TW202314037A - 電子元件的製造方法 - Google Patents
電子元件的製造方法 Download PDFInfo
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- TW202314037A TW202314037A TW111121506A TW111121506A TW202314037A TW 202314037 A TW202314037 A TW 202314037A TW 111121506 A TW111121506 A TW 111121506A TW 111121506 A TW111121506 A TW 111121506A TW 202314037 A TW202314037 A TW 202314037A
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- side layer
- plating
- plating bath
- surface side
- tin
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- 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
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
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- 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
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- 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
- 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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- 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
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- 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
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- C23C18/1635—Composition of the substrate
- C23C18/1637—Composition of the substrate metallic substrate
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- 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
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- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
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- 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
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- C23C18/1601—Process or apparatus
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- C23C18/1655—Process features
- C23C18/1658—Process features with two steps starting with metal deposition followed by addition of reducing agent
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- 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
- C23C18/1689—After-treatment
- C23C18/1692—Heat-treatment
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- 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
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- 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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- 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
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- C23C18/1841—Multistep pretreatment with use of metal first
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- 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
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- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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
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- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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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
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- C23C18/52—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 using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
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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
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- C23C28/021—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 alloy layer
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25D3/30—Electroplating: Baths therefor from solutions of tin
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- 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
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
- C25D5/44—Aluminium
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- 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
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Abstract
本發明旨在提供一種電子元件的製造方法,其能夠穩定地製造具有足夠厚的鍍Sn膜且連接可靠性優異的電子元件。電子元件的製造方法包括:在由銅或銅合金、或者鋁或鋁合金形成的基材(101)上形成由鎳等形成的基材側層(121)的步驟;將選自由金、鈀、鉑、銀、銠、鈷、錫、銅、銥、鋨以及釕所構成的組中的一種或兩種以上的金屬作為催化劑(122)賦予在基材側層(121)上的步驟;以及通過含有三價鈦作為還原劑並含有焦磷酸鹽作為錯合劑的無電解鍍錫浴來形成表面側層(123)的步驟。表面側層(123)的厚度為0.5μm以上。
Description
本發明係關於一種電子元件的製造方法。
由錫(Sn)或Sn合金形成的Sn皮膜特別適合作為焊料接合部。因此,Sn皮膜被廣泛使用在印刷線路板或晶圓等電子元件中。
近年來,隨著電子元件和電路的小型化、微細化,產生了無法以電鍍法鍍覆的部分,因此形成Sn皮膜的主流方法為無電解鍍覆法。在無電解鍍覆法中,置換型無電解鍍浴使用置換析出反應,因此若要形成厚的鍍膜,則會對基底銅等進行較大幅度的蝕刻,鍍膜的膜厚分布會變得不均勻,並且焊料潛入阻焊劑下方等,焊料接合特性顯著降低。使基底銅等溶解的結果是,存在布線斷線、外觀變色等問題。
為了抑制基底溶解,開發了一種還原型鍍Sn浴,其含有三價鈦等還原劑,通過該還原劑的還原作用來形成鍍膜。但是,在含有三價鈦作為還原劑的鍍Sn浴的情況下,存在三價鈦迅速地氧化成四價鈦,鍍膜停止生長的問題。還研究了一邊將四價鈦還原成三價鈦、一邊進行鍍覆的方法,但除了要供給還原劑以外,還存在鍍浴的穩定性低、容易發生浴分解的問題,形成厚的鍍Sn膜相當困難。若鍍Sn膜的膜厚薄,在安裝時添加大量熱歷程的話,鍍Sn膜則會因與基底金屬的合金化而消失,導致連接可靠性降低。
還探討了通過反復交替地形成鍍Sn膜和銅鍍膜來實現鍍Sn膜的厚膜化的方法(例如,參照專利文獻1)。
專利文獻1:日本特開2010-202895號公報
-發明欲解決之技術問題-
通過交替地形成皮膜而能夠可靠地使鍍膜實現厚膜化,但由於必須要反復交替地形成皮膜,因此存在處理變得繁雜的問題。
本發明的目的在於:能夠穩定地製造具有足夠厚的鍍Sn膜且連接可靠性優異的電子元件。
-用於解決技術問題之技術手段-
