CN114150299A - 用于超低轮廓铜箔及其覆铜板制备的化学沉积方法 - Google Patents
用于超低轮廓铜箔及其覆铜板制备的化学沉积方法 Download PDFInfo
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- copper
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000011889 copper foil Substances 0.000 title claims abstract description 63
- 238000005234 chemical deposition Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 53
- 230000004913 activation Effects 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 238000003892 spreading Methods 0.000 claims abstract description 28
- 230000007480 spreading Effects 0.000 claims abstract description 28
- 239000012691 Cu precursor Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 15
- 230000003213 activating effect Effects 0.000 claims abstract description 14
- 239000002585 base Substances 0.000 claims description 31
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 22
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical group O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910052802 copper Inorganic materials 0.000 claims description 19
- 239000010949 copper Substances 0.000 claims description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- 239000012752 auxiliary agent Substances 0.000 claims description 15
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical group COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 14
- 239000005749 Copper compound Substances 0.000 claims description 14
- 239000003638 chemical reducing agent Substances 0.000 claims description 14
- 230000000536 complexating effect Effects 0.000 claims description 14
- 239000008139 complexing agent Substances 0.000 claims description 14
- 150000001880 copper compounds Chemical class 0.000 claims description 14
- 239000006184 cosolvent Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 230000003746 surface roughness Effects 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 12
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 12
- 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 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 12
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 12
- 239000000276 potassium ferrocyanide Substances 0.000 claims description 12
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 9
