一步改进:
步骤1 热镀锌处理
碳钢件经表面处理后,浸入锌液中,浸渍30~75秒后提出镀件,水冷至室温后吹干,然后浸入60~75℃钝化液中,浸渍35~65分钟后提出镀件,去离子水冲洗干净后吹干,得到表面镀锌件;
所述表面处理,碳钢件进行表面除锈、碱水浴除油、热水洗涤、酸洗除锈、冷水冲洗;
所述锌液的温度为422~443℃;
所述钝化液,由锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水组成;
所述锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水的质量比为4~7:5~8:1~3:3~5:23~40。
步骤2化学复合镀处理
(1)化学复合镀的镀液配制
所述化学复合镀的镀液,以重量份计,包括以下组分:
20~28份NiSO4·6H2O
12~20份NiCl2·6H2O
20~33份NaH2PO2·H2O
9~15份H3BO4
10~16份柠檬酸三铵
6~11 份CH4N2S
2~4.5份C2H10BN
1.5~2.5份C12H25SO4Na
0.5~1.5份仲烷基磺酸钠
38~56份炭黑分散液
70~95份去离子水;
A、炭黑分散液的制备:
将1,2,4-丁三醇、异辛醇磷酸酯钾盐、月桂基磺化琥珀酸单酯二钠溶解于去离子水中,加入改性炭黑后,4500~6500转/分下强力搅拌1~2小时后,超声分散15~40分钟得到炭黑分散液;
所述1,2,4-丁三醇的加入量为去离子水质量的15~26%;
所述异辛醇磷酸酯钾盐的加入量为去离子水质量的1~2%;
所述月桂基磺化琥珀酸单酯二钠的加入量为去离子水质量的0.5~2%;
所述改性炭黑的加入量为去离子水质量的50~65%。
B、改性炭黑的制备:
强力搅拌下将炭黑加入强氧化剂溶液中,超声分散均匀后,加热搅拌反应完成后离心分离,得到的沉淀用去离子水洗涤三遍,然后烘干得到改性炭黑;
所述强力搅拌,搅拌速率为4000~5000转/分;
所述炭黑,粒径30~95nm;
所述炭黑与强氧化剂溶液的质量比为2~5:8;
所述强氧化剂溶液,由H2XeO4、Na2S2O8、双氧水组成;
所述H2XeO4、Na2S2O8、双氧水的质量比为1~4:3~6:15~20;
所述双氧水,H2O2的浓度为20~30wt%;
所述超声分散,超声时间25~45分钟;
所述加热搅拌反应,温度为80~90℃,搅拌速率为1200~1500转/分,反应时间2~5小时;
C、化学复合镀的镀液配制工艺:
按配方中各原料重量份,将NiSO4·6H2O、NiCl2·6H2O、NaH2PO2·H2O
H3BO4、柠檬酸三铵、CH4N2S、C2H10BN、C12H25SO4Na、仲烷基磺酸钠加入到去离子水中,搅拌溶解后,将搅拌速率提升至2500~3500转/分,缓慢加入炭黑分散液,强烈搅拌0.5~1.5小时后得到均一稳定的镀液。
(2)施镀
控制搅拌速率150~400转/分,镀液温度85~95℃下,将热镀锌处理后的碳钢件全部浸入镀液中,施镀40~90分钟,然后取出用去离子水清洗并吹干,得到含炭黑镀层的碳钢件。
与现有技术相比,本发明取得以下有益效果:
1、采用本发明所述的复合镀方法,在碳钢表面制备出了两层结构的复合镀层,底层为热镀锌层,外层为含改性炭黑的化学复合镀镀层,得到的复合镀层耐酸碱腐蚀性好且能长期耐受中性盐雾的腐蚀;
2、采用本发明所述的复合镀方法处理后的碳钢件,硫酸溶液中的腐蚀速率1.27~1.88g/m2•h,氢氧化钠溶液中的腐蚀速率3.1×10-5~4.3×10-5g/m2•h,中性盐雾试验1069~1236小时后碳钢件表面出现肉眼可见锈点;
3、采用本发明所述的复合镀方法处理后的碳钢件,镀层的结合力强,采用弯曲法测试时,碳钢镀件弯曲54~67次,镀层表面才出现折痕;采用热震法时,碳钢镀件经过29~36次循环后,表面镀层才开始出现起皮脱落现象。
具体实施方式
以下对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。
实施例1:一种碳钢表面的复合镀方法
