CN117070956A - 一种金属-陶瓷封装外壳的电镀前处理方法 - Google Patents
一种金属-陶瓷封装外壳的电镀前处理方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 108
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 82
- 238000009713 electroplating Methods 0.000 title claims abstract description 24
- 238000002203 pretreatment Methods 0.000 title claims description 8
- 238000000034 method Methods 0.000 claims abstract description 47
- 239000000243 solution Substances 0.000 claims description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 52
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- 230000001590 oxidative effect Effects 0.000 claims description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 23
- 238000004140 cleaning Methods 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- 238000007747 plating Methods 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 18
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 12
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 12
- GYBINGQBXROMRS-UHFFFAOYSA-J tetrasodium;2-(1,2-dicarboxylatoethylamino)butanedioate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CC(C([O-])=O)NC(C([O-])=O)CC([O-])=O GYBINGQBXROMRS-UHFFFAOYSA-J 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 8
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 7
- 239000011790 ferrous sulphate Substances 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 6
- 229940117975 chromium trioxide Drugs 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 6
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims description 6
- 239000008139 complexing agent Substances 0.000 claims description 6
- 150000002815 nickel Chemical class 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 3
- 229940061605 tetrasodium glutamate diacetate Drugs 0.000 claims description 3
- UZVUJVFQFNHRSY-OUTKXMMCSA-J tetrasodium;(2s)-2-[bis(carboxylatomethyl)amino]pentanedioate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CC[C@@H](C([O-])=O)N(CC([O-])=O)CC([O-])=O UZVUJVFQFNHRSY-OUTKXMMCSA-J 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 2
- 229940080258 tetrasodium iminodisuccinate Drugs 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 2
- WZSWPMDIARCYDN-UHFFFAOYSA-N copper;oxosilver Chemical compound [Ag].[Cu]=O WZSWPMDIARCYDN-UHFFFAOYSA-N 0.000 abstract description 12
