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TWI624563B - 於感光性樹脂之表面形成金屬層的方法 - Google Patents

於感光性樹脂之表面形成金屬層的方法 Download PDF

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Publication number
TWI624563B
TWI624563B TW106123627A TW106123627A TWI624563B TW I624563 B TWI624563 B TW I624563B TW 106123627 A TW106123627 A TW 106123627A TW 106123627 A TW106123627 A TW 106123627A TW I624563 B TWI624563 B TW I624563B
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Taiwan
Prior art keywords
photosensitive resin
item
patent application
metal layer
application scope
Prior art date
Application number
TW106123627A
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English (en)
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TW201908521A (zh
Inventor
黃堂傑
莊朝欽
許家福
Original Assignee
律勝科技股份有限公司
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Priority to TW106123627A priority Critical patent/TWI624563B/zh
Priority to CN201810373443.3A priority patent/CN109252148B/zh
Application granted granted Critical
Publication of TWI624563B publication Critical patent/TWI624563B/zh
Priority to JP2018120432A priority patent/JP6585777B2/ja
Priority to KR1020180073348A priority patent/KR102105988B1/ko
Priority to US16/020,901 priority patent/US20190017175A1/en
Publication of TW201908521A publication Critical patent/TW201908521A/zh

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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
    • 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
    • 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
    • C23C18/48—Coating with alloys
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J7/065—Low-molecular-weight organic substances, e.g. absorption of additives in the surface of the article
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    • C08J7/12—Chemical modification
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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