包括以下步骤:
1、热镀锌处理
碳钢件经表面处理后,浸入锌液中,浸渍50秒后提出镀件,水冷至室温后吹干,然后浸入70℃钝化液中,浸渍55分钟后提出镀件,去离子水冲洗干净后吹干,得到表面镀锌件;
所述表面处理,碳钢件进行表面除锈、碱水浴除油、热水洗涤、酸洗除锈、冷水冲洗;
所述锌液的温度为430℃;
所述钝化液,由锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水组成;
所述锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水的质量比为7:8:3:5:40。
2、化学复合镀处理
(1)化学复合镀的镀液配制
所述化学复合镀的镀液,以重量份计,包括以下组分:
24份NiSO4·6H2O
16份NiCl2·6H2O
25份NaH2PO2·H2O
13份H3BO4
14份柠檬酸三铵
8份CH4N2S
3份C2H10BN
2份C12H25SO4Na
1份 仲烷基磺酸钠
52份炭黑分散液
80份去离子水;
A、炭黑分散液的制备:
将1,2,4-丁三醇、异辛醇磷酸酯钾盐、月桂基磺化琥珀酸单酯二钠溶解于去离子水中,加入改性炭黑后,6000转/分下强力搅拌1.5小时后,超声分散30分钟得到炭黑分散液;
所述1,2,4-丁三醇的加入量为去离子水质量的20%;
所述异辛醇磷酸酯钾盐的加入量为去离子水质量的1.6%;
所述月桂基磺化琥珀酸单酯二钠的加入量为去离子水质量的1.1%;
所述改性炭黑的加入量为去离子水质量的60%。
B、改性炭黑的制备:
强力搅拌下将炭黑加入强氧化剂溶液中,超声分散均匀后,加热搅拌反应完成后离心分离,得到的沉淀用去离子水洗涤三遍,然后烘干得到改性炭黑;
所述强力搅拌,搅拌速率为4600转/分;
所述炭黑,粒径60nm;
所述炭黑与强氧化剂溶液的质量比为1:2;
所述强氧化剂溶液,由H2XeO4、Na2S2O8、双氧水组成;
所述H2XeO4、Na2S2O8、双氧水的质量比为2:5:18;
所述双氧水,H2O2的浓度为26wt%;
所述超声分散,超声时间35分钟;
所述加热搅拌反应,温度为86℃,搅拌速率为1400转/分,反应时间4小时;
C、化学复合镀的镀液配制工艺:
按配方中各原料重量份,将NiSO4·6H2O、NiCl2·6H2O、NaH2PO2·H2O、
H3BO4、柠檬酸三铵、CH4N2S、C2H10BN、C12H25SO4Na、仲烷基磺酸钠加入到去离子水中,搅拌溶解后,将搅拌速率提升至3000转/分,缓慢加入炭黑分散液,强烈搅拌1小时后得到均一稳定的镀液。
(2)施镀
控制搅拌速率300转/分,镀液温度90℃下,将热镀锌处理后的碳钢件全部浸入镀液中,施镀70分钟,然后取出用去离子水清洗并吹干,得到含炭黑镀层的碳钢件。
实施例2:一种碳钢表面的复合镀方法
包括以下步骤:
1、热镀锌处理
碳钢件经表面处理后,浸入锌液中,浸渍30秒后提出镀件,水冷至室温后吹干,然后浸入60℃钝化液中,浸渍35分钟后提出镀件,去离子水冲洗干净后吹干,得到表面镀锌件;
所述表面处理,碳钢件进行表面除锈、碱水浴除油、热水洗涤、酸洗除锈、冷水冲洗;
所述锌液的温度为422℃;
所述钝化液,由锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水组成;
所述锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水的质量比为5:7:1:3:30。
2、化学复合镀处理
(1)化学复合镀的镀液配制
所述化学复合镀的镀液,以重量份计,包括以下组分:
20份NiSO4·6H2O
12份NiCl2·6H2O
20份NaH2PO2·H2O
9份H3BO4
10份柠檬酸三铵
6份CH4N2S
2份C2H10BN
1.5份C12H25SO4Na
0.5份仲烷基磺酸钠
38份炭黑分散液
70份去离子水;
A、炭黑分散液的制备:
将1,2,4-丁三醇、异辛醇磷酸酯钾盐、月桂基磺化琥珀酸单酯二钠溶解于去离子水中,加入改性炭黑后,4500转/分下强力搅拌1小时后,超声分散15分钟得到炭黑分散液;