- 239000011248 coating agent Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 239000006260 foam Substances 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 238000005507 spraying Methods 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 229910000833 kovar Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- LJRGBERXYNQPJI-UHFFFAOYSA-M sodium;3-nitrobenzenesulfonate Chemical compound [Na+].[O-][N+](=O)C1=CC=CC(S([O-])(=O)=O)=C1 LJRGBERXYNQPJI-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Classifications
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- 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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
-
- 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
- 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
- C23C22/05—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
- C23C22/06—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 acidic solutions with pH less than 6
- C23C22/24—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 acidic solutions with pH less than 6 containing hexavalent chromium compounds
-
- 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
- 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
- C23C22/05—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
- C23C22/06—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 acidic solutions with pH less than 6
- C23C22/24—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 acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/26—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 acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also organic compounds
- C23C22/27—Acids
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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
- 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
- C23C22/05—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
- C23C22/06—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 acidic solutions with pH less than 6
- C23C22/24—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 acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/33—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 acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also phosphates
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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
- 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
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
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- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/103—Other heavy metals copper or alloys of copper
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Abstract
本发明属于表面处理技术领域,具体公开了一种金属‑陶瓷封装外壳的电镀前处理方法。本发明利用氧化,还原,一次水洗,酸浸,二次水洗的操作,重复多次可以将银铜氧化层与合金焊料进行分离,达到去除合金焊料中银铜氧化层的目的,本发明的电镀前处理方法操作简便、工序简单,成本低廉,处理时间短,所得镀层均匀平滑且致密,结合力强,可焊性高,有效解决了现有技术中所用处理液在处理银铜氧化层时容易与其他部位发生反应,易发生残留,处理液处理效果较差,所得镀层不均匀,易起皮起泡,且操作时间长,工序复杂,成本高的问题。
Description
技术领域
本发明属于表面处理技术领域,具体公开了一种金属-陶瓷封装外壳的电镀前处理方法。
背景技术
随着近年集成电路技术的迅猛发展,工艺逐步成熟,金属-陶瓷这种形式的封装外壳得到了越来越多的应用,其封装体可靠性高,导热性能好,同时具有优秀的电性能,可实现多层布线,并具有对复杂器件进行一体化封装的能力。金属-陶瓷封装外壳主要组成部分为底座、墙体、引线、陶瓷件及焊料,这些组成部件在石墨模具中装载成型,再经高温扩散炉进行焊接。但是石墨模具耐磨性差,金属-陶瓷封装外壳在焊接过程中易粘附石墨,为避免石墨对外壳性能和可靠性产生影响,通常会对粘附的石墨采取化学氧化加物理轰击的方法去除,但是在去除石墨过程中焊接位置的银铜合金会发生氧化,生成一层较厚的氧化膜,这层氧化膜会导致外壳电镀后出现镀层颜色不一致、粗糙、起皮、起泡等缺陷,严重影响外壳镀层的可靠性,因此需要一种方法将该银铜氧化膜去除,但在去除氧化膜的同时保证外壳其它组成部分如可伐合金、氧化铝陶瓷、镍镀层等不受影响。
现有技术中多采用液体去除法,使用的处理液是浓硝酸、冰乙酸、浓硫酸、浓盐酸其中一种或几种,再添加一些缓蚀剂的溶液,但该方法存在以下缺陷:①在处理银铜氧化层的同时,对外壳其它部位如可伐合金也发生反应,影响材料可靠性;②溶液处理效果较差,易产生残留,所得镀层结合力低,可焊性差;③废液处理工艺处理时间长,操作复杂,成本高。因此,研发一种可将金属-陶瓷封装外壳底座中的银铜氧化层完全剥离,且不会对可伐合金产生腐蚀,废液处理简单,操作简便、成本较低的处理方法对于金属-陶瓷封装外壳的发展有重大意义。
发明内容
针对现有技术中,所用处理液在处理银铜氧化层时容易与其他部位发生反应,易发生残留,处理液处理效果较差,所得镀层不均匀,易起皮起泡,结合力低、可焊性差,且操作时间长,工序复杂,成本高的问题。本发明提供了一种金属-陶瓷封装外壳的电镀前处理方法,利用氧化,还原,一次水洗,酸浸,二次水洗的操作,重复多次可以将银铜氧化层与合金基体进行分离,达到去除氧化物的目的,此方法可提升金属-陶瓷封装外壳后续电镀工艺的表面状态一致性和可靠性。
为达到上述发明目的,本发明提供了如下的技术方案:
本发明第一方面提供了一种金属-陶瓷封装外壳的电镀前处理方法,所述前处理方法,包括如下步骤:
步骤一、将待处理金属-陶瓷封装外壳浸渍于氧化液中,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳浸渍于还原液中,得第二处理金属-陶瓷封装外壳;
步骤三、将所述第二处理金属-陶瓷封装外壳经一次水洗、酸浸、二次水洗,得第三处理金属-陶瓷封装外壳;
步骤四、重复操作步骤一至步骤三2-5次,得处理后的金属-陶瓷封装外壳。
优选的,所述氧化液以体积为1L计,包括如下组分:1g-10g的铬氧化剂,1mL-10mL的酸、2g-10g的络合剂、1g-5g的镍盐和余量的水。
相比于现有技术,本发明提供了一种金属-陶瓷封装外壳的电镀前处理方法,结合氧化剥离和还原中和,将外壳焊接位置的银铜焊料表面上的氧化层去除,又对外壳其它组成部分无影响,处理效果好,所述金属-陶瓷封装外壳经处理后无浮灰残留,可靠性高,其中,所述氧化剥离过程中所用氧化液,由铬氧化剂、酸、络合剂和镍盐组成,与现有技术中单一的处理液不同,本发明以铬氧化剂为主要成分,用于浸蚀银铜氧化层,将银和铜转化为银离子和铜离子,达到剥离银铜氧化层的目的,在酸性环境中,可进一步促进铬氧化剂的浸蚀能力,而浸蚀过程中产生的杂质则与络合剂结合,形成络合物,保证氧化液的稳定性,镍盐的加入可保证强氧化剂不与其他部分发生反应,避免其他部位被腐蚀,在氧化剥离之后再通过还原中和的方式,中和外壳表面残留的氧化液,使所述金属-陶瓷封装外壳保持中性,避免对后续工艺产生干扰。