本發明的電子元件的製造方法的一樣態包括基材側層形成步驟、催化劑賦予步驟以及表面側層形成步驟,在前述基材側層形成步驟中,通過無電解鍍鎳浴或無電解鍍鎳合金浴在由銅或銅合金、或者鋁或鋁合金形成的基材上形成由鎳或鎳合金形成的基材側層,在前述催化劑賦予步驟中,將選自由金、鈀、鉑、銀、銠、鈷、錫、銅、銥、鋨以及釕所構成的組中的一種或兩種以上的金屬作為催化劑賦予在前述基材側層上,在前述表面側層形成步驟中,通過含有三價鈦作為還原劑並含有焦磷酸鹽作為錯合劑的無電解鍍錫浴或無電解鍍錫合金浴來形成表面側層。在前述表面側層形成步驟中,形成厚度為0.5μm以上的表面側層。
-發明之效果-
根據本發明的電子元件的製造方法,能夠穩定地製造具有足夠厚的鍍Sn膜且連接可靠性優異的電子元件。
通過本實施方式的電子元件的製造方法能夠形成層壓膜102,其具有如圖1所示的形成在基材101上的基材側層121、催化劑122以及表面側層123。
能夠使基材101例如是在印刷線路板或半導體晶圓等的表面上形成的布線層或連接焊盤等。也可以是在布線層或連接焊盤等的表面上通過鍍覆或濺射等形成的金屬層等。能夠使基材101例如是由銅(Cu)或鋁(Al)或它們的合金形成的層。銅合金和鋁合金除了含有銅或鋁以外,還能夠含有鎳、鉻、錳、鐵、鈷、鎢、鈦以及矽等作為合金成分。合金成分的含量較佳為50%以下,更佳為10%以下。基材101的厚度並無特別限定,較佳為0.05μm以上,更佳為0.1μm以上,並且較佳為100μm以下,更佳為60μm以下。
能夠使基材側層121是由鎳(Ni)或者含有磷或硼等作為合金成分的鎳合金形成的層。基材側層121中的合金成分的含量較佳為50%以下,更佳為15%以下。其中由含磷的鎳-磷形成的層容易形成良好的皮膜,因而由含磷的鎳-磷形成的層較佳。基材側層121的厚度並無特別限定,從連接可靠性的觀點來看,較佳為0.05μm以上,更佳為0.1μm以上,並且較佳為15μm以下,更佳為7μm以下。
能夠使催化劑122為選自由金(Au)、鈀(Pd)、鉑(Pt)、銀(Ag)、銠(Rh)、鈷(Co)、錫(Sn)、銅(Cu)、銥(Ir)、鋨(Os)以及釕(Ru)所構成的組中的一種或兩種以上的金屬。其中,金、鈀、鉑、銀以及銠的催化效果高,賦予也容易,因此較佳。如圖1所示,催化劑122能夠形成為覆蓋基材側層121的整個表面的層狀。不過,催化劑122也可以不覆蓋基材側層121的整個表面,而是將催化劑122賦予成使基材側層121的表面的一部分暴露的島狀或網狀。被賦予了催化劑的那部分的厚度並無特別限定,從形成良好的表面側層123的觀點來看,較佳為0.0001μm以上,更佳為0.001μm以上,並且較佳為0.1μm以下。
能夠使表面側層123是由錫(Sn)或錫合金形成的層。從連接可靠性的觀點來看,表面側層123的厚度為0.5μm以上,較佳為1.0μm以上。從皮膜的形成時間等的觀點來看,膜厚的上限較佳為15μm以下,更佳為10μm以下。除了錫之外,還能舉例出:錫合金含有銀(Ag)、銅(Cu)、鉍(Bi)、鎳(Ni)等作為合金成分。作為具體示例,能舉例出:Sn-Ag、Sn-Ag-Cu、Sn-Cu、Sn-Bi、Sn-Cu-Ni、以及Sn-Cu-Bi等。
本實施方式的層壓膜102能夠按照下述方式形成。對基材101的表面進行脫脂、軟蝕刻以及酸洗等處理後,使用無電解鍍鎳或無電解鍍鎳合金(以下,將兩者合稱為無電解鍍鎳等)來形成基材側層121。在基材101由銅等形成的情況下,在進行無電解鍍鎳等之前賦予催化劑即可。能夠使催化劑是鈀(Pd)、銀(Ag)、金(Au)或鉑(Pt)等。在基材101由鋁等形成的情況下,能夠在進行浸鋅處理後進行無電解鍍鎳等。
接著,將催化劑122賦予在基材側層121的表面上。催化劑122的賦予例如能夠通過將基材浸漬在含有電位高的金屬的鹽溶液中來進行。能夠通過使膠體狀的金屬催化劑物理性地吸附於基材側層121的表面來進行。
在已被賦予了催化劑122的基材側層121上,使用無電解鍍錫浴來形成表面側層123。無電解鍍錫浴含有錫化合物、作為還原劑的三價鈦和作為錯合劑的焦磷酸鹽。
錫化合物只要是在鍍浴中產生二價錫離子的化合物即可。例如,能夠使錫化合物為氯化錫(II)、氯化錫(IV)、硫酸錫(II)、焦磷酸錫(II)、溴化錫(II)、溴化錫(IV)、碘化錫(II)、碘化錫(IV)、氟化錫(II)、氟化錫(IV)以及磷酸錫(II)等。錫化合物在鍍浴中的濃度並無特別限定,從皮膜的品質、析出速度等觀點來看,錫的濃度較佳為0.1g/L以上,更佳為1g/L以上,並且較佳為30g/L以下,更佳為15g/L以下。
作為還原劑的三價鈦例如能夠為三價的鹵化鈦或硫酸鈦等,例如能夠為氯化鈦(III)、溴化鈦(III)、碘化鈦(III)或硫酸鈦(III)等,較佳為其中的氯化鈦(III)。從使錫充分析出的觀點和鍍浴穩定性的觀點來看,還原劑即三價鈦在鍍浴中的濃度較佳為0.1g/L以上,更佳為1g/L以上,並且較佳為10g/L以下,更佳為7g/L以下。
能夠使作為錯合劑的焦磷酸鹽例如是焦磷酸四鉀、焦磷酸四鈉或焦磷酸二氫鈉等。從鍍浴的穩定性的觀點來看,錯合劑即焦磷酸在鍍浴中的濃度較佳為20g/L以上,更佳為50g/L以上,並且較佳為400g/L以下,更佳為300g/L以下。
通過使用三價的鈦作為還原劑、使用焦磷酸鹽作為錯合劑,能夠抑制鍍浴發生浴分解。由此而能夠形成較厚的表面側層123,能夠大幅度提升層壓膜102的連接可靠性。當採用鍍浴穩定性差的鍍浴時,即使能夠在實驗室水準下形成厚的鍍錫層,也難以進行工業生產。另一方面,本發明的鍍浴的穩定性高,因此能夠容易地在工業上生產出厚度為0.5μm以上的厚鍍錫層。