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 9
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 8
- -1 polyethylene terephthalate Polymers 0.000 claims description 8
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical group CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000007602 hot air drying Methods 0.000 claims description 6
- 238000010345 tape casting Methods 0.000 claims description 6
- 239000004642 Polyimide Substances 0.000 claims description 5
- HFDWIMBEIXDNQS-UHFFFAOYSA-L copper;diformate Chemical compound [Cu+2].[O-]C=O.[O-]C=O HFDWIMBEIXDNQS-UHFFFAOYSA-L 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 229920006254 polymer film Polymers 0.000 claims description 5
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 239000011112 polyethylene naphthalate Substances 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 claims description 2
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 2
- 238000005137 deposition process Methods 0.000 claims 3
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 claims 1
- 229920000915 polyvinyl chloride Polymers 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000010842 industrial wastewater Substances 0.000 abstract 1
- 238000010924 continuous production Methods 0.000 description 6
- 229940071575 silver citrate Drugs 0.000 description 5
- QUTYHQJYVDNJJA-UHFFFAOYSA-K trisilver;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Ag+].[Ag+].[Ag+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QUTYHQJYVDNJJA-UHFFFAOYSA-K 0.000 description 5
- 238000004804 winding Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 241001089723 Metaphycus omega Species 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000003851 corona treatment Methods 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
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- 238000003912 environmental pollution Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 238000003908 quality control method Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- 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
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
-
- 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
- C23C18/1655—Process features
