CN111441041A - 基于化学镀镍和电镀锡的管式瓷介电容电极制作方法 - Google Patents
基于化学镀镍和电镀锡的管式瓷介电容电极制作方法 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 239000000919 ceramic Substances 0.000 title claims abstract description 98
- 238000007747 plating Methods 0.000 title claims abstract description 92
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 64
- 239000000126 substance Substances 0.000 title claims abstract description 56
- 239000003990 capacitor Substances 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 80
- 230000004913 activation Effects 0.000 claims abstract description 42
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 26
- 230000008719 thickening Effects 0.000 claims abstract description 13
- 230000003213 activating effect Effects 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 60
- 229910052573 porcelain Inorganic materials 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 29
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 19
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 18
- 229910052763 palladium Inorganic materials 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000001856 Ethyl cellulose Substances 0.000 claims description 9
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 9
- 238000009713 electroplating Methods 0.000 claims description 9
- 229920001249 ethyl cellulose Polymers 0.000 claims description 9
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 9
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 9
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 6
- JALQQBGHJJURDQ-UHFFFAOYSA-L bis(methylsulfonyloxy)tin Chemical compound [Sn+2].CS([O-])(=O)=O.CS([O-])(=O)=O JALQQBGHJJURDQ-UHFFFAOYSA-L 0.000 claims description 6
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229940116411 terpineol Drugs 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 238000007788 roughening Methods 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 7
- 239000004332 silver Substances 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- 238000009413 insulation Methods 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000003860 storage Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 3