本實施方式的無電解鍍錫浴,作為促進錫析出的促進劑可以含有不含氮的有機硫醇。能夠使不含氮的有機硫醇例如是:1-丙硫醇、1-丁硫醇、1,2-乙二硫醇、1,2-丙二硫醇、1,4-丁二硫醇、1,5-戊二硫醇、1,6-己二硫醇、2-胺基乙硫醇、3-巰基-1,2-丙二醇、1,4-二巰基-2,3-丁二醇、3-巰基丙酸乙酯、苯硫醇、苯三硫醇、2,3-二氯苯硫醇、2,4-二甲基苯硫醇、2-胺基苯硫醇、2-萘硫醇、巰基苯甲酸、巰基琥珀酸、3-巰基丙酸、巰基乙酸、巰基水楊酸、2-巰基丙酸、6-巰基-1-己醇、3-巰基丙醇、3-巰基-1-己醇、3-巰基乙醇、2-巰基乙磺酸鈉、3-巰基-1-丙磺酸鈉、以及2,3-二巰基丙磺酸鈉一水合物中的任意一種以上。能夠通過不含氮的有機硫醇來促進鍍層析出。不含氮的有機硫醇的濃度較佳為0.1g/L以上,更佳為0.2g/L以上,並且較佳為10g/L以下,更佳為5g/L以下。
從促進鍍層析出、縮短週期時間的觀點來看,鍍浴較佳含有促進劑,但如果使用三價鈦作為還原劑、使用焦磷酸鹽作為錯合劑,則即使在不含有不含氮的有機硫醇等促進劑的情況下,也能夠穩定地形成厚鍍錫層。
在本實施方式的無電解鍍錫浴中,作為促進劑,能夠使用硫的含氧酸代替不含氮的有機硫醇,或者不含氮的有機硫醇與硫的含氧酸一起使用。作為硫的含氧酸,能舉例出:連二硫酸、連三硫酸、連四硫酸、連二亞硫酸以及硫代硫酸等。它們也可以是鹽的狀態。作為鹽,能舉例出:鈉鹽、鉀鹽以及銨鹽等。具體而言,能舉例出:連四硫酸鈉、連四硫酸鉀、連三硫酸鈉、連二硫酸鈉、連二亞硫酸鈉、硫代硫酸鈉、硫代硫酸鉀以及硫代硫酸銨等。利用硫的含氧酸,能夠促進鍍層析出。硫的含氧酸的濃度較佳為0.1mg/L以上,更佳為1 mg/L以上,並且較佳為10g/L以下,更佳為1g/L以下。
本實施方式的無電解鍍錫液也可以含有抗氧化劑。能夠使抗氧化劑例如是鄰苯二酚、鄰苯三酚(pyrogallol)、間苯二酚、對苯二酚、抗壞血酸及山梨糖醇等中的任意一種以上。從鍍浴的穩定性的觀點來看,抗氧化劑的濃度較佳為0.1g/L以上,並且較佳為50g/L以下,更佳為10g/L以下。
本實施方式的無電解鍍錫浴的pH值較佳為5.0以上,更佳為7.0以上,並且較佳為10.0以下,更佳為9.0以下。為了使pH值在適當範圍內,能夠使用pH調節劑。pH調整劑能夠使用磷酸、鹽酸、硫酸以及硝酸等無機酸;甲酸、乙酸、蘋果酸和乳酸等有機酸。也能夠使用磷酸緩衝劑等具有緩衝作用的化合物。除此以外,也可以含有界面活性劑和光亮劑等。
使表面側層123析出時的無電解鍍錫浴的浴溫較佳為40℃以上,更佳為60℃以上,並且較佳為90℃以下,更佳為80℃以下。鍍覆時間較佳為10分鐘以上,並且較佳為180分鐘以下,更佳為60分鐘以下。
本實施方式的無電解鍍錫浴能夠通過電解還原處理等將隨著鍍覆的進行而從三價氧化成四價的鈦再次還原為三價後再加以使用。四價鈦向三價鈦的還原,例如能夠通過圖2所示的電解還原槽201進行。電解還原槽201被陽離子交換膜213劃分為陽極室211和陰極室212。在陽極室211中布置有由鈦-鉑合金等形成的陽極215,在陰極室212中布置有由金屬錫等形成的陰極216。通過在陽極室211中置入硫酸等陽極液,在陰極室212中置入鍍液並使電流流通,四價鈦便能夠在陰極216上被還原為三價鈦。作為副反應,錫離子被還原成金屬,H+被還原而產生氫氣。
從四價鈦向三價鈦的還原,能夠通過批次處理進行,但也能夠與鍍覆處理並行進行。於此情況,使鍍液在進行鍍覆處理的鍍槽和電解還原槽201的陰極室212之間循環即可。於此情況,可以採用將鍍槽內的一定量的鍍液向電解還原槽送出,在電解還原處理結束後再送回鍍槽的方法,也可以採用使鍍液在鍍槽和電解還原槽之間連續循環的連續循環方式。
本實施方式的電子元件的製造方法能夠在印刷線路板和晶圓等上穩定地形成膜厚為0.5μm以上的鍍錫膜。因此,即使在安裝時的熱歷程大的情況下,也能夠避免鍍錫膜與基底金屬合金化而消失的情況出現,從而能夠大幅提升連接可靠性。因此,作為需要確保連接可靠性的電子元件的製造方法等是有用的。
<實施例>
以下,使用實施例對本發明進一步加以說明。以下實施例為示例,並沒有限定本發明。
<連接可靠性試驗>
使用規定的鍍浴,在球柵陣列(BGA)基板(上村工業製)上形成了具有基材側層、金屬催化劑、表面側層的層壓膜。使用了助熔劑(529D-1、千住金屬製)將焊球(φ0.6mm的Sn-3.0Ag-0.5Cu類焊球、千住金屬製)接合到形成有層壓膜的BGA基板上。焊球的接合是通過下述方式進行的,即:以最高溫度240℃對BGA基板進行回流處理後,安裝焊球,在安裝好焊球後再次以最高溫度240℃進行回流處理。
對回流後的焊球進行焊球拉拔測試,求出破壞模式下的焊料斷裂率,將焊料斷裂率為80%以上的情況評價為良好(連接),將焊料斷裂率小於80%的情況評價為不良(斷開)。
<無電解鍍錫浴>
配製了含有下述物質的鍍浴作為鍍浴A:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有氯化鈦(III)5g/L,作為錯合劑含有焦磷酸鉀200g/L,作為不含氮的有機硫醇含有硫代蘋果酸2g/L。
配製了含有下述物質的鍍浴作為鍍浴B:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有氯化鈦(III)5g/L,作為錯合劑含有乙二胺四乙酸(EDTA)50g/L,作為不含氮的有機硫醇含有硫代蘋果酸2g/L。
配製了含有下述物質的鍍浴作為鍍浴C:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有硼氫化鈉0.5g/L,作為錯合劑含有焦磷酸鉀200g/L,作為不含氮的有機硫醇含有硫代蘋果酸2g/L。