优选的,所述氧化液的制备方法包括如下步骤:按照设计配比称取各组分,将所述铬氧化剂溶解后依次加入酸、络合剂、镍盐,混合,加入余量的水,混合均匀,得氧化液。
优选的,所述铬氧化剂为高锰酸钾、重铬酸钾或三氧化铬中的一种或多种。
优选的,所述酸为浓硫酸、浓磷酸或冰醋酸中的一种或多种。
优选的,所述络合剂为谷氨酸二乙酸四钠或亚氨基二琥珀酸钠中的一种或两种。
优选的,所述镍盐为硫酸镍或氯化镍中的一种或两种。
优选的,所述还原液为质量浓度为10g/L-25g/L的硫酸亚铁溶液。
优选的,所述酸浸采用的酸性溶液的浓度为硫酸溶液、盐酸溶液、磷酸溶液或醋酸溶液中的一种或多种。
本发明为保证外壳表面残留氧化层被去除干净,又通过酸浸的方式对其进行处理,避免产生银铜氧化层残留,影响后续电镀镀层性能。
进一步优选的,所述酸性溶液的体积浓度为2mL/L-40mL/L。
优选的,步骤一中,所述金属-陶瓷封装外壳在氧化液中浸渍的温度为20℃-40℃,浸渍的时间为20s-60s。
优选的,步骤二中,所述金属-陶瓷封装外壳在还原液中浸渍的温度为20℃-40℃,浸渍的时间为10s-40s。
优选的,步骤三中,所述酸浸的时间为10s-40s。
优选的,步骤三中,所述一次水洗和二次水洗的具体操作均为将所述金属-陶瓷外壳放入去离子水中浸渍30s-60s,然后采用去离子水喷淋清洗30s-60s。
针对现有技术中,所用处理液在处理银铜氧化层时容易与其他部位发生反应,影响材料可靠性,且易发生残留,处理液处理效果较差,操作时间长,工序复杂,成本高的问题,本发明提供了一种金属-陶瓷封装外壳的电镀前处理方法,利用氧化,还原,一次水洗,酸浸,二次水洗的操作,重复多次可以将银铜氧化层与合金焊料进行分离,达到去除银铜氧化层的目的。本发明提供的电镀前处理方法可提升金属-陶瓷封装外壳后续电镀工艺的表面状态一致性和可靠性,且本发明所用处理方法操作简便,用时较短,成本较低,有效解决了现有技术中镀层不均匀,易起皮起泡以及镀层结合力低、可焊性差的技术问题。
附图说明
图1为未处理的金属-陶瓷封装外壳在形状轮廓测量显微镜下的照片;
图2为实施例1处理后的金属-陶瓷封装外壳在形状轮廓测量显微镜下的照片;
图3为对比例1处理后的金属-陶瓷封装外壳在形状轮廓测量显微镜下的照片。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合具体实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
实施例1
本实施例提供了一种金属-陶瓷封装外壳的电镀前处理方法,具体处理方法如下:
本实施例所述氧化液以体积为1L计,包括如下组分:10g的重铬酸钾,5mL的浓硫酸、5g的亚氨基二琥珀酸钠、3g的硫酸镍和余量的水;
所述还原液为质量浓度为20g/L的硫酸亚铁溶液;
所述氧化液的制备方法如下:按照设计配比称取各组分,将重铬酸钾溶解溶解后,边搅拌边加入浓硫酸,将体系降至室温后加入亚氨基二琥珀酸钠和硫酸镍,混合均匀后加入余量的水,混合均匀,得氧化液;
所述金属-陶瓷封装外壳的电镀前处理方法具体内容如下:
步骤一、将所述金属-陶瓷封装外壳完全浸渍于所述氧化液中,于30℃下浸渍30s,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳完全浸渍于所述还原液中,于30℃下浸渍20s,得第二处理金属-陶瓷封装外壳;
步骤三、将所述第二处理金属-陶瓷封装外壳放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,将清洗后的外壳放入10mL/L的硫酸溶液中浸洗30s,捞出后将所述外壳再次放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,得第三处理金属-陶瓷封装外壳;
步骤四、重复操作步骤一至步骤三4次,得处理后的金属-陶瓷封装外壳。
实施例2
本实施例提供了一种金属-陶瓷封装外壳的电镀前处理方法,具体处理方法如下:
本实施例所述氧化液以体积为1L计,包括如下组分:8g的三氧化铬,6mL的浓磷酸、5g的亚氨基二琥珀酸钠、3g的氯化镍和余量的水;
所述还原液为质量浓度为20g/L的硫酸亚铁溶液;
所述氧化液的制备方法如下:按照设计配比称取各组分,将三氧化铬溶解溶解后,边搅拌边加入浓磷酸,将体系降至室温后加入亚氨基二琥珀酸钠和氯化镍,混合均匀后加入余量的水,混合均匀,得氧化液;
所述金属-陶瓷封装外壳的电镀前处理方法具体内容如下:
步骤一、将所述金属-陶瓷封装外壳完全浸渍于所述氧化液中,于30℃下浸渍30s,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳完全浸渍于所述还原液中,于30℃下浸渍20s,得第二处理金属-陶瓷封装外壳;