- 206010070834 Sensitisation Diseases 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical class [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
Classifications
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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
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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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
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- 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
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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
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—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
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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
- C23C28/023—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 only coatings of metal elements only
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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- H01G4/002—Details
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Abstract
本发明公开了一种基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,包括以下步骤:对挤制或干压成型后烧制的瓷管进行粗化;高温活化;次亚磷酸钠溶液活化;化学预镀镍;第一次盐酸活化;化学镀镍;第二次盐酸活化;加厚镀镍;电镀锡处理;磨掉两端端头,露出瓷基体;检查和电性能测试,完成管式瓷介电容电极的制作。本发明采用特定工艺流程制作管式瓷介电容的电极,得到的产品完全满足耐电压、绝缘电阻、电容量、介质损耗角正切、可焊性和结合力等性能参数需求,产品质量高、寿命长,而且因为不用手工涂银而提高了生产效率,节约了生产成本;本发明尤其适合C型管式瓷介电容电极的制作。
Description
技术领域
本发明涉及一种材料为钛酸盐系列陶瓷的管式瓷介电容电极制作方法,尤其涉及一种基于化学镀镍和电镀锡的管式瓷介电容电极制作方法。
背景技术
瓷介电容器就是介质材料为陶瓷的电容器,根据陶瓷材料的不同,可分为低频瓷介电容器和高频瓷介电容器;按结构形式分类,又分为圆片状电容器、管状电容器、矩形电容器、穿心电容器等,其端电极的制备通常采用涂覆银浆再烧结的工艺方法。
传统管式瓷介电容的电极大都采用手工涂银(或钯银)后进行烧渗的工艺进行制作,为达到产品性能要求,一般需进行三次涂银、三次烧结。该工艺存在如下缺陷:需用大量的贵金属银或钯,制备一批产品所需的工艺时间长;同一产品的容量,与涂覆的面积息息相关,因此,由于人为因素,产品涂覆后的容量均一性差别较大;另外对于短且小的瓷管,涂覆操作更难。
目前,另一种电极制作工艺就是对陶瓷材料采用化学镀的方式。化学镀是在不通电的情况下,利用氧化还原反应在具有催化表面的镀件上,获得金属镀层的方法,比如化学镀镍是用还原剂把溶液中的镍离子还原沉积在具有催化活性的表面上。化学镀不仅可以在金属表面施镀,通过特殊的粗化、敏化、活化化学处理,也可以在非金属表面上进行,化学镀层厚度均匀,镀液稳定易控。
目前,针对氧化铝系列陶瓷,其电极采用的是“粗化-敏化-活化-化学镀镍-热处理”的工艺进行镀镍制作,但是对于钛酸钡系列的管式瓷介电容,则难以采用此工艺制作电极,因镍层可焊性较锡差,且保存时间不够长,因此在镍层上需再进行电镀锡,以满足产品可焊性能和长时间保存的要求,然而采用上述工艺镀镍后,需要热处理提高镍镀层与陶瓷之间结合力,而热处理后的镍镀层表面氧化层严重影响电镀锡。