配製了含有下述物質的鍍浴作為鍍浴D:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有硼氫化鈉0.5g/L,作為錯合劑含有乙二胺四乙酸(EDTA)50g/L,作為不含氮的有機硫醇含有硫代蘋果酸2g/L。
配製了含有下述物質的鍍浴作為鍍浴E:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有氯化鈦(III)5g/L,作為錯合劑含有焦磷酸鉀200g/L,作為硫的含氧酸含有硫代硫酸鈉100mg/L。
配製了含有下述物質的鍍浴作為鍍浴F:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有氯化鈦(III)5g/L,作為錯合劑含有焦磷酸鉀200g/L,作為硫的含氧酸含有連二亞硫酸鈉1g/L。
配製了含有下述物質的鍍浴作為鍍浴G:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有氯化鈦(III)5g/L,作為錯合劑含有焦磷酸鉀200g/L,作為硫的含氧酸含有連四硫酸鉀1g/L。
配製了含有下述物質的鍍浴作為鍍浴H:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有氯化鈦(III)5g/L,作為錯合劑含有乙二胺四乙酸(EDTA)50g/L,作為硫的含氧酸含有硫代硫酸鈉100mg/L。
配製了含有下述物質的鍍浴作為鍍浴I:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有硼氫化鈉0.5g/L,作為錯合劑含有焦磷酸鉀200g/L,作為硫的含氧酸含有硫代硫酸鈉100mg/L。
配製了含有下述物質的鍍浴作為鍍浴J:作為錫化合物含有氯化錫(II)以錫濃度計為10g/L,作為還原劑含有硼氫化鈉0.5g/L,作為錯合劑含有乙二胺四乙酸(EDTA)50g/L,作為硫的含氧酸含有硫代硫酸鈉100mg/L。
所配製的無電解鍍錫浴的組成匯總起來示於表1和表2。
<浴穩定性>
確認將所配製的無電解鍍錫浴在70℃的鍍覆溫度下靜置1小時之際是否因浴分解而產生析出(燒杯析出)。如果沒有產生析出,評為良好;如果產生了析出,則評為不良。
(實施例1)
對由銅形成的基底層(基材層)的表面進行脫脂、軟蝕刻以及酸洗作為預處理。將鈀催化劑賦予在預處理後的基底層上,通過無電解鍍鎳浴(無電解鍍鎳液NPR-4、上村工業製)形成了厚度為2.0μm的基材側層。對基材側層賦予銀(Ag)作為金屬催化劑後,使用無電解鍍浴A形成了厚度為0.5μm的表面側層。鍍覆時間為15分鐘,鍍覆溫度為70℃。需要說明的是,使用X射線螢光膜厚測量儀(FT150,Hitachi High-Tech Science製)測量了膜厚。
即使在鍍覆溫度即70℃下靜置了1小時的情況下,也未因浴分解而產生燒杯析出,鍍浴穩定。在相同條件下在BGA基板上形成皮膜,進行了連接可靠性試驗,其結果為連接良好。
(實施例2)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例1相同。連接可靠性試驗的結果為良好。
(實施例3)
除了將金(Au)作為金屬催化劑以外,其他都與實施例1相同。連接可靠性試驗的結果為良好。
(實施例4)
對由鋁-銅合金形成的基底層的表面進行了脫脂、酸洗、一次浸鋅處理、酸洗、二次浸鋅處理作為預處理。將鈀催化劑賦予在預處理後的基底層上,通過無電解鍍鎳浴(無電解鍍鎳液NPR-4、上村工業製)形成了厚度為2.0μm的基材側層。將銀(Ag)作為金屬催化劑賦予在基材側層後,使用無電解鍍浴A形成了厚度為0.5μm的表面側層。鍍覆時間為15分鐘,鍍覆溫度為70℃。
在相同條件下在BGA基板上形成皮膜,進行了連接可靠性試驗,其結果為連接良好。
(實施例5)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例4相同。連接可靠性試驗的結果為良好。
(實施例6)
除了將金(Au)作為金屬催化劑以外,其他都與實施例4相同。連接可靠性試驗的結果為良好。
(比較例1)
除了未將金屬催化劑賦予在基材側層上以外,其他都與實施例1相同。未發生錫的析出,未能形成表面側層。在未形成表面側層的狀態下進行了連接可靠性試驗,其結果為連接不良。
(比較例2)
除了未將金屬催化劑賦予在基材側層上以外,其他都與實施例4相同。未發生錫的析出,未能形成表面側層。在未形成表面側層的狀態下進行了連接可靠性試驗,其結果為連接不良。
(比較例3)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例1相同。連接可靠性試驗的結果為不良。
(比較例4)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例2相同。連接可靠性試驗的結果為不良。
(比較例5)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例3相同。連接可靠性試驗的結果為不良。
(比較例6)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例4相同。連接可靠性試驗的結果為不良。
(比較例7)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例5相同。連接可靠性試驗的結果為不良。
(比較例8)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例6相同。連接可靠性試驗的結果為不良。