所述1,2,4-丁三醇的加入量为去离子水质量的15%;
所述异辛醇磷酸酯钾盐的加入量为去离子水质量的1%;
所述月桂基磺化琥珀酸单酯二钠的加入量为去离子水质量的0.5%;
所述改性炭黑的加入量为去离子水质量的50%。
B、改性炭黑的制备:
强力搅拌下将炭黑加入强氧化剂溶液中,超声分散均匀后,加热搅拌反应完成后离心分离,得到的沉淀用去离子水洗涤三遍,然后烘干得到改性炭黑;
所述强力搅拌,搅拌速率为4000转/分;
所述炭黑,粒径30nm;
所述炭黑与强氧化剂溶液的质量比为1:4;
所述强氧化剂溶液,由H2XeO4、Na2S2O8、双氧水组成;
所述H2XeO4、Na2S2O8、双氧水的质量比为1:3:15;
所述双氧水,H2O2的浓度为20wt%;
所述超声分散,超声时间25分钟;
所述加热搅拌反应,温度为80℃,搅拌速率为1200转/分,反应时间2小时;
C、化学复合镀的镀液配制工艺:
按配方中各原料重量份,将NiSO4·6H2O、NiCl2·6H2O、NaH2PO2·H2O、H3BO4、柠檬酸三铵、CH4N2S、C2H10BN、C12H25SO4Na、仲烷基磺酸钠加入到去离子水中,搅拌溶解后,将搅拌速率提升至2500转/分,缓慢加入炭黑分散液,强烈搅拌0.5小时后得到均一稳定的镀液。
(2)施镀
控制搅拌速率150转/分,镀液温度85℃下,将热镀锌处理后的碳钢件全部浸入镀液中,施镀40分钟,然后取出用去离子水清洗并吹干,得到含炭黑镀层的碳钢件。
实施例3:一种碳钢表面的复合镀方法
包括以下步骤:
1、热镀锌处理
碳钢件经表面处理后,浸入锌液中,浸渍75秒后提出镀件,水冷至室温后吹干,然后浸入75℃钝化液中,浸渍65分钟后提出镀件,去离子水冲洗干净后吹干,得到表面镀锌件;
所述表面处理,碳钢件进行表面除锈、碱水浴除油、热水洗涤、酸洗除锈、冷水冲洗;
所述锌液的温度为443℃;
所述钝化液,由锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水组成;
所述锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水的质量比为4:5:2:3:23。
2、化学复合镀处理
(1)化学复合镀的镀液配制
所述化学复合镀的镀液,以重量份计,包括以下组分:
28份NiSO4·6H2O
20份NiCl2·6H2O
33份NaH2PO2·H2O
15份H3BO4
16份柠檬酸三铵
11份CH4N2S
4.5份C2H10BN
2.5份C12H25SO4Na
1.5份 仲烷基磺酸钠
56份炭黑分散液
95份去离子水;
A、炭黑分散液的制备:
将1,2,4-丁三醇、异辛醇磷酸酯钾盐、月桂基磺化琥珀酸单酯二钠溶解于去离子水中,加入改性炭黑后,6500转/分下强力搅拌2小时后,超声分散40分钟得到炭黑分散液;
所述1,2,4-丁三醇的加入量为去离子水质量的26%;
所述异辛醇磷酸酯钾盐的加入量为去离子水质量的2%;
所述月桂基磺化琥珀酸单酯二钠的加入量为去离子水质量的2%;
所述改性炭黑的加入量为去离子水质量的65%。
B、改性炭黑的制备:
强力搅拌下将炭黑加入强氧化剂溶液中,超声分散均匀后,加热搅拌反应完成后离心分离,得到的沉淀用去离子水洗涤三遍,然后烘干得到改性炭黑;
所述强力搅拌,搅拌速率为5000转/分;
所述炭黑,粒径95nm;
所述炭黑与强氧化剂溶液的质量比为5:8;
所述强氧化剂溶液,由H2XeO4、Na2S2O8、双氧水组成;
所述H2XeO4、Na2S2O8、双氧水的质量比为2:3:10;
所述双氧水,H2O2的浓度为30wt%;
所述超声分散,超声时间45分钟;
所述加热搅拌反应,温度为90℃,搅拌速率为1500转/分,反应时间5小时;
C、化学复合镀的镀液配制工艺:
按配方中各原料重量份,将NiSO4·6H2O、NiCl2·6H2O、NaH2PO2·H2O、
H3BO4、柠檬酸三铵、CH4N2S、C2H10BN、C12H25SO4Na、仲烷基磺酸钠加入到去离子水中,搅拌溶解后,将搅拌速率提升至3500转/分,缓慢加入炭黑分散液,强烈搅拌1.5小时后得到均一稳定的镀液。