- C23C18/1657—Electroless forming, i.e. substrate removed or destroyed at the end of the process
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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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1813—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by radiant energy
- C23C18/1817—Heat
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1831—Use of metal, e.g. activation, sensitisation with noble 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
- 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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1841—Multistep pretreatment with use of metal first
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Abstract
本发明公开了一种用于超低轮廓铜箔及其覆铜板制备的化学沉积方法,包括以下步骤:对基材表面预处理,基材表面活化处理:将活化溶液均匀铺展于预处理后的基材表面,加热处理,在基材上得到活化层,进行一次或重复多次以下步骤,得到覆铜板:将铜前驱体溶液水平铺展在活化层的表面,加热处理。采用本发明公开的制备方法与工艺技术,可以流水线方式连续、高效地生产超低轮廓的铜箔或覆有超低轮廓铜箔的覆铜板,相应流程模式的建立,将两种产品的生产过程合二为一,显著降低了投资成本,可极大提高企业经济效益。同时,采用薄层溶液方式实施的化学沉积模式,避免了大量工业废水的产生与排放,有利于可持续发展与环境保护。
Description
技术领域
本发明属于铜箔或覆铜板制造技术领域,具体来说涉及一种用于超低轮廓铜箔及其覆铜板制备的化学沉积方法。
背景技术
目前用于铜箔及其覆铜板生产的常规方法如下:首先通过电解、压延等方式生产铜箔,再通过压合、胶粘等方式将其粘附于基材表面形成覆铜板。这种生产方式的不足之处在于:
(1)在目前的技术水平下,以该方式得到的铜箔,其表面粗糙度较高,难以满足日益增长的5G通信、自动驾驶以及远程医疗等系统对于高品质铜箔及其覆铜板的迫切需求,无法保证高频高速信号的传输质量。例如,制备的超低轮廓铜箔(VLP)乃至所谓的极低轮廓铜箔(HVLP),其Ra值仍处于100nm以上。尽管曾有文献(Sci.Rep.,2014,4,6230)和(Nanoscale,2014,6,12943)报道,通过溅射或气相沉积等方法制备的覆铜板,其Ra值可低至数十纳米,但因存在过程复杂、制造设备昂贵等缺点,以及缺乏相应工业技术积累,难以实现连续化操作,因而无法直接用于工业化的批量生产。
(2)传统的电解或压延方式生产的铜箔厚度通常在6μm以上,难以满足电子产品轻薄化的发展趋势。
(3)以该方式生产覆铜板时,需要先制备铜箔,然后再将其粘附于基材,铜箔制备与覆铜板生产分属不同工业领域,过程分散,牵涉环节多,品控管理复杂,设备投资大,经济效益低,无法建立从溶铜工序开始直至最终生产出覆铜板的统一、完整的工艺流程,实现真正意义上的覆铜板连续生产。
(4)以传统的电解方式生产铜箔时,生产过程能耗高,所需的各种化学品种类繁多,产品指标控制多通过众多的助剂使用来达成,整个反应过程原料液用量大、污染危害严重,原料利用率低,且产生的废液较多,不利于环境保护与可持续发展。
发明内容
为降低铜箔及其覆铜板表面的粗糙度,实现从溶铜工序开始直至最终生产出覆铜板的连续生产,大幅减少废液排放,本发明的目的在于提供一种制备超低轮廓铜箔的覆铜板的化学沉积方法,该化学沉积方法通过水平铺展的薄层溶液方式实施化学沉积以降低铜表面的粗糙度。
本发明的目的是通过下述技术方案予以实现的。
一种制备覆有超低轮廓铜箔的覆铜板的化学沉积方法,包括以下步骤:
1)对基材表面预处理;
在所述步骤1)中,所述预处理包括:电晕、等离子体、酸洗、碱洗和除尘中的一种或几种。
在所述步骤1)中,所述基材为表面粗糙度Ra低于20nm的聚合物薄膜材料或刚性材料。
在上述技术方案中,所述聚合物薄膜材料为聚对苯二甲酸乙二醇酯(polyethylene terephthalate,PET)、聚酰亚胺(Polyimide,PI)、聚碳酸酯(Polycarbonate,PC)、聚萘二甲酸乙二醇酯(polyethylene naphthalate,PEN)、聚氯乙烯(Polyvinyl chloride,PVC)或聚四氟乙烯(Polytetra fluoroethylene,PTFE),刚性材料为玻璃、硅片或陶瓷。