(比較例9)
除了使用無電解鍍錫浴B、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例1相同。當在鍍覆溫度下靜置了1小時之際發生了燒杯析出,鍍浴不穩定。連接可靠性試驗的結果為不良。
(比較例10)
除了使用無電解鍍錫浴B、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例2相同。連接可靠性試驗的結果為不良。
(比較例11)
除了使用無電解鍍錫浴B、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例3相同。連接可靠性試驗的結果為不良。
(比較例12)
除了使用無電解鍍錫浴B、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例4相同。連接可靠性試驗的結果為不良。
(比較例13)
除了使用無電解鍍錫浴B、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例5相同。連接可靠性試驗的結果為不良。
(比較例14)
除了使用無電解鍍錫浴B、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例6相同。連接可靠性試驗的結果為不良。
(比較例15)
除了設鍍覆時間為25分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.5μm以外,其他都與比較例9相同。連接可靠性試驗的結果為良好,但由於鍍浴不穩定,因此難以反復使用。
(比較例16)
除了使用無電解鍍錫浴C、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例1相同。當在鍍覆溫度下靜置了1小時之際發生了燒杯析出,鍍浴不穩定。連接可靠性試驗的結果為不良。
(比較例17)
除了使用無電解鍍錫浴C、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例2相同。連接可靠性試驗的結果為不良。
(比較例18)
除了使用無電解鍍錫浴C、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例3相同。連接可靠性試驗的結果為不良。
(比較例19)
除了使用無電解鍍錫浴C、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例4相同。連接可靠性試驗的結果為不良。
(比較例20)
除了使用無電解鍍錫浴C、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例5相同。連接可靠性試驗的結果為不良。
(比較例21)
除了使用無電解鍍錫浴C、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例6相同。連接可靠性試驗的結果為不良。
(比較例22)
除了設鍍覆時間為25分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.5μm以外,其他都與比較例17相同。連接可靠性試驗的結果為良好,但由於鍍浴不穩定,因此難以反復使用。
(比較例23)
除了使用無電解鍍錫浴D、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例1相同。當在鍍覆溫度下靜置了1小時之際發生了燒杯析出,鍍浴不穩定。連接可靠性試驗的結果為不良。
(比較例24)
除了使用無電解鍍錫浴D、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例2相同。連接可靠性試驗的結果為不良。
(比較例25)
除了使用無電解鍍錫浴D、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例3相同。連接可靠性試驗的結果為不良。
(比較例26)
除了使用無電解鍍錫浴D、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例4相同。連接可靠性試驗的結果為不良。
(比較例27)
除了使用無電解鍍錫浴D、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例5相同。連接可靠性試驗的結果為不良。
(比較例28)
除了使用無電解鍍錫浴D、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例6相同。連接可靠性試驗的結果為不良。
(比較例29)
除了設鍍覆時間為25分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.5μm以外,其他都與比較例25相同。連接可靠性試驗的結果為良好,但由於鍍浴不穩定,因此難以反復使用。
將各實施例及比較例的結果匯總起來示於表3~表7。
(實施例7)
與實施例1一樣,將基材層的材料設為Cu、將賦予在基材側層上的金屬催化劑設為Ag,使用無電解鍍錫浴E在70℃下進行15分鐘的鍍敷,形成了厚度為0.5μm的表面側層。即使在鍍覆溫度即70℃下靜置了1小時的情況下,也未因浴分解而產生燒杯析出,鍍浴穩定。連接可靠性試驗的結果為良好。
(實施例8)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例7相同。連接可靠性試驗的結果為良好。
(實施例9)