另外,也有采用“涂银打底-化学镀镍-电镀锡”的工艺制作管式瓷介电容电极的,但该工艺制作流程也较长且不经济。
发明内容
本发明的目的就在于为了解决上述问题而提供一种基于化学镀镍和电镀锡的管式瓷介电容电极制作方法。
本发明通过以下技术方案来实现上述目的:
一种基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,包括以下步骤:
步骤1、对挤制或干压成型后烧制的瓷管进行粗化;
步骤2、对粗化后的瓷管进行高温活化;
步骤3、对高温活化后的瓷管进行次亚磷酸钠溶液活化;
步骤4、对次亚磷酸钠溶液活化后的瓷管进行化学预镀镍;
步骤5、对化学预镀镍后的瓷管进行第一次盐酸活化;
步骤6、对第一次盐酸活化后的瓷管进行化学镀镍;
步骤7、对化学镀镍后的瓷管进行第二次盐酸活化;
步骤8、对第二次盐酸活化后的瓷管进行加厚镀镍;
步骤9、对加厚镀镍后的瓷管进行电镀锡处理;
步骤10、对电镀锡处理后的瓷管两端端头磨掉至容量和产品尺寸要求范围,露出瓷基体,而后进行清洗和干燥;
步骤11、对磨掉端头后的瓷管进行检查和电性能测试后,完成管式瓷介电容电极的制作。
作为优选,所述步骤1的具体方法是:将挤制或干压成型后烧制的瓷管浸入浓度为(5~10)%的氢氟酸中,浸泡时间为(10~15)min,并不时进行搅拌翻浸,以使瓷管内外表面粗化均匀,然后将瓷管取出水洗,再进行酒精脱水并干燥,完成粗化。
作为优选,所述步骤2的具体方法是:将粗化后的瓷管浸入钯浆料中,搅拌翻浸(1~5)min,使瓷管内外表面均匀浸上钯浆料,然后放入(80~120)℃的烘箱中烘干,再将烘干后的瓷管放入(600~700)℃的马弗炉中灼烧(10~30)min,取出后完成高温活化;所述钯浆料包括如下重量比的各组分:乙基纤维素(2~10)%,松油醇(30~45)%,乙二醇乙醚(20~40)%,混合油酸(0.2~1)%,氯化钯(1~2)%,体积比为1:1的盐酸溶液(5~20)%,聚乙二醇(5~20)%;所述钯浆料的配制方法为:称量好乙基纤维素和松油醇,于(30~40)℃保温约(6~10)h,溶解,再加入乙二醇乙醚、混合油酸,于球磨机中研磨40h以上,配制成乙基纤维素混合液;而后向上述混合液中加入采用体积比为1:1的盐酸溶解的氯化钯液、聚乙二醇,继续于球磨机中球磨48h以上,配制成钯浆料。
作为优选,所述步骤3的具体方法是:将高温活化后的瓷管浸入浓度为(10~40)g/L的次亚磷酸钠溶液,搅拌翻浸(3~5)min后取出,完成次亚磷酸钠溶液活化。
作为优选,所述步骤4的具体方法是:将次亚磷酸钠溶液活化后的瓷管浸入温度为(50~70)℃的化学预镀镍溶液中,翻浸(5~10)min后取出水洗,水洗后取出完成化学预镀镍;所述化学预镀镍液以水为溶剂且包括以下含量的各原料:硫酸镍(10~30)g/L、次亚磷酸钠(10~30)g/L。
作为优选,所述步骤5的具体方法是:将化学预镀镍后的瓷管置于浓度为(5~15)%的盐酸溶液中活化,时间不超过5min,而后取出水洗,水洗后取出完成第一次盐酸活化。
作为优选,所述步骤6的具体方法是:将第一次盐酸活化后的瓷管浸入温度为(80~90)℃的化学镀镍溶液中,翻浸时间不少于30min,然后取出水洗,水洗后取出完成化学镀镍;所述化学镀镍溶液以水为溶剂,以水为溶剂且包括以下含量的各原料:硫酸镍(30~50)g/L、次亚磷酸钠(10~30)g/L、乙酸钠(8~15)g/L。
作为优选,所述步骤7的具体方法是:将化学镀镍后的瓷管置于浓度为(5~15)%的盐酸溶液中活化,时间不超过3min,而后取出水洗,水洗后取出完成第二次盐酸活化。
作为优选,所述步骤8的具体方法是:将第二次盐酸活化后的瓷管浸入温度为(80~90)℃的加厚镀镍溶液中,翻浸一定时间,该翻浸时间加上化学镀镍时间不少于2h,然后取出水洗,水洗后取出完成加厚镀镍;所述加厚镀镍溶液以水为溶剂且包括以下含量的各原料:硫酸镍(30~40)g/L、次亚磷酸钠(10~30)g/L、柠檬酸三钠(8~15)g/L。
作为优选,所述步骤9的具体方法是:首先,对加厚镀镍后的瓷管用浓度为(100~150)g/L的甲磺酸活化;然后进行哑光电镀纯锡,即将甲磺酸活化后的瓷管置于镀液中电镀,电镀条件为:电流密度为(0.2~0.5)A/dm2,温度为室温,完成电镀后取出,完成电镀锡处理;所述镀液包括以下含量的各原料:甲磺酸亚锡(10~20)g/L、甲磺酸(100~150)g/L、添加剂(15~20)ml/L。
本发明的有益效果在于:
本发明采用“粗化-高温活化-次亚磷酸钠溶液活化-化学预镀镍-第一次盐酸活化-化学镀镍-第二次盐酸活化-加厚镀镍-电镀锡处理-磨掉端头-性能测试”的工艺流程制作管式瓷介电容的电极,通过对瓷管进行高温活化,使后续化学镀镍层与瓷管有良好的结合力,从而确保耐电压、绝缘电阻、电容量、介质损耗角正切等性能参数测试结果达到产品要求;由于镀镍层可焊性会随着保存时间的延长而快速下降,再加之如果瓷管焊接性能差,产品在焊接装配后的性能(耐电压、绝缘电阻、电容量、介质损耗角正切、结合力等)会受到严重影响,所以本发明在镍层上再电镀锡,使产品具有良好可焊性,同时满足产品保存期限和其它性能参数的要求;另外,因为不用手工涂银而提高了生产效率,节约了生产成本;本发明尤其适合C型管式瓷介电容电极的制作。