步骤三、将所述第二处理金属-陶瓷封装外壳放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,将清洗后的外壳放入5mL/L的硫酸溶液中浸洗30s,捞出后将所述外壳再次放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,得第三处理金属-陶瓷封装外壳;
步骤四、重复步骤一和步骤三3次,得处理后的金属-陶瓷封装外壳。
实施例3
本实施例提供了一种金属-陶瓷封装外壳的电镀前处理方法,具体处理方法如下:
本实施例所述氧化液以体积为1L计,包括如下组分:10g的重铬酸钾,5mL的冰醋酸、5g的谷氨酸二乙酸四钠、3g的硫酸镍和余量的水;
所述还原液为质量浓度为15g/L的硫酸亚铁溶液;
所述氧化液的制备方法如下:按照设计配比称取各组分,将重铬酸钾溶解溶解后,边搅拌边加入冰醋酸,将体系降至室温后加入亚氨基二琥珀酸钠和硫酸镍,混合均匀后加入余量的水,混合均匀,得氧化液;
所述金属-陶瓷封装外壳的电镀前处理方法具体内容如下:
步骤一、将所述金属-陶瓷封装外壳完全浸渍于所述氧化液中,于30℃下浸渍30s,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳完全浸渍于所述还原液中,于30℃下浸渍20s,得第二处理金属-陶瓷封装外壳;
步骤三、将所述第二处理金属-陶瓷封装外壳放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,将清洗后的外壳放入15mL/L的硫酸溶液中浸洗30s,捞出后将所述外壳再次放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,得第三处理金属-陶瓷封装外壳;
步骤四、重复步骤一和步骤三4次,得处理后的金属-陶瓷封装外壳。
实施例4
本实施例提供了一种金属-陶瓷封装外壳的电镀前处理方法,具体处理方法如下:
本实施例所述氧化液以体积为1L计,包括如下组分:10g的三氧化铬,4mL的浓磷酸和1mL的浓硫酸、5g的亚氨基二琥珀酸钠、3g的硫酸镍和余量的水;
所述还原液为质量浓度为20g/L的硫酸亚铁溶液;
所述氧化液的制备方法如下:按照设计配比称取各组分,将三氧化铬溶解溶解后,边搅拌边加入浓磷酸和浓硫酸,将体系降至室温后加入亚氨基二琥珀酸钠和硫酸镍,混合均匀后加入余量的水,混合均匀,得氧化液;
所述金属-陶瓷封装外壳的电镀前处理方法具体内容如下:
步骤一、将所述金属-陶瓷封装外壳完全浸渍于所述氧化液中,于30℃下浸渍30s,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳完全浸渍于所述还原液中,于30℃下浸渍20s,得第二处理金属-陶瓷封装外壳;
步骤三、将所述第二处理金属-陶瓷封装外壳放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,将清洗后的外壳放入40mL/L的醋酸溶液中浸洗30s,捞出后将所述外壳再次放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,得第三处理金属-陶瓷封装外壳;
步骤四、重复步骤一和步骤三4次,得处理后的金属-陶瓷封装外壳。
实施例5
本实施例提供了一种金属-陶瓷封装外壳的电镀前处理方法,具体处理方法如下:
本实施例所述氧化液以体积为1L计,包括如下组分:10g的重铬酸钾,4mL的冰醋酸和1mL的浓硫酸、5g的亚氨基二琥珀酸钠、2.5g的硫酸镍和余量的水;
所述还原液为质量浓度为20g/L的硫酸亚铁溶液;
所述氧化液的制备方法如下:按照设计配比称取各组分,将重铬酸钾溶解溶解后,边搅拌边加入冰醋酸和浓硫酸,将体系降至室温后加入亚氨基二琥珀酸钠和硫酸镍,混合均匀后加入余量的水,混合均匀,得氧化液;
所述金属-陶瓷封装外壳的电镀前处理方法具体内容如下:
步骤一、将所述金属-陶瓷封装外壳完全浸渍于所述氧化液中,于30℃下浸渍30s,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳完全浸渍于所述还原液中,于30℃下浸渍30s,得第二处理金属-陶瓷封装外壳;
步骤三、将所述第二处理金属-陶瓷封装外壳放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,将清洗后的外壳放入20mL/L的盐酸溶液中浸洗30s,捞出后将所述外壳再次放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,得第三处理金属-陶瓷封装外壳;
步骤四、重复步骤一和步骤三4次,得处理后的金属-陶瓷封装外壳。
对比例1
本对比例采用现有技术中的处理液对金属-陶瓷封装外壳进行前处理,所用处理液包括如下组分:600mL/L的63-68wt%的硝酸,300mL/L的95-98wt%的硫酸和100g/L的3-硝基苯磺酸钠;
具体处理工艺如下:
步骤一、将所述金属-陶瓷封装外壳完全浸渍于所述处理液中,于30℃下浸渍30s,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,将清洗后的外壳放入20mL/L的盐酸溶液中浸洗30s,捞出后将所述外壳再次放入去离子水中浸渍60s,然后采用去离子水喷淋清洗30s,得第二处理金属-陶瓷封装外壳;