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    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1862—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by radiant energy
    • C23C18/1868—Radiation, e.g. UV, laser
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1886—Multistep pretreatment
    • C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • 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
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    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
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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
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    • C23C18/2026—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by radiant energy
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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
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    • 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
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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
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    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
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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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    • C23C18/00—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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    • 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
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Abstract

本發明提供一種於特定之感光性樹脂表面形成金屬層的方法，包含以下步驟：(i)前處理，使用鹼性水溶液對感光性樹脂之表面進行清潔及預活化；(ii)表面改質，將感光性樹脂浸泡於表面改質劑中，形成有機改質層；(iii)表面活化，加入觸媒金屬離子，使有機改質層與觸媒金屬離子形成金屬離子錯合物；(iv)還原反應，以還原劑將金屬離子錯合物還原成奈米金屬觸媒；(v)化學鍍，將感光性樹脂浸泡於化學鍍液中，形成導電金屬層；(vi)熱處理，將感光性樹脂於100-250℃的條件下烘烤；及(vii)電鍍增厚，將烘烤後的感光性樹脂進行電鍍，增厚導電金屬層。

Description

於感光性樹脂之表面形成金屬層的方法
本發明關於一種於感光性樹脂之表面形成金屬層的方法，特別是指對特定之感光性聚醯亞胺樹脂表面金屬化，以形成金屬層的方法。
聚醯亞胺為軟性印刷電路板及IC封裝業界常用的基材材料，其為具有可撓性、耐化學溶劑性(耐化性)、耐高溫且不導電的有機材料。隨著電子產品的薄型化及多功能化之趨勢，高佈線密度及導孔微小化已成軟性印刷電路板的基本需求。然而，一般非感光性的聚醯亞胺耐化性佳，因此不容易藉由化學蝕刻製作平面及垂直導體溝槽，往往需要透過雷射鑽孔或乾式蝕孔搭配光阻進行微導孔的加工，再施以化學處理活化，方能形成金屬層，製程較為複雜。然而即使在非感光性的聚醯亞胺上能夠形成金屬層，此金屬層與聚醯亞胺的結合強度並不高，且在製作多層板時，容易被高溫烘壓製程破壞。