具体实施方式
下面结合实施例对本发明作进一步说明:
实施例:
一种基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,包括以下步骤:
步骤1、对挤制或干压成型后烧制的瓷管进行粗化,具体方法是:将挤制或干压成型后烧制的瓷管浸入浓度为(5~10)%的氢氟酸中,浸泡时间为(10~15)min,并不时进行搅拌翻浸,以使瓷管内外表面粗化均匀,然后将瓷管取出水洗,再进行酒精脱水并干燥,完成粗化。
步骤2、对粗化后的瓷管进行高温活化,具体方法是:将粗化后的瓷管浸入钯浆料中,搅拌翻浸(1~5)min,使瓷管内外表面均匀浸上钯浆料,然后放入(80~120)℃的烘箱中烘干,再将烘干后的瓷管放入(600~700)℃的马弗炉中灼烧(10~30)min,取出后完成高温活化;所述钯浆料包括如下重量比的各组分:乙基纤维素(2~10)%,松油醇(30~45)%,乙二醇乙醚(20~40)%,混合油酸(0.2~1)%,氯化钯(1~2)%,体积比为1:1的盐酸溶液(5~20)%,聚乙二醇(5~20)%;所述钯浆料的配制方法为:称量好乙基纤维素和松油醇,于(30~40)℃保温约(6~10)h,溶解,再加入乙二醇乙醚、混合油酸,于球磨机中研磨40h以上,配制成乙基纤维素混合液;而后向上述混合液中加入采用体积比为1:1的盐酸溶解的氯化钯液、聚乙二醇,继续于球磨机中球磨48h以上,配制成钯浆料。
步骤3、对高温活化后的瓷管进行次亚磷酸钠溶液活化,具体方法是:将高温活化后的瓷管浸入浓度为(10~40)g/L的次亚磷酸钠溶液,搅拌翻浸(3~5)min后取出,完成次亚磷酸钠溶液活化。
步骤4、对次亚磷酸钠溶液活化后的瓷管进行化学预镀镍,具体方法是:将次亚磷酸钠溶液活化后的瓷管浸入温度为(50~70)℃的化学预镀镍溶液中,翻浸(5~10)min后取出水洗,水洗后取出完成化学预镀镍;所述化学预镀镍液以水为溶剂且包括以下含量的各原料:硫酸镍(10~30)g/L、次亚磷酸钠(10~30)g/L。
步骤5、对化学预镀镍后的瓷管进行第一次盐酸活化,具体方法是:将化学预镀镍后的瓷管置于浓度为(5~15)%的盐酸溶液中活化,时间不超过5min,而后取出水洗,水洗后取出完成第一次盐酸活化。
步骤6、对第一次盐酸活化后的瓷管进行化学镀镍,具体方法是:将第一次盐酸活化后的瓷管浸入温度为(80~90)℃的化学镀镍溶液中,翻浸时间不少于30min,然后取出水洗,水洗后取出完成化学镀镍;所述化学镀镍溶液以水为溶剂,以水为溶剂且包括以下含量的各原料:硫酸镍(30~50)g/L、次亚磷酸钠(10~30)g/L、乙酸钠(8~15)g/L。
步骤7、对化学镀镍后的瓷管进行第二次盐酸活化,具体方法是:将化学镀镍后的瓷管置于浓度为(5~15)%的盐酸溶液中活化,时间不超过3min,而后取出水洗,水洗后取出完成第二次盐酸活化。
步骤8、对第二次盐酸活化后的瓷管进行加厚镀镍,具体方法是:将第二次盐酸活化后的瓷管浸入温度为(80~90)℃的加厚镀镍溶液中,翻浸一定时间,该翻浸时间加上化学镀镍时间不少于2h,然后取出水洗,水洗后取出完成加厚镀镍;所述加厚镀镍溶液以水为溶剂且包括以下含量的各原料:硫酸镍(30~40)g/L、次亚磷酸钠(10~30)g/L、柠檬酸三钠(8~15)g/L。
步骤9、对加厚镀镍后的瓷管进行电镀锡处理,具体方法是:首先,对加厚镀镍后的瓷管用浓度为(100~150)g/L的甲磺酸活化;然后进行哑光电镀纯锡,即将甲磺酸活化后的瓷管置于镀液中电镀,电镀条件为:电流密度为(0.2~0.5)A/dm2,温度为室温,完成电镀后取出,完成电镀锡处理;所述镀液包括以下含量的各原料:甲磺酸亚锡(10~20)g/L、甲磺酸(100~150)g/L、添加剂(15~20)ml/L。
步骤10、对电镀锡处理后的瓷管两端端头磨掉至容量和产品尺寸要求范围,露出瓷基体,而后进行清洗和干燥。
步骤11、对磨掉端头后的瓷管进行检查和电性能测试后,完成管式瓷介电容电极的制作。
上述各步骤中,具体的方法流程参数和溶液浓度、含量等可以根据实际需要在上述各对应限定范围内进行选择,在此不一一列举。
上述实施例只是本发明的较佳实施例,并不是对本发明技术方案的限制,只要是不经过创造性劳动即可在上述实施例的基础上实现的技术方案,均应视为落入本发明专利的权利保护范围内。
Claims (10)
1.一种基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:包括以下步骤:
步骤1、对挤制或干压成型后烧制的瓷管进行粗化;
步骤2、对粗化后的瓷管进行高温活化;
步骤3、对高温活化后的瓷管进行次亚磷酸钠溶液活化;
步骤4、对次亚磷酸钠溶液活化后的瓷管进行化学预镀镍;
步骤5、对化学预镀镍后的瓷管进行第一次盐酸活化;
步骤6、对第一次盐酸活化后的瓷管进行化学镀镍;
步骤7、对化学镀镍后的瓷管进行第二次盐酸活化;
步骤8、对第二次盐酸活化后的瓷管进行加厚镀镍;
步骤9、对加厚镀镍后的瓷管进行电镀锡处理;