2)基材表面活化处理:将活化溶液均匀铺展于预处理后的基材表面,在60-200℃下加热处理5-10min,在基材上得到活化层,其中,所述活化溶液包括:0.1-50g/L的含活化金属元素的化合物、50-800g/L的络合溶剂和0-700g/L的助溶剂;
在所述步骤2)中,所述活化金属元素为金、银、铂、镍和铜中的一种。
在所述步骤2)中,所述络合溶剂为1,2-丙二胺、仲丁胺、叔丁胺或异丙胺,所述助溶剂为甲醇、乙醇或异丙醇。
3)进行1次或重复多次以下步骤,用于在活化层的表面生成厚度为200nm-6μm的铜箔,得到覆铜板:将铜前驱体溶液铺展在活化层的表面,60-80℃加热处理5-10min。
在所述步骤3)中,所述铜前驱体溶液包括:0.1-100g/L的铜化合物、0.1-100g/L的络合剂、0.1-100g/L的还原剂、0.1-100g/L的pH调节剂、0.001-1g/L的助剂和0-500g/L的溶液粘度调节剂和0-500g/L的表面张力调节剂。
在所述步骤3)中,所述铜化合物为甲酸铜、氯化铜、硝酸铜、硫酸铜或乙酸铜;络合剂为乙二胺四乙酸二钠、甲酸铵、硫酸铵、硝酸铵和氯化铵中的一种或多种;还原剂为甲醛;pH调节剂为氢氧化钠;助剂为亚铁氰化钾、2-2联吡啶和联喹啉中的一种或多种;溶液粘度调节剂为甲醇、乙醇、乙二醇或丙三醇;表面张力调节剂为丙二醇甲醚。
在所述步骤3)中,在所述加热处理后进行水洗和50-90℃热风烘干。
在上述技术方案中,所述铺展采用刮棒涂布、刮刀涂布、流延涂布或喷雾涂布。
在上述技术方案中,所述活化溶液的铺展的厚度为0.1-1mm,铜前驱体溶液的铺展的厚度为0.5-5mm。
一种制备铜箔的方法,将所述化学沉积方法获得的覆铜板进行基材溶解或基材剥离。
本发明的有益效果包括:
(1)本发明所提供的技术路线和实施方案,兼顾了铜箔和覆铜板两种产品的生产特点和不同需求,在强调两者共性的基础上,建立了统一便捷的连续生产体系,使之既可用于覆铜板的直接制备,也可采用首先制备柔性的覆铜板、然后再溶解或剥离其基材的方式,实现超低轮廓铜箔卷对卷模式的连续化生产。
(2)本发明所提供的技术方案,将覆铜板常规生产模式中的先制备铜箔、然后再将其粘附于基材的制备过程合二为一,建立起从溶铜工序开始直至最终生产出覆铜板的统一、完整的工艺流程,投资成本显著降低,经济效益极大提高。
(3)采用本发明所生产的铜箔和覆铜板,质量更好,表面粗糙度更低、铜箔厚度可控,实现了超低轮廓铜箔及其覆铜板的批量制备。
(4)沉积反应在水平铺展的薄层溶液中进行,使得原料利用率大大提高,材料成本大幅节约,产生的废液显著减少,环境污染程度得到有效改善。
具体实施方式
下面结合具体实施例进一步说明本发明的技术方案。
下述实施例中的加热为将基材水平放置于金属或陶瓷类加热平板之上进行加热,或是通过一个具有恒温加热功能的腔室进行加热。
当选择聚合物薄膜材料时,既可通过卷对卷的方式生产柔性覆铜板;也可结合特定基材的选择、铜前驱体溶液配方的调整及后续的基材溶解或剥离等环节,连续生产超低轮廓的单纯铜箔;当选择刚性材料时,可将其用于包含有基材分发和产品收集装置的工艺流程中,实现刚性覆铜板的连续生产。
下述实施例所涉及药品的购买源如下:
所有药品均购买于天津市元立化工有限公司。
实施例1
一种制备覆有超低轮廓铜箔的覆铜板的化学沉积方法,包括以下步骤:
1)准备基材,基材为表面粗糙度Ra为9nm的聚对苯二甲酸乙二醇酯(polyethyleneterephthalate,PET)薄膜。
对基材表面预处理,预处理包括:先2kW电晕处理5s,再硅胶滚轮除尘。
2)基材表面活化处理:采用流延涂布将活化溶液均匀铺展于预处理后的基材表面,活化溶液的铺展的厚度为0.3mm,通过加热板在150℃下加热处理10min,在基材上得到活化层,其中,活化溶液包括:15g/L的含活化金属元素的化合物、750g/L的络合溶剂和80g/L的助溶剂,化合物为柠檬酸银,络合溶剂为1,2-丙二胺,助溶剂为甲醇;
3)进行1次以下步骤,用于在活化层的表面生成厚度为300nm的铜箔,得到覆铜板:采用流延涂布将铜前驱体溶液铺展在活化层的表面,80℃加热处理5min,进行喷淋水洗和80℃热风烘干15s,其中,铜前驱体溶液的铺展的厚度为3mm。铜前驱体溶液包括:15g/L的铜化合物、70g/L的络合剂、30g/L的还原剂、40g/L的pH调节剂、0.09g/L的助剂和180g/L的溶液粘度调节剂和130g/L的表面张力调节剂;铜化合物为甲酸铜;络合剂为乙二胺四乙酸二钠和甲酸铵,乙二胺四乙酸二钠的浓度为40g/L,甲酸铵的浓度为30g/L;还原剂为甲醛;pH调节剂为氢氧化钠;助剂为亚铁氰化钾、2-2联吡啶和联喹啉,亚铁氰化钾的浓度为0.03g/L,2-2联吡啶的浓度为0.03g/L,联喹啉的浓度为0.03g/L;溶液粘度调节剂为丙三醇;表面张力调节剂为丙二醇甲醚。
本实施例获得的覆铜板表面(即覆铜板表面的铜箔)粗糙度Ra为14nm,方块电阻值为89mΩ/□,铜箔厚度为300nm。
实施例2
一种制备覆有超低轮廓铜箔的覆铜板的化学沉积方法,包括以下步骤:
1)准备基材,基材为表面粗糙度Ra为4nm的玻璃板。
对基材表面预处理,预处理包括:pH=1的酸液进行3min酸洗处理和硅胶滚轮除尘处理。