而感光性聚醯亞胺有別於傳統聚醯亞胺，其具有感光成孔的加工特色，無需額外使用雷射鑽孔或乾式蝕孔搭配光阻進行垂直導電單元的製作。然而，目前仍未存在一種實用的方法，能夠在感光性聚醯亞胺樹脂上 形成高結合強度的金屬層。
本發明提供一種於特定之感光性樹脂之表面形成金屬層的方法，其包括前處理步驟、濕式化學表面改質步驟，以及金屬化步驟。此方法可以應用在特定的感光性聚醯亞胺樹脂，結合其感光成孔的特性，能使多層積體垂直導電單元之金屬導線製作製程更為精簡。
根據本發明，提供一種於感光性樹脂之表面形成金屬層的方法。所述感光性樹脂包含(a)環氧化合物、(b)感光性聚醯亞胺及(c)光起始劑。環氧化合物佔感光性樹脂之固體重量的5-40%。感光性聚醯亞胺具有式(1)之結構：
其中m、n各自獨立為1至600；X為四價有機基團，其主鏈部份含脂環族基團；Y為二價有機基團，其主鏈部份含矽氧烷基團；Z為二價有機基團，其支鏈部份至少含酚基或羧基，此感光性聚醯亞胺佔感光性樹脂之固體重量的30-90%。光起始劑佔感光性樹脂之固體重量的0.1-15%。
所述於感光性樹脂之表面形成金屬層的方法包含下列步驟：
(i)前處理，使用鹼性水溶液對感光性樹脂之表面進行清潔及預活化；
(ii)表面改質，將感光性樹脂浸泡於表面改質劑中，於感光性樹脂上形成有機改質層。表面改質劑選自式(2)至式(6)至少其中一種胺基化合物之水 溶液： 其中n=1-3，R1為NH2、NHCH3或NH(CH3)2，R2為H或CmH2mNH2，m=1-3，R3為NH2、SH或OH，R4為SH、、
(iii)表面活化，加入觸媒金屬離子，使有機改質層與觸媒金屬離子於該感光性樹脂表面形成金屬離子錯合物。
(iv)還原反應，以還原劑將附著於感光性樹脂表面的金屬離子錯合物 還原成奈米金屬觸媒。
(v)化學鍍，將已形成奈米金屬觸媒的感光性樹脂浸泡於化學鍍液中，形成導電金屬層。
(vi)熱處理，將已形成導電金屬層的感光性樹脂於100-250℃的條件下烘烤。以及
(vii)電鍍增厚，將烘烤後的感光性樹脂進行電鍍，增厚導電金屬層。
一實施例中，表面改質步驟(ii)中的浸泡時間為1-20分，且表面改質劑之胺基化合物的濃度為0.1-10g/L，溫度為30-75℃。
一實施例中，表面活化步驟(iii)加入的觸媒金屬離子為包括Cu、Ni、Ag、Au或Pd離子的酸性水溶液。
一實施例中，還原反應步驟(iv)加入的還原劑為次磷酸鈉、硼氫化鈉、二甲基胺硼烷或聯胺水溶液。
一實施例中，化學鍍步驟(v)加入的化學鍍液包含銅離子、鎳離子、螯合劑、還原劑、pH緩衝劑、界面活性劑及pH調整劑。
一實施例中，化學鍍液中銅離子之來源為硝酸銅、硫酸銅、氯化銅或氨基磺酸銅。
一實施例中，化學鍍液中鎳離子之來源為硫酸鎳、硝酸鎳、氯化鎳、硫酸鎳或氨基磺酸鎳。
一實施例中，化學鍍液中之螯合劑為檸檬酸鈉、酒石酸鉀鈉或乙二胺四乙酸。
一實施例中，化學鍍步驟(v)形成的導電金屬層厚度為50-200nm。
一實施例中，熱處理步驟(vi)的烘烤時間為10-60分。
一實施例中，前處理步驟(i)更包括以平行紫外光或電漿對感光性樹脂之表面進行清潔及預活化。
一實施例中，當以平行紫外光進行前處理步驟(i)時，平行紫外光的照射波長為100-280nm，表面累積照輻強度為1-20J/cm2，且照射時間為1-30分。
一實施例中，當以電漿進行前處理步驟(i)時，輸出功率為100-5000W，且處理時間為0.5-30分。
一實施例中，電鍍增厚步驟(vii)係將導電金屬層之厚度增加至12-18μm。
為使本發明之上述及其他方面更為清楚，下文特舉實施例，配合文字進行詳細說明。
本發明所述之在感光性樹脂之表面形成金屬層的方法包括下列步驟：
(i)表面處理(前處理)
(ii)表面開環(改質)
(iii)觸媒粒子吸附(表面活化)
(iv)觸媒粒子還原
(v)化學鍍(無電電鍍)
(vi)熱處理
(vii)電鍍
(viii)除水風乾
本發明中，作為基材(基板)在其上形成金屬層的感光性樹脂，主要成分是感光性聚醯亞胺。感光性樹脂之成分包括(a)環氧化合物、(b)感光性聚醯亞胺以及(c)光起始劑。感光性聚醯亞胺具有式(1)之結構：
其中m、n各自獨立為1至600；X為四價有機基團，其主鏈部份含脂環族基團，較佳為不含苯環的脂環族基團，包含(但不限於)、
Y為二價有機基團，其主鏈部份含矽氧烷基團，例如下列所示：
