CN107268043B - 一种用于铜互连hdi电镀填孔的抑制剂及电镀铜浴 - Google Patents
一种用于铜互连hdi电镀填孔的抑制剂及电镀铜浴 Download PDFInfo
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 44
- 239000010949 copper Substances 0.000 title claims abstract description 44
- 238000007747 plating Methods 0.000 title claims abstract description 40
- 239000003112 inhibitor Substances 0.000 title claims abstract description 29
- 238000011049 filling Methods 0.000 title claims abstract description 15
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- -1 polydithio-dipropyl Polymers 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 claims description 3
- ZCYAYDMGVNGKJC-UHFFFAOYSA-N sulfanyl propane-1-sulfonate Chemical compound CCCS(=O)(=O)OS ZCYAYDMGVNGKJC-UHFFFAOYSA-N 0.000 claims description 3
- YXYDKEGYAUWLIT-UHFFFAOYSA-N 3-(1,3-benzothiazol-2-ylsulfanyl)propane-1-sulfonic acid;sodium Chemical compound [Na].C1=CC=C2SC(SCCCS(=O)(=O)O)=NC2=C1 YXYDKEGYAUWLIT-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 2
- 230000003044 adaptive effect Effects 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 229910001431 copper ion Inorganic materials 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- NASDQFMKXPTVGB-UHFFFAOYSA-N s-formyl methanethioate Chemical compound O=CSC=O NASDQFMKXPTVGB-UHFFFAOYSA-N 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims 3
- MQVMJSWYKLYFIG-UHFFFAOYSA-N propane-1-sulfonic acid;sodium Chemical compound [Na].CCCS(O)(=O)=O MQVMJSWYKLYFIG-UHFFFAOYSA-N 0.000 claims 1
- NPAWNPCNZAPTKA-UHFFFAOYSA-M sodium;propane-1-sulfonate Chemical compound [Na+].CCCS([O-])(=O)=O NPAWNPCNZAPTKA-UHFFFAOYSA-M 0.000 claims 1
- 238000009713 electroplating Methods 0.000 abstract description 10
- 230000000996 additive effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 229920000768 polyamine Polymers 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
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- 238000003756 stirring Methods 0.000 description 3
- 206010016825 Flushing Diseases 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XKTMIJODWOEBKO-UHFFFAOYSA-M Guinee green B Chemical compound [Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C=CC=CC=2)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 XKTMIJODWOEBKO-UHFFFAOYSA-M 0.000 description 1