(2)施镀
控制搅拌速率400转/分,镀液温度95℃下,将热镀锌处理后的碳钢件全部浸入镀液中,施镀90分钟,然后取出用去离子水清洗并吹干,得到含炭黑镀层的碳钢件。
耐酸碱腐蚀性测试:
从实施例1、2、3得到的碳钢镀件上取4cm×2cm的试样,试样上无镀层的横截面用耐腐蚀的环氧胶密封,然后分别放入5wt%的硫酸水溶液中浸泡15小时,放入6.5wt%的氢氧化钠溶液浸泡120小时,通过测量浸泡前后的重量变化,计算腐蚀速率,计算公式为V腐蚀速率=(M前-M后)/ST,其中V腐蚀速率的单位为g/m2·h,M前为腐蚀前试样的质量,M后为腐蚀后试样的质量,S为试样的浸泡表面积,单位m2,T为腐蚀时间,单位h,测试结果见表1;
表1
耐中性盐雾测试:
从实施例1、2、3得到的碳钢镀件上取15cm×10cm的试样,放于盐雾箱中,盐雾箱内温度控制在35±1℃,用5±0.2wt%浓度的氯化钠溶液连续喷雾1300小时,记录碳钢镀件表面开始出现肉眼可见锈点的时间,测试结果见表2;
表2
镀层结合力测试:
1、采用弯曲法测试时,弯曲角度超过90°,实施例1、2、3得到的碳钢镀件分别弯曲67次、58次、54次,镀层表面才出现折痕;
2、采用热震法时,将实施例1、2、3得到的碳钢镀件放入马弗炉中加热到200℃,保温30分钟后,取出试样立即投入水中骤冷,实施例1、2、3得到的镀件分别经过36次、29次、32次循环后,表面镀层才开始出现起皮脱落现象。
Claims (6)
1.一种碳钢表面的复合镀方法,其特征在于:包括热镀锌处理和化学复合镀处理;所述化学复合镀处理,包括化学复合镀的镀液配制和施镀;
所述化学复合镀的镀液,以重量份计,包括20~28份NiSO4·6H2O、12~20份NiCl2·6H2O、20~33份NaH2PO2·H2O、9~15份H3BO4、10~16份柠檬酸三铵、6~11份CH4N2S、2~4.5份C2H10BN、1.5~2.5份C12H25SO4Na、0.5~1.5份仲烷基磺酸钠、38~56份炭黑分散液、70~95份去离子水;
所述炭黑分散液的制备方法为将1,2,4-丁三醇、异辛醇磷酸酯钾盐、月桂基磺化琥珀酸单酯二钠溶解于去离子水中,加入改性炭黑后,4500~6500转/分下搅拌1~2小时后,超声分散15~40分钟得到;
所述改性炭黑的制备方法为强力搅拌下将炭黑加入强氧化剂溶液中,超声分散均匀后,加热搅拌反应完成后离心分离,得到的沉淀用去离子水洗涤三遍,然后烘干得到改性炭黑;
所述强氧化剂溶液,由H2XeO4、Na2S2O8、双氧水组成;
所述热镀锌处理,碳钢件热镀锌后水冷至室温,吹干后浸入60~75℃钝化液中,浸渍35~65分钟后提出镀件,去离子水冲洗干净后吹干,得到表面镀锌件;
所述钝化液,由锡酸钠、高铁酸钠、次氯酸钠、高锰酸钾、去离子水按质量比4~7:5~8:1~3:3~5:23~40组成。
2.根据权利要求1所述的一种碳钢表面的复合镀方法,其特征在于:所述1,2,4-丁三醇的加入量为去离子水质量的15~26%;所述异辛醇磷酸酯钾盐的加入量为去离子水质量的1~2%;所述月桂基磺化琥珀酸单酯二钠的加入量为去离子水质量的0.5~2%;所述改性炭黑的加入量为去离子水质量的50~65%。
3.根据权利要求1所述的一种碳钢表面的复合镀方法,其特征在于:所述炭黑,粒径30~95nm;所述炭黑与强氧化剂溶液的质量比为2~5:8;所述H2XeO4、Na2S2O8、双氧水的质量比为1~4:3~6:15~20;所述双氧水,H2O2的浓度为20~30wt%。
4.根据权利要求1所述的一种碳钢表面的复合镀方法,其特征在于:所述强力搅拌,搅拌速率为4000~5000转/分;所述超声分散,超声时间25~45分钟;所述加热搅拌反应,温度为80~90℃,搅拌速率为1200~1500转/分,反应时间2~5小时。