其中Y之鏈長以短為佳(p=0)，最長可到p=20，過長將破壞感光性聚醯亞胺之性質。Z為二價有機基團，其支鏈部份至少含酚基或羧基。酚基或羧基的含量約佔感光性聚醯亞胺莫耳數之5-30%，並可藉由調整支鏈覆蓋基的莫耳比來控制顯影的時間，當支鏈酚基或羧基的含量較高，則鹼性顯影液對其溶解性較佳，則可提升其顯影性。Z可包括但不限於下列基團：
感光性聚醯亞胺佔感光性樹脂之固體重量的30-90%；環氧化合物佔感光性樹脂之固體重量的5-40%；而光起始劑佔感光性樹脂之固體重量的0.1-15%。這類的感光性聚醯亞胺由於具表面有矽氧烷基團、醯亞胺環基團與羧基等基團，較容易與本發明使用之表面改質劑的胺基進行耦合反應。
(i)表面處理(前處理)
首先，對感光性樹脂基材進行表面清潔及預活化。使用的方法包括照射平行紫外光、電漿以及以鹼性水溶液浸泡，可以選擇其中一種，或多種一起配合使用。當以平行紫外光進行前處理時，平行紫外光的照射波長為100-280nm，表面累積照輻強度為1-20J/cm2，且照射時間為1-30分；當以電漿進行前處理時，輸出功率為100-5000W，且處理時間為0.5-30分。本實施例中係以平行紫外光照射10分，接著以40℃、5M濃度之KOH水溶液，浸泡感光性樹脂基材數分鐘後取出。浸泡鹼性水溶液的目的係為了使式(1)之感光性樹脂表面的羰基(C=O)開環，形成一層含有大量羰酸基(COOH)的有機改質層。接著以去離子水沖洗，將表面殘留的鹼性水溶液或其他有機物沖洗乾淨。
(ii)表面改質
再來，浸泡感光性樹脂於表面改質劑內，對感光性樹脂表面的羰酸基(COOH)及羥基(OH)官能基表面進一步改質。表面改質劑可選自下式(2)至式(6)至少其中一種胺基化合物之水溶液，且胺基化合物的濃度介於胺基化合物的濃度為0.1-10g/L： 其中n=1-3，R1為NH2,NHCH3或NH(CH3)2，R2為H或CmH2mNH2，m為1-3，R3為NH2、SH或OH，R4為SH、、、 或，且改質反應溫度為30-75℃(較佳為 50℃)，浸泡時間為1-20分。表面改質劑可與感光性樹脂表面之矽氧烷基團、醯亞胺環基團及羧基等有機基團進行耦合反應。
(iii)表面活化
接著，將感光性樹脂基材浸泡於於一活化液，活化液例如為含有鈀金屬離子水溶液，其包含0.4g/L之氯化鈀及0.4g/L之氯化銨，溫度為30℃且浸泡時間為2分鐘，活化液中的金屬離子將與有機改質層形成錯合物。在其他實施例中，也可以使用其他金屬離子的酸性水溶液作為活化液，例如Cu、Ni、Ag或Au。
(iv)還原反應
接續將上述步驟(iii)中活化後的感光型樹脂基材浸泡於一含有還原劑的水溶液中，進行鈀金屬離子的還原反應。還原液組成含有28.6g/L次磷酸鈉及去離子水，操作溫度為30℃且浸泡時間為2分鐘。亦可使用如硼氫化鈉、二甲基胺硼烷或聯胺水溶液等的其它種類還原劑。
(v)化學鍍
目前的感光性樹脂基材的表面已有觸媒離子還原後產生的金屬鈀。接著進行無電電鍍，使奈米金屬顆粒沉積於感光型聚醯亞胺基板表面並形成一金屬導電層(膜)，其沉積厚度為50-200nm。無電電鍍液較佳選用無甲醛配方的無電電鍍液，配成pH=9且操作溫度為50℃的水溶液。
一實施例中，化學鍍液較佳包含銅離子、鎳離子、螯合劑、還原劑、pH緩衝劑、界面活性劑及pH調整劑。其中銅離子之來源為硝酸銅、硫酸銅、氯化銅或氨基磺酸銅；鎳離子之來源為硫酸鎳、硝酸鎳、氯化鎳、硫酸鎳或氨基磺酸鎳；螯合劑為檸檬酸鈉、酒石酸鉀鈉或乙二胺四乙酸。
(vi)熱處理
再來，透過熱處理促使感光性樹脂基材表面與金屬導電層間的交聯反應，進而提升感光性樹脂基材表面與金屬導電層間的附著力。本實施例中，熱處理的操作溫度範圍為150℃且反應時間為60分鐘，然時間跟溫度可依需求進行調整。
(vii)電鍍
最後，選用含有化學添加劑的電鍍銅液進行電鍍增厚，加厚金屬導電層，其電鍍厚度為18μm。所使用的電鍍銅溶液組成如下：CuSO4.5H2O：100g/L
H2SO4：127.4g/L
PEG8000(聚乙二醇)：0.2g/L
SPS(聚二硫二丙烷磺酸鈉)：0.004g/L
經上述實施例步驟處理後，形成於感光性樹脂上的金屬層，其抗撕強度可達0.7kgf/cm；在150℃的溫度下放置168小時後，其抗撕強度依然可維持於0.6kgf/cm。反之，不進行表面改質(省略步驟ii)直接形成的金屬層，其抗撕強度僅有0.2kgf/cm左右，可知本發明的方法能夠提高金屬層的抗撕強度達3倍以上。
另外，在一般多層電路板的製程中，每層金屬層完成後需要經過循環烘壓製程，以多次高溫高壓之製程方式壓合增層之高分子層與金屬層，以增加異質材料層間的密合度。然而，傳統在聚醯亞胺/感光性聚醯亞胺上形成金屬層的方法，其形成的金屬層經由循環烘壓處理後，反而會大幅降低金屬層的抗撕強度(低於1/10)。然而，本發明在感光性樹脂上形成的金屬 層，在經由多次高溫185℃及高壓24.5kgf/cm的循環烘壓製程後，其抗撕強度依然可維持0.5kgf/cm左右，因此能夠用於多層板的製作。