2)基材表面活化处理:采用刮棒涂布将活化溶液均匀铺展于预处理后的基材表面,活化溶液的铺展的厚度为0.2mm,通过加热板在150℃下加热处理10min,在基材上得到活化层,其中,活化溶液包括:10g/L的含活化金属元素的化合物、650g/L的络合溶剂和150g/L的助溶剂,化合物为柠檬酸银,络合溶剂为1,2-丙二胺,助溶剂为甲醇;
3)进行1次以下步骤,用于在活化层的表面生成厚度为200nm的铜箔,得到覆铜板:采用刮棒涂布将铜前驱体溶液铺展在活化层的表面,70℃加热处理8min,进行喷淋水洗和80℃热风烘干15s,其中,铜前驱体溶液的铺展的厚度为2mm。铜前驱体溶液包括:20g/L的铜化合物、95g/L的络合剂、40g/L的还原剂、45g/L的pH调节剂、0.15g/L的助剂和160g/L的溶液粘度调节剂和180g/L的表面张力调节剂;铜化合物为硫酸铜;络合剂为乙二胺四乙酸二钠和硫酸铵,乙二胺四乙酸二钠的浓度为60g/L,硫酸铵的浓度为35g/L;还原剂为甲醛;pH调节剂为氢氧化钠;助剂为亚铁氰化钾、2-2联吡啶和联喹啉,亚铁氰化钾的浓度为0.05g/L,2-2联吡啶的浓度为0.05g/L,联喹啉的浓度为0.05g/L,溶液粘度调节剂为乙二醇;表面张力调节剂为丙二醇甲醚。
本实施例获得的覆铜板表面(即覆铜板表面的铜箔)粗糙度Ra为11nm,方块电阻值为144mΩ/□,铜箔厚度为200nm。
实施例3
一种制备覆有超低轮廓铜箔的覆铜板的化学沉积方法,包括以下步骤:
1)准备基材,基材为表面粗糙度Ra为9nm的聚对苯二甲酸乙二醇酯(polyethyleneterephthalate,PET)薄膜。
对基材表面预处理,预处理包括:2kW电晕处理5s和硅胶滚轮除尘处理。
2)基材表面活化处理:采用刮棒涂布将活化溶液均匀铺展于预处理后的基材表面,活化溶液的铺展的厚度为0.3mm,于加热腔室内在150℃下加热处理10min,在基材上得到活化层,其中,活化溶液包括:5g/L的含活化金属元素的化合物、600g/L的络合溶剂和240g/L的助溶剂,化合物为柠檬酸银,络合溶剂为1,2-丙二胺,助溶剂为甲醇;
3)重复10次以下步骤,用于在活化层的表面生成厚度为3μm的铜箔,得到覆铜板:采用刮棒涂布将铜前驱体溶液铺展在活化层的表面,在加热腔室内80℃加热处理5min,进行喷淋水洗和80℃热风烘干15s,其中,铜前驱体溶液的铺展的厚度为3mm。铜前驱体溶液包括:20g/L的铜化合物、70g/L的络合剂、30g/L的还原剂、40g/L的pH调节剂、0.15g/L的助剂和190g/L的溶液粘度调节剂和140g/L的表面张力调节剂;铜化合物为甲酸铜;络合剂为乙二胺四乙酸二钠和甲酸铵,乙二胺四乙酸二钠的浓度为40g/L,甲酸铵的浓度为30g/L;还原剂为甲醛;pH调节剂为氢氧化钠;助剂为亚铁氰化钾、2-2联吡啶和联喹啉,亚铁氰化钾的浓度为0.05g/L,2-2联吡啶的浓度为0.05g/L,联喹啉的浓度为0.05g/L;溶液粘度调节剂为丙三醇;表面张力调节剂为丙二醇甲醚。
本实施例获得的覆铜板表面(即覆铜板表面的铜箔)粗糙度Ra为37nm,方块电阻值为11mΩ/□,铜箔厚度为3μm。
实施例4
一种制备超低轮廓铜箔的化学沉积方法,包括以下步骤:
1)准备基材,基材为表面粗糙度Ra为12nm的聚酰亚胺(Polyimide,PI)薄膜。
对基材表面预处理,预处理包括:pH=13的碱液进行1min碱洗处理和除尘处理。
2)基材表面活化处理:采用流延涂布将活化溶液均匀铺展于预处理后的基材表面,活化溶液的铺展的厚度为0.1mm,于加热腔室内在150℃下加热处理10min,在基材上得到活化层,其中,活化溶液包括:10g/L的含活化金属元素的化合物、600g/L的络合溶剂和240g/L的助溶剂,化合物为柠檬酸银,络合溶剂为1,2-丙二胺,助溶剂为甲醇;
3)重复10次以下步骤,用于在活化层的表面生成厚度为3μm的铜箔,得到覆铜板:采用流延涂布将铜前驱体溶液铺展在活化层的表面,在加热腔室内60℃加热处理10min,进行喷淋水洗和80℃热风烘干15s,其中,铜前驱体溶液的铺展的厚度为1mm。铜前驱体溶液包括:15g/L的铜化合物、70g/L的络合剂、30g/L的还原剂、40g/L的pH调节剂、0.15g/L的助剂和120g/L的溶液粘度调节剂和130g/L的表面张力调节剂;铜化合物为硝酸铜;络合剂为乙二胺四乙酸二钠和硝酸铵,乙二胺四乙酸二钠的浓度为40g/L,硝酸铵的浓度为30g/L;还原剂为甲醛;pH调节剂为氢氧化钠;助剂为亚铁氰化钾、2-2联吡啶和联喹啉,亚铁氰化钾的浓度为0.05g/L,2-2联吡啶的浓度为0.05g/L,联喹啉的浓度为0.05g/L;溶液粘度调节剂为甲醇;表面张力调节剂为丙二醇甲醚。
再经过剥离工艺过程将铜箔剥离下来,本实施例获得的铜箔表面粗糙度Ra为44nm,方块电阻值为11mΩ/□,铜箔厚度为3μm。
其中,剥离工艺过程为:
1.在覆铜板上铜箔一面的边缘粘贴3M VHB高粘度双面胶,并将3M VHB高粘度双面胶的另一面粘贴在全自动收卷机的相应位置;
2.启动全自动收卷机,实现铜箔与基材的剥离,同时将铜箔进行收卷。
实施例5
一种制备覆有超低轮廓铜箔的覆铜板的化学沉积方法,包括以下步骤:
1)准备基材,基材为表面粗糙度Ra为9nm的聚对苯二甲酸乙二醇酯(polyethyleneterephthalate,PET)薄膜。
对基材表面预处理,预处理包括:2kW电晕处理5s和硅胶滚轮除尘处理。