除了將金(Au)作為金屬催化劑以外,其他都與實施例7相同。連接可靠性試驗的結果為良好。
(實施例10)
與實施例4一樣,將基材層的材料設為Al-Cu、將賦予在基材側層上的金屬催化劑設為Ag,使用無電解鍍錫浴E在70℃下進行15分鐘的鍍敷,形成了厚度為0.5μm的表面側層。連接可靠性試驗的結果為良好。
(實施例11)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例10相同。連接可靠性試驗的結果為良好。
(實施例12)
除了將金(Au)作為金屬催化劑以外,其他都與實施例10相同。連接可靠性試驗的結果為良好。
(實施例13)
除了使用無電解鍍錫浴F以外,其他都與實施例7相同。即使在鍍覆溫度即70℃下靜置了1小時的情況下,也未因浴分解而產生燒杯析出,鍍浴穩定。連接可靠性試驗的結果為良好。
(實施例14)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例13相同。連接可靠性試驗的結果為良好。
(實施例15)
除了將金(Au)作為金屬催化劑以外,其他都與實施例13相同。連接可靠性試驗的結果為良好。
(實施例16)
除了使用無電解鍍錫浴F以外,其他都與實施例10相同。連接可靠性試驗的結果為良好。
(實施例17)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例16相同。連接可靠性試驗的結果為良好。
(實施例18)
除了將金(Au)作為金屬催化劑以外,其他都與實施例16相同。連接可靠性試驗的結果為良好。
(實施例19)
除了使用無電解鍍錫浴G以外,其他都與實施例7相同。即使在鍍覆溫度即70℃下靜置了1小時的情況下,也未因浴分解而產生燒杯析出,鍍浴穩定。連接可靠性試驗的結果為良好。
(實施例20)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例19相同。連接可靠性試驗的結果為良好。
(實施例21)
除了將金(Au)作為金屬催化劑以外,其他都與實施例19相同。連接可靠性試驗的結果為良好。
(實施例22)
除了使用無電解鍍錫浴G以外,其他都與實施例10相同。連接可靠性試驗的結果為良好。
(實施例23)
除了將鈀(Pd)作為金屬催化劑以外,其他都與實施例22相同。連接可靠性試驗的結果為良好。
(實施例24)
除了將金(Au)作為金屬催化劑以外,其他都與實施例22相同。連接可靠性試驗的結果為良好。
(比較例30)
除了未將金屬催化劑賦予在表面側層上以外,其他都與實施例7相同。未發生錫的析出,未能形成表面側層。在未形成表面側層的狀態下進行了連接可靠性試驗,其結果為連接不良。
(比較例31)
除了未將金屬催化劑賦予在表面側層上以外,其他都與實施例10相同。未發生錫的析出,未能形成表面側層。在未形成表面側層的狀態下進行了連接可靠性試驗,其結果為連接不良。
(比較例32)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例7相同。連接可靠性試驗的結果為不良。
(比較例33)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例8相同。連接可靠性試驗的結果為不良。
(比較例34)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例9相同。連接可靠性試驗的結果為不良。
(比較例35)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例10相同。連接可靠性試驗的結果為不良。
(比較例36)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例11相同。連接可靠性試驗的結果為不良。
(比較例37)
除了設鍍覆時間為12分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.4μm以外,其他都與實施例12相同。連接可靠性試驗的結果為不良。
(比較例38)
除了使用無電解鍍錫浴H、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例7相同。在鍍覆溫度即70℃下靜置了1小時的情況下發生了燒杯析出,鍍浴不穩定。連接可靠性試驗的結果為不良。
(比較例39)
除了使用無電解鍍錫浴H、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例8相同。連接可靠性試驗的結果為不良。
(比較例40)
除了使用無電解鍍錫浴H、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例9相同。連接可靠性試驗的結果為不良。
(比較例41)
除了使用無電解鍍錫浴H、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例10相同。連接可靠性試驗的結果為不良。
(比較例42)
除了使用無電解鍍錫浴H、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例11相同。連接可靠性試驗的結果為不良。
(比較例43)
除了使用無電解鍍錫浴H、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例12相同。連接可靠性試驗的結果為不良。
(比較例44)
除了設鍍覆時間為25分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.5μm以外,其他都與比較例38相同。連接可靠性試驗的結果為良好,但由於鍍浴不穩定,因此難以反復使用。