5.根据权利要求1所述的一种碳钢表面的复合镀方法,其特征在于:所述化学复合镀的镀液配制,按配方中各原料重量份,将NiSO4·6H2O、NiCl2·6H2O、NaH2PO2·H2O、H3BO4、柠檬酸三铵、CH4N2S、C2H10BN、C12H25SO4Na、仲烷基磺酸钠加入到去离子水中,搅拌溶解后,将搅拌速率提升至2500~3500转/分,缓慢加入炭黑分散液,强烈搅拌0.5~1.5小时后得到均一稳定的镀液。
6.根据权利要求1所述的一种碳钢表面的复合镀方法,其特征在于:所述施镀,控制搅拌速率150~400转/分,镀液温度85~95℃下,将热镀锌处理后的碳钢件全部浸入镀液中,施镀40~90分钟,然后取出用去离子水清洗并吹干,得到含炭黑镀层的碳钢件。
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070237957A1 (en) * | 2005-11-15 | 2007-10-11 | Meisei Industrial Company Limited | Composite plated film, a manufacturing method thereof, laminated films, films for metals used in the dark, a method of preventing corrosion of metal in the dark and composite films |
CN103276377A (zh) * | 2013-05-27 | 2013-09-04 | 四川理工学院 | 一种具有纳米孔结构的超黑涂层制备方法 |
CN103806078A (zh) * | 2012-11-08 | 2014-05-21 | 新光电气工业株式会社 | 散热部件及其制造方法 |
CN105603399A (zh) * | 2016-01-08 | 2016-05-25 | 华北理工大学 | 低碳钢表面化学镀Ni-Zn-P/纳米SiO2复合镀层的制备工艺 |
CN106958013A (zh) * | 2017-03-24 | 2017-07-18 | 东北电力大学 | 一种化学镀Ni‑P‑PTFE复合镀层制备工艺 |
-
2022
- 2022-02-24 CN CN202210169012.1A patent/CN114231874B/zh active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070237957A1 (en) * | 2005-11-15 | 2007-10-11 | Meisei Industrial Company Limited | Composite plated film, a manufacturing method thereof, laminated films, films for metals used in the dark, a method of preventing corrosion of metal in the dark and composite films |
CN103806078A (zh) * | 2012-11-08 | 2014-05-21 | 新光电气工业株式会社 | 散热部件及其制造方法 |
CN103276377A (zh) * | 2013-05-27 | 2013-09-04 | 四川理工学院 | 一种具有纳米孔结构的超黑涂层制备方法 |
CN105603399A (zh) * | 2016-01-08 | 2016-05-25 | 华北理工大学 | 低碳钢表面化学镀Ni-Zn-P/纳米SiO2复合镀层的制备工艺 |
CN106958013A (zh) * | 2017-03-24 | 2017-07-18 | 东北电力大学 | 一种化学镀Ni‑P‑PTFE复合镀层制备工艺 |
Non-Patent Citations (1)
Title |
---|
杨建明 等: "轻质环氧树脂/镀镍碳纤维/乙炔炭黑", 《塑料工业》 * |
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