- XXACTDWGHQXLGW-UHFFFAOYSA-M Janus Green B chloride Chemical compound [Cl-].C12=CC(N(CC)CC)=CC=C2N=C2C=CC(\N=N\C=3C=CC(=CC=3)N(C)C)=CC2=[N+]1C1=CC=CC=C1 XXACTDWGHQXLGW-UHFFFAOYSA-M 0.000 description 1
- VJDDAARZIFHSQY-UHFFFAOYSA-N basic black 2 Chemical compound [Cl-].C=1C2=[N+](C=3C=CC=CC=3)C3=CC(N(CC)CC)=CC=C3N=C2C=CC=1NN=C1C=CC(=O)C=C1 VJDDAARZIFHSQY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- KBELKISESIWDNY-UHFFFAOYSA-M sodium;3-sulfanylidenepropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CCC=S KBELKISESIWDNY-UHFFFAOYSA-M 0.000 description 1
- FTCLAXOKVVLHEG-UHFFFAOYSA-N sodium;3-sulfanylpropane-1-sulfonic acid Chemical compound [Na].OS(=O)(=O)CCCS FTCLAXOKVVLHEG-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001629 suppression Effects 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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/423—Plated through-holes or plated via connections characterised by electroplating method
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0703—Plating
- H05K2203/0713—Plating poison, e.g. for selective plating or for preventing plating on resist
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
本发明属于印制电路板电镀技术领域,提供一种用于铜互连HDI电镀填孔的抑制剂及电镀铜浴;本发明抑制剂为有机聚胺类化合物,其分子结构为:R1,R2为苯基、甲基、甲氧苯基或苯基衍生物;本发明抑制剂具有在HDI板盲孔孔底快速填铜的同时抑制HDI板面铜的生长速率,从而达到在填充镀铜后,面铜厚度较薄的特性,此外还具有添加剂操作窗口宽,镀液寿命较长等优点。
Description
技术领域
本发明属于印制电路板电镀技术领域,涉及微盲孔填孔镀铜工艺,具体为一种用于铜互连HDI电镀填孔的抑制剂及电镀铜浴。
背景技术
PCB板电镀工艺是一项繁琐的工作,随着越来越多的层数,越来越小的过孔直径(通孔和盲孔)、更高性能的材料及电镀体系中电力线在孔中与孔口处分布不均,导致现在的技术难度急剧增大,如HDI印制电路板和集成电路封装基板要求布线的高密度化,通孔孔径和微盲孔<100μm;此外,在印制电路板中,也要求同时进行通孔电镀和盲孔填铜;因此,铜互连HDI电镀填孔的电镀铜浴、以及作为电镀铜浴中的必要添加剂的抑制剂成为研究的重点。
目前,台湾中兴大学窦维平教授以PEG为抑制剂,聚二硫二丙烷磺酸钠(SPS)和3-巯基-1-丙烷磺酸钠(MPS)为加速剂,健那绿B(Janus Green B,JGB)和二嗪黑(DiazineBlack,DB)为整平剂([1]W.p.Dow et al.Electrochim.Acta.53(2008)3610–3619.[2]W.-P.Dow et al./Electrochimica Acta 54(2009)5894–5901.[3]W.P.Dow etal.J.Electrochem.Soc.152(2005)C425-C434.[4]W.P.Dow et al.Electrochem.Solid-State Lett.9(2006)C134-C1 37.),并且在有适量的氯离子存在的酸性体系中,对不同厚径比的微盲孔电镀填铜做了大量的实验,但上述的以PEG为抑制剂的体系会存在镀铜表面沉积厚度厚,添加剂操作窗口窄,镀液的寿命较低等缺陷,不适合大规模生产。
发明内容
本发明的目的在于针对背景技术的缺陷,提供一种铜互连HDI电镀填孔电镀铜浴及其中使用的抑制剂,能够加速HDI板盲孔孔底镀铜速率及抑制面铜生长速率,填充镀铜后,面铜厚度较薄,盲孔孔口平整。
为实现上述目的,本发明采用的技术方案为:
一种用于铜互连HDI电镀填孔的抑制剂,其特征在于,所述抑制剂为有机聚胺类化合物,其分子结构为:
其中,R1,R2为苯基、甲基、甲氧苯基或苯基衍生物。
进一步的,包含上述抑制剂的电镀铜浴,包含:60~220g/L的铜离子、20~160g/L的H2SO4、20-80mg/L的氯离子、0.5~20ml/L的加速剂及0.5~380ml/L的抑制剂,其余为水,所述水为超纯水。
更进一步的,所述加速剂采用聚二硫二丙烷磺酸钠、醇硫基丙烷磺酸钠、二甲基甲酰胺基丙烷磺酸钠、3-(苯骈噻唑-2-硫基)丙烷磺酸钠、3-硫基-1-丙磺酸钠盐以及二甲基-二硫甲酰胺磺酸中的一种或几种的组合。