步骤10、对电镀锡处理后的瓷管两端端头磨掉至容量和产品尺寸要求范围,露出瓷基体,而后进行清洗和干燥;
步骤11、对磨掉端头后的瓷管进行检查和电性能测试后,完成管式瓷介电容电极的制作。
2.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤1的具体方法是:将挤制或干压成型后烧制的瓷管浸入浓度为(5~10)%的氢氟酸中,浸泡时间为(10~15)min,并不时进行搅拌翻浸,以使瓷管内外表面粗化均匀,然后将瓷管取出水洗,再进行酒精脱水并干燥,完成粗化。
3.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤2的具体方法是:将粗化后的瓷管浸入钯浆料中,搅拌翻浸(1~5)min,使瓷管内外表面均匀浸上钯浆料,然后放入(80~120)℃的烘箱中烘干,再将烘干后的瓷管放入(600~700)℃的马弗炉中灼烧(10~30)min,取出后完成高温活化;所述钯浆料包括如下重量比的各组分:乙基纤维素(2~10)%,松油醇(30~45)%,乙二醇乙醚(20~40)%,混合油酸(0.2~1)%,氯化钯(1~2)%,体积比为1:1的盐酸溶液(5~20)%,聚乙二醇(5~20)%;所述钯浆料的配制方法为:称量好乙基纤维素和松油醇,于(30~40)℃保温约(6~10)h,溶解,再加入乙二醇乙醚、混合油酸,于球磨机中研磨40h以上,配制成乙基纤维素混合液;而后向上述混合液中加入采用体积比为1:1的盐酸溶解的氯化钯液、聚乙二醇,继续于球磨机中球磨48h以上,配制成钯浆料。
4.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤3的具体方法是:将高温活化后的瓷管浸入浓度为(10~40)g/L的次亚磷酸钠溶液,搅拌翻浸(3~5)min后取出,完成次亚磷酸钠溶液活化。
5.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤4的具体方法是:将次亚磷酸钠溶液活化后的瓷管浸入温度为(50~70)℃的化学预镀镍溶液中,翻浸(5~10)min后取出水洗,水洗后取出完成化学预镀镍;所述化学预镀镍液以水为溶剂且包括以下含量的各原料:硫酸镍(10~30)g/L、次亚磷酸钠(10~30)g/L。
6.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤5的具体方法是:将化学预镀镍后的瓷管置于浓度为(5~15)%的盐酸溶液中活化,时间不超过5min,而后取出水洗,水洗后取出完成第一次盐酸活化。
7.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤6的具体方法是:将第一次盐酸活化后的瓷管浸入温度为(80~90)℃的化学镀镍溶液中,翻浸时间不少于30min,然后取出水洗,水洗后取出完成化学镀镍;所述化学镀镍溶液以水为溶剂,以水为溶剂且包括以下含量的各原料:硫酸镍(30~50)g/L、次亚磷酸钠(10~30)g/L、乙酸钠(8~15)g/L。
8.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤7的具体方法是:将化学镀镍后的瓷管置于浓度为(5~15)%的盐酸溶液中活化,时间不超过3min,而后取出水洗,水洗后取出完成第二次盐酸活化。
9.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤8的具体方法是:将第二次盐酸活化后的瓷管浸入温度为(80~90)℃的加厚镀镍溶液中,翻浸一定时间,该翻浸时间加上化学镀镍时间不少于2h,然后取出水洗,水洗后取出完成加厚镀镍;所述加厚镀镍溶液以水为溶剂且包括以下含量的各原料:硫酸镍(30~40)g/L、次亚磷酸钠(10~30)g/L、柠檬酸三钠(8~15)g/L。
10.根据权利要求1所述的基于化学镀镍和电镀锡的管式瓷介电容电极制作方法,其特征在于:所述步骤9的具体方法是:首先,对加厚镀镍后的瓷管用浓度为(100~150)g/L的甲磺酸活化;然后进行哑光电镀纯锡,即将甲磺酸活化后的瓷管置于镀液中电镀,电镀条件为:电流密度为(0.2~0.5)A/dm2,温度为室温,完成电镀后取出,完成电镀锡处理;所述镀液包括以下含量的各原料:甲磺酸亚锡(10~20)g/L、甲磺酸(100~150)g/L、添加剂(15~20)ml/L。
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CN115175466A (zh) * | 2022-07-04 | 2022-10-11 | 江苏富乐华半导体科技股份有限公司 | 一种提升陶瓷覆铜基板表面电镀锡镍合金的焊接方法 |
CN115175466B (zh) * | 2022-07-04 | 2023-06-06 | 江苏富乐华半导体科技股份有限公司 | 一种提升陶瓷覆铜基板表面电镀锡镍合金的焊接方法 |
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