綜上所述，依照本發明之步驟，於感光性樹脂上形成的金屬層，不但具有較高的抗撕強度，且可應用於多層軟性印刷電路板、多層HDI印刷電路板之增層製程及IC載板的半加成製程。此外本發明之方法相較傳統非感光性樹脂及其他非感光性高分子之濕式金屬化及增層製程相對簡易，傳統非感光性樹脂皆須仰賴乾式蝕刻、雷射鑽孔及機械鑽孔的加工方法，接續再搭配除膠渣/除光阻、中和處理、粗化及金屬化製程等製作程序；而本發明使用之感光性樹脂可透過照紫外光成型，不會產生膠渣，省略除膠渣與中和處理之程序，可有效節省製程成本、降低多道藥水處理之失效率並提升生產速率。
雖然本發明以實施例說明如上，惟此些實施例並非用以限制本發明。本領域之通常知識者在不脫離本發明技藝精神的範疇內，當可對此些實施例進行等效實施或變更，故本發明的保護範圍應以其後所附之申請專利範圍為準。

Claims (13)

  1. 一種於感光性樹脂之表面形成金屬層的方法，所述感光性樹脂包含(a)環氧化合物、(b)感光性聚醯亞胺及(c)光起始劑；該環氧化合物佔該感光性樹脂之固體重量的5-40%；該感光性聚醯亞胺具有式(1)之結構：
    Figure TWI624563B_C0001
    其中m、n各自獨立為1至600；X為四價有機基團，其主鏈部份含脂環族基團；Y為二價有機基團，其主鏈部份含矽氧烷基團；Z為二價有機基團，其支鏈部份至少含酚基或羧基，該感光性聚醯亞胺佔該感光性樹脂之固體重量的30-90%；該光起始劑佔該感光性樹脂之固體重量的0.1-15%，所述方法包含下列步驟：(i)前處理，使用鹼性水溶液及平行紫外光或電漿對該感光性樹脂之表面進行清潔及預活化；(ii)表面改質，將該感光性樹脂浸泡於表面改質劑中，於該感光性樹脂上形成有機改質層，該表面改質劑選自式(2)至式(6)至少其中一種胺基化合物之水溶液：
    Figure TWI624563B_C0002
    Figure TWI624563B_C0003
    Figure TWI624563B_C0004
    Figure TWI624563B_C0005
    及
    Figure TWI624563B_C0006
    其中n=1-3，R1為NH2、NHCH3或NH(CH3)2，R2為H或CmH2mNH2，m=1-3，R3為NH2、SH或OH，R4為SH、
    Figure TWI624563B_C0007
    (iii)表面活化，加入觸媒金屬離子，使該有機改質層與該觸媒金屬離子於該感光性樹脂表面形成金屬離子錯合物；(iv)還原反應，以還原劑將附著於該感光性樹脂表面的該金屬離子錯合物還原成奈米金屬觸媒；(v)化學鍍，將已形成奈米金屬觸媒的該感光性樹脂浸泡於化學鍍液中，形成導電金屬層；(vi)熱處理，將已形成導電金屬層的該感光性樹脂於100-250℃的條件下烘烤；以及(vii)電鍍增厚，將烘烤後的感光性樹脂進行電鍍，增厚該導電金屬層。
  2. 如申請專利範圍第1項所述之方法，其中表面改質步驟(ii)中的浸泡時間為1-20分，且該表面改質劑之胺基化合物的濃度為0.1-10g/L，溫度為30-75℃。
  3. 如申請專利範圍第1項所述之方法，其中表面活化步驟(iii)加入的該觸媒金屬離子為包括Cu、Ni、Ag、Au或Pd離子的酸性水溶液。
  4. 如申請專利範圍第1項所述之方法，其中還原反應步驟(iv)加入的該還原劑為次磷酸鈉、硼氫化鈉、二甲基胺硼烷或聯胺水溶液。
  5. 如申請專利範圍第1項所述之方法，其中化學鍍步驟(v)加入的該化學鍍液包含銅離子、鎳離子、螯合劑、還原劑、pH緩衝劑、界面活性劑及pH調整劑。
  6. 如申請專利範圍第5項所述之方法，其中該銅離子之來源為硝酸銅、硫酸銅、氯化銅或氨基磺酸銅。
  7. 如申請專利範圍第5項所述之方法，其中該鎳離子之來源為硫酸鎳、硝酸鎳、氯化鎳、硫酸鎳或氨基磺酸鎳。
  8. 如申請專利範圍第5項所述之方法，其中該螯合劑為檸檬酸鈉、酒石酸鉀鈉或乙二胺四乙酸。
  9. 如申請專利範圍第1項所述之方法，其中化學鍍步驟(v)形成的該導電金屬層厚度為50-200nm。
  10. 如申請專利範圍第1項所述之方法，其中熱處理步驟(vi)的烘烤時間為10-60分。
  11. 如申請專利範圍第1項所述之方法，其中當以平行紫外光進行前處理時，該平行紫外光的照射波長為100-280nm，表面累積照輻強度為1-20J/cm2，且照射時間為1-30分。
  12. 如申請專利範圍第1項所述之方法，其中當以電漿進行前處理時，輸出功率為100-5000W，且處理時間為0.5-30分。
  13. 如申請專利範圍第1項所述之方法，其中該電鍍增厚步驟(vii)中，係將該導電金屬層之厚度增加至12-18μm。
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