步骤三、重复步骤一和步骤二4次,得处理后的金属-陶瓷封装外壳。
对比例2
本对比例提供了一种金属-陶瓷封装外壳的电镀前处理方法,与实施例1相比,区别在于将10g重铬酸钾替换为10mL的过氧化氢,其它组分和制备工艺不变,此处不再赘述。
对比例3
本对比例提供了一种金属-陶瓷封装外壳的电镀前处理方法,与实施例1相比,区别在于将硫酸镍替换为等量的乙二胺四乙酸二钠,其它组分和制备工艺不变,此处不再赘述。
对比例4
本对比例提供了一种金属-陶瓷封装外壳的电镀前处理方法,与实施例1相比,区别在于将硫酸镍替换为等量的硫脲,其它组分和制备工艺不变,此处不再赘述。
本发明为了以进一步说明清洗效果,将1000片金属-陶瓷封装外壳经本发明实施例和对比例的处理方法处理后进行电镀镍、金,其中所得外观按照GJB1941-94中“3.8.12镀层外观质量”的要求进行测试,采用目视检验,也可借助四倍放大镜观察;结合力采取烘烤实验检验,烘烤条件为190±10℃,1h;可焊性采取GJB360.18中规定方法进行验证,所得电镀层的效果及电镀层的合格率如表1所示:
表1各实施例和对比例所得处理后的金属-陶瓷封装外壳电镀层的效果
根据表1可以看出,本发明实施例提供的金属-陶瓷封装外壳的电镀前处理方法可对所述外壳焊接位置的银铜氧化层进行处理,处理后的外壳在电镀电镀镍、金后,镀层表面均匀、平滑且镀层更为致密,结合力更强,在长时间的烘烤下也不会出现镀层剥落、起皮、起泡现象,符合GJB360.18规定的合格品要求。
所述实施例1和对比例1处理后的金属-陶瓷封装外壳的目视结果如图1所示,由图1可以看出,本发明实施例1进行处理后的外壳的表面光洁明亮,无银铜氧化层残留,其他部位保留完整,无腐蚀迹象,而对比例1进行处理后的外壳的表面有明显的银铜氧化层残留,其他部位被腐蚀。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换或改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种金属-陶瓷封装外壳的电镀前处理方法,其特征在于:所述前处理方法包括如下步骤:
步骤一、将待处理金属-陶瓷封装外壳浸渍于氧化液中,得第一处理金属-陶瓷封装外壳;
步骤二、将所述第一处理金属-陶瓷封装外壳浸渍于还原液中,得第二处理金属-陶瓷封装外壳;
步骤三、将所述第二处理金属-陶瓷封装外壳经一次水洗、酸浸、二次水洗,得第三处理金属-陶瓷封装外壳;
步骤四、重复操作步骤一至步骤三2-5次,得处理后的金属-陶瓷封装外壳;
其中,所述氧化液以体积为1L计,包括如下组分:1g-10g的铬氧化剂,1mL-10mL的酸、2g-10g的络合剂、1g-5g的镍盐和余量的水。
2.如权利要求1所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:所述氧化液的制备方法包括如下步骤:按照设计配比称取各组分,将所述铬氧化剂溶解后依次加入酸、络合剂、镍盐,混合,加入余量的水,混合均匀,得氧化液。
3.如权利要求1或2任一项所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:所述铬氧化剂为重铬酸钾或三氧化铬中的一种或两种;和/或
所述酸为浓硫酸、浓磷酸或冰醋酸中的一种或多种;和/或
所述络合剂为谷氨酸二乙酸四钠或亚氨基二琥珀酸钠中的一种或两种;和/或
所述镍盐为硫酸镍或氯化镍中的一种或两种。
4.如权利要求1所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:步骤二中,所述还原液为质量浓度为10g/L-25g/L的硫酸亚铁溶液。
5.如权利要求1所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:步骤三中,所述酸浸采用的酸性溶液为硫酸溶液、盐酸溶液、磷酸溶液或醋酸溶液中的一种或多种。
6.如权利要求5所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:所述酸性溶液的体积浓度为5mL/L-40mL/L。
7.如权利要求1所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:步骤一中,所述金属-陶瓷封装外壳在氧化液中浸渍的温度为20℃-40℃,浸渍的时间为20s-60s。
8.如权利要求1所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:步骤二中,所述金属-陶瓷封装外壳在还原液中浸渍的温度为20℃-40℃,浸渍的时间为10s-40s。
9.如权利要求1所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:步骤三中,所述酸浸的时间为10s-40s。
10.如权利要求1所述的金属-陶瓷封装外壳的电镀前处理方法,其特征在于:步骤三中,所述一次水洗和二次水洗的具体操作均为将所述金属-陶瓷外壳放入去离子水中浸渍30s-60s,然后采用去离子水喷淋清洗30s-60s。
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