所述电镀铜浴的工艺条件为:电流密度:0.01~6A/dm2,适应温度:10-40℃。
所述电镀铜浴还包含整平剂,采用健那绿(JGB)及其衍生物二嗪黑(DB)。
本发明的有益效果在于:
本发明提供一种铜互连HDI电镀填孔的抑制剂以及包含该抑制剂的电镀铜浴,该抑制剂具有在HDI板盲孔孔底快速填铜的同时抑制HDI板面铜的生长速率,从而达到在填充镀铜后,面铜厚度较薄的特点,此外还具有添加剂操作窗口宽,镀液寿命较长等优点;同时,组合使用该抑制剂和加速剂得到电镀铜浴,通过合理的电镀工艺能够实现HDI微盲孔及通孔的无缺陷电镀,有助于提高电镀铜与基材的结合力;并且,由于抑制剂对电路板表面的抑制作用较强,而加速剂更易于吸附在盲孔底部,能够在短时间内实现超级盲孔填铜,即保证高的填充速度,同时电镀后基板表面沉积铜的厚度较薄;进而,提高HDI铜互连品质,降低HDI铜互连制作的成本,提升生产效率。
附图说明
图1是由实施例1得到的电镀盲孔的剖面金相显微镜图片。
图2是由实施例2得到的电镀盲孔的剖面金相显微镜图片。
图3是由实施例3得到的电镀通孔的剖面金相显微镜图片。
具体实施方式
以下结合具体实施例和附图对本发明的技术方案作进一步详细说明。
实施例1
抑制剂的配制:先将100g分析纯硫酸加入2000g超纯水中配置成约5%硫酸溶液,再将10g抑制剂加入到1000ml的5%硫酸溶液中,在30℃下搅拌10min,配制得抑制剂;
加速剂的配制:先将1g聚二硫二丙烷磺酸钠加入500g的5%硫酸溶液中,在30℃下搅拌10min;然后,再添加5%硫酸溶液定容至1L,持续搅拌1h后,配制得加速剂;
电镀铜浴的配制:在2000mL酸铜电镀液中(含220g/L CuSO4·5H2O、55gH2SO4和60mg/L Cl-),依次加入抑制剂40ml、加速剂12ml,搅拌5min后得到电镀铜浴;
电镀前处理过程为:上板、除油、水洗、微蚀、水洗、镀铜等,微蚀刻中缓蚀剂为A成分,不含预浸过程。
以125×75μm(其中,孔直径为125μm)盲孔孔型为例:
控制镀槽温度15℃,控制阴极电流密度为1.5ASD,继续电镀60min,整个电镀过程在2.5NL/min打气下完成,电镀完成后取出盲孔板,用大量蒸馏水冲洗,冷风吹干后,即得样品;采用本实施方式制备的电镀填孔样品的盲孔剖面金相显微照片如图1所示,面铜厚度为17μm。
实施例2
以120×75μm(其中,孔直径为120μm)盲孔孔型为例:
采用与实施例1相同的抑制剂配置及电镀铜浴配置,
加速剂的配制:将1g醇硫基丙烷磺酸钠加入到1000g 5%硫酸溶液中,在30℃下搅拌15min,配制得加速剂;
控制镀槽温度20℃,控制阴极电流密度为2ASD,继续电镀30min,整个电镀过程在2.5NL/min打气下完成,电镀完成后取出阴极盲孔板,用大量蒸馏水冲洗,冷风吹干后,即得样品;采用本实施方式制备的电镀填孔样品的盲孔剖面金相显微照片如图2所示,面铜厚度为8.9μm。
实施例3
以0.3mm×3.0mm(其中孔直径为0.3mm)通孔孔型为例,抑制剂、加速剂及电镀铜浴配制及实验条件如实施例2所示,采用本实施方式制备的电镀通孔样品的盲孔剖面金相显微照片如图3所示;通孔中心点面铜厚度为7.3μm。
尽管本发明的内容已经通过上述优选实施例作了较为详细的介绍,应当指出,对于本领域的普通技术人员来说,在阅读了上述内容后,对于本发明的多种修改和替代都将是显而易见的。
以上所述,仅为本发明的具体实施方式,本说明书中所公开的任一特征,除非特别叙述,均可被其他等效或具有类似目的的替代特征加以替换;所公开的所有特征、或所有方法或过程中的步骤,除了互相排斥的特征和/或步骤以外,均可以任何方式组合。
Claims (5)
1.一种抑制剂在铜互连HDI电镀填孔中的应用,其特征在于,所述抑制剂的分子结构为:
其中,R1,R2为苯基、甲基、甲氧苯基或苯基衍生物。
2.包含按权利要求1所述抑制剂的电镀铜浴,包含:60~220g/L的铜离子、20~160g/L的H2SO4、20-80mg/L的氯离子、0.5~20ml/L的加速剂及0.5~380ml/L的抑制剂。
3.按权利要求2所述电镀铜浴,其特征在于,所述加速剂采用聚二硫二丙烷磺酸钠、醇硫基丙烷磺酸钠、二甲基甲酰胺基丙烷磺酸钠、3-(苯骈噻唑-2-硫基)丙烷磺酸钠、3-硫基-1-丙磺酸钠盐以及二甲基-二硫甲酰胺磺酸中的一种或几种的组合。
4.按权利要求2所述电镀铜浴,其特征在于,所述电镀铜浴的工艺条件为:电流密度:0.01~6A/dm2,适应温度:10-40℃。
5.按权利要求2所述电镀铜浴,其特征在于,所述电镀铜浴还包含整平剂,采用健那绿(JGB)及其衍生物二嗪黑(DB)。
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CN107385487B (zh) * | 2017-07-24 | 2019-05-10 | 电子科技大学 | 2,4,8,10-四氧杂-3,9-二磷杂螺环化合物在hdi板快速镀铜前处理溶液的应用及其前处理工艺 |
CN113026066A (zh) * | 2021-03-04 | 2021-06-25 | 江西博泉化学有限公司 | 一种非预浸体系的盲孔填孔镀铜液及其镀铜工艺 |
CN114351195A (zh) * | 2022-03-19 | 2022-04-15 | 深圳市创智成功科技有限公司 | 一种脉冲通孔填孔的电镀铜配方及其电镀工艺 |
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