2)基材表面活化处理:采用流延涂布将活化溶液均匀铺展于预处理后的基材表面,活化溶液的铺展的厚度为3mm,于加热腔室内在150℃下加热处理10min,在基材上得到活化层,其中,活化溶液包括:10g/L的含活化金属元素的化合物、700g/L的络合溶剂和150g/L的助溶剂,化合物为柠檬酸银,络合溶剂为1,2-丙二胺,助溶剂为甲醇;
3)重复10次以下步骤,用于在活化层的表面生成厚度为300nm的铜箔,得到覆铜板:采用流延涂布将铜前驱体溶液铺展在活化层的表面,在腔室内于80℃加热处理5min,进行喷淋水洗和80℃热风烘干15s,其中,铜前驱体溶液的铺展的厚度为3mm。铜前驱体溶液包括:20g/L的铜化合物、95g/L的络合剂、40g/L的还原剂、60g/L的pH调节剂、0.15g/L的助剂和190g/L的溶液粘度调节剂和140g/L的表面张力调节剂;铜化合物为甲酸铜;络合剂为乙二胺四乙酸二钠和甲酸铵,乙二胺四乙酸二钠的浓度为60g/L,甲酸铵的浓度为35g/L;还原剂为甲醛;pH调节剂为氢氧化钠;助剂为亚铁氰化钾、2-2联吡啶和联喹啉,亚铁氰化钾的浓度为0.05g/L,2-2联吡啶的浓度为0.05g/L,联喹啉的浓度为0.05g/L;溶液粘度调节剂为丙三醇;表面张力调节剂为丙二醇甲醚。
上述步骤获得的覆铜板表面(即覆铜板表面的铜箔)粗糙度Ra为14nm,方块电阻值为98mΩ/□,铜箔厚度为300nm。
按照上述步骤1)~3)对基材的另一面进行处理,获得的覆铜板表面粗糙度Ra为17nm,方块电阻值为94mΩ/□,铜箔厚度为300nm。
在本发明的技术方案中,关于由覆铜板去除基材得到单纯铜箔的生产环节,可以采用以下方法之一:
一是基材溶解,选择较易通过有机溶剂进行溶解的基材进行上述化学沉积方法,去除基材的具体实施方式为将制备的覆铜板直接浸泡于相应的有机溶剂中,待基材完全溶解后即可得到单纯铜箔。
二是基材剥离,与生产覆铜板不同,预处理过程不需要进行增加附着力的相关处理,仅需要进行表面的简单清洗与除尘。具体的剥离工艺可通过全自动收卷机进行,简单叙述如下:
1.在覆铜板上铜箔一面的边缘粘贴3M VHB高粘度双面胶,并将3M VHB高粘度双面胶的另一面粘贴在全自动收卷机的相应位置;
2.启动全自动收卷机,实现铜箔与基材的剥离,同时将铜箔进行收卷。
以上对本发明做了示例性的描述,应该说明的是,在不脱离本发明的核心的情况下,任何简单的变形、修改或者其他本领域技术人员能够不花费创造性劳动的等同替换均落入本发明的保护范围。
Claims (10)
1.一种制备超低轮廓铜箔的覆铜板的化学沉积方法,其特征在于,包括以下步骤:
1)对基材表面预处理;
2)基材表面活化处理:将活化溶液均匀铺展于预处理后的基材表面,在60-200℃下加热处理5-10min,在基材上得到活化层,其中,所述活化溶液包括:0.1-50g/L的含活化金属元素的化合物、50-800g/L的络合溶剂和0-700g/L的助溶剂;
3)进行1次或重复多次以下步骤,用于在活化层的表面生成厚度为200nm-6μm的铜箔,得到覆铜板:将铜前驱体溶液铺展在活化层的表面,60-80℃加热处理5-10min。
2.根据权利要求1所述的化学沉积方法,其特征在于,在所述步骤1)中,所述预处理包括:电晕、等离子体、酸洗、碱洗和除尘中的一种或几种;
在所述步骤1)中,所述基材为表面粗糙度Ra低于20nm的聚合物薄膜材料或刚性材料,所述聚合物薄膜材料为聚对苯二甲酸乙二醇酯、聚酰亚胺、聚碳酸酯、聚萘二甲酸乙二醇酯、聚氯乙烯或聚四氟乙烯,刚性材料为玻璃、硅片或陶瓷。
3.根据权利要求1所述的化学沉积方法,其特征在于,在所述步骤2)中,所述活化金属元素为金、银、铂、镍和铜中的一种。
4.根据权利要求1所述的化学沉积方法,其特征在于,在所述步骤2)中,所述络合溶剂为1,2-丙二胺、仲丁胺、叔丁胺或异丙胺,所述助溶剂为甲醇、乙醇或异丙醇。
5.根据权利要求1所述的化学沉积方法,其特征在于,在所述步骤3)中,所述铜前驱体溶液包括:0.1-100g/L的铜化合物、0.1-100g/L的络合剂、0.1-100g/L的还原剂、0.1-100g/L的pH调节剂、0.001-1g/L的助剂和0-500g/L的溶液粘度调节剂和0-500g/L的表面张力调节剂。
6.根据权利要求5所述的化学沉积方法,其特征在于,在所述步骤3)中,所述铜化合物为甲酸铜、氯化铜、硝酸铜、硫酸铜或乙酸铜;络合剂为乙二胺四乙酸二钠、甲酸铵、硫酸铵、硝酸铵和氯化铵中的一种或多种;还原剂为甲醛;pH调节剂为氢氧化钠;助剂为亚铁氰化钾、2-2联吡啶和联喹啉中的一种或多种;溶液粘度调节剂为甲醇、乙醇、乙二醇或丙三醇;表面张力调节剂为丙二醇甲醚。
7.根据权利要求1所述的化学沉积方法,其特征在于,在所述步骤3)中,在所述加热处理后进行水洗和50-90℃热风烘干。
8.根据权利要求1所述的化学沉积方法,其特征在于,所述铺展采用刮棒涂布、刮刀涂布、流延涂布或喷雾涂布。
9.根据权利要求1所述的化学沉积方法,其特征在于,所述活化溶液的铺展的厚度为0.1-1mm,铜前驱体溶液的铺展的厚度为0.5-5mm。
10.一种制备铜箔的方法,将权利要求1~9中任意一项所述化学沉积方法获得的覆铜板进行基材溶解或基材剥离。
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