(比較例45)
除了使用無電解鍍錫浴I、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例7相同。在鍍覆溫度即70℃下靜置了1小時的情況下發生了燒杯析出,鍍浴不穩定。連接可靠性試驗的結果為不良。
(比較例46)
除了使用無電解鍍錫浴I、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例8相同。連接可靠性試驗的結果為不良。
(比較例47)
除了使用無電解鍍錫浴I、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例9相同。連接可靠性試驗的結果為不良。
(比較例48)
除了使用無電解鍍錫浴I、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例10相同。連接可靠性試驗的結果為不良。
(比較例49)
除了使用無電解鍍錫浴I、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例11相同。連接可靠性試驗的結果為不良。
(比較例50)
除了使用無電解鍍錫浴I、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例12相同。連接可靠性試驗的結果為不良。
(比較例51)
除了設鍍覆時間為25分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.5μm以外,其他都與比較例46相同。連接可靠性試驗的結果為良好,但由於鍍浴不穩定,因此難以反復使用。
(比較例52)
除了使用無電解鍍錫浴J、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例7相同。在鍍覆溫度即70℃下靜置了1小時的情況下發生了燒杯析出,鍍浴不穩定。連接可靠性試驗的結果為不良。
(比較例53)
除了使用無電解鍍錫浴J、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例8相同。連接可靠性試驗的結果為不良。
(比較例54)
除了使用無電解鍍錫浴J、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例9相同。連接可靠性試驗的結果為不良。
(比較例55)
除了使用無電解鍍錫浴J、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例10相同。連接可靠性試驗的結果為不良。
(比較例56)
除了使用無電解鍍錫浴J、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例11相同。連接可靠性試驗的結果為不良。
(比較例57)
除了使用無電解鍍錫浴J、設鍍覆時間為5分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.1μm以外,其他都與實施例12相同。連接可靠性試驗的結果為不良。
(比較例58)
除了設鍍覆時間為25分鐘、鍍覆溫度為70℃、表面側層的膜厚為0.5μm以外,其他都與比較例54相同。連接可靠性試驗的結果為良好,但由於鍍浴不穩定,因此難以反復使用。
將各實施例及比較例的結果匯總起來示於表8~表14。
<表9>
-產業上的可利用性-
本發明的電子元件的製造方法能夠穩定地製造連接可靠性優異且足夠厚的鍍Sn膜,因而作為電子元件等的製造方法是有用的。
101:基材
102:層壓膜
121:基材側層
122:催化劑
123:表面側層
201:電解還原槽
211:陽極室
212:陰極室
213:陽離子交換膜
215:陽極
216:陰極
圖1是示出一實施方式所關係之層壓膜的剖視圖;
圖2是示出電解還原槽之一例的示意圖。
101:基材層
102:層壓膜
121:基材側層
122:催化劑
123:表面側層
Claims (4)
- 一種電子元件的製造方法,其包括基材側層形成步驟、催化劑賦予步驟以及表面側層形成步驟,在前述基材側層形成步驟中,通過無電解鍍鎳浴或無電解鍍鎳合金浴在由銅或銅合金、或者鋁或鋁合金形成的基材上形成由鎳或鎳合金形成的基材側層, 在前述催化劑賦予步驟中,將選自由金、鈀、鉑、銀、銠、鈷、錫、銅、銥、鋨以及釕所構成的組中的一種或兩種以上的金屬作為催化劑賦予在前述基材側層上, 在前述表面側層形成步驟中,通過含有三價鈦作為還原劑並含有焦磷酸鹽作為錯合劑的無電解鍍錫浴或無電解鍍錫合金浴來形成表面側層, 在前述表面側層形成步驟中,形成厚度為0.5μm以上的表面側層。
- 如請求項1所記載之電子元件的製造方法,其中前述無電解鍍錫浴或前述無電解鍍錫合金浴含有不含氮的有機硫醇。
- 如請求項1所記載之電子元件的製造方法,其中前述無電解鍍錫浴或前述無電解鍍錫合金浴含有硫的含氧酸。
- 如請求項1到3中任一項所記載之電子元件的製造方法,其中前述電子元件的製造方法還包括鈦還原步驟,在該鈦還原步驟中,通過電解處理將在前述表面側層形成步驟中在前述無電解鍍錫浴或前述無電解鍍錫合金浴中生成的四價鈦還原成三價鈦, 前述鈦還原步驟是在具有由陽離子交換膜隔開的陽極室和陰極室的還原處理槽中,使進行形成前述表面側層的步驟的鍍槽中的鍍液的一部分向前述陰極室移動而進行的, 前述表面側層形成步驟和前述鈦還原步驟並行進行。
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