TWI753581B - 層合體及其製造方法 - Google Patents

層合體及其製造方法 Download PDF

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Publication number
TWI753581B
TWI753581B TW109132667A TW109132667A TWI753581B TW I753581 B TWI753581 B TW I753581B TW 109132667 A TW109132667 A TW 109132667A TW 109132667 A TW109132667 A TW 109132667A TW I753581 B TWI753581 B TW I753581B
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Taiwan
Prior art keywords
nickel
film layer
gold
layer
plating
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TW109132667A
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English (en)
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TW202125594A (zh
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古谷章
小島忠昭
鈴木広志
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日商昭和電工股份有限公司
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
    • H01L21/687—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches
    • H01L21/68714—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches the wafers being placed on a susceptor, stage or support
    • H01L21/68757—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches the wafers being placed on a susceptor, stage or support characterised by a coating or a hardness or a material
    • C—CHEMISTRY; METALLURGY
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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
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
    • B32B15/015—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium the said other metal being copper or nickel or an alloy thereof
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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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    • C23C18/00—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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    • C23C18/1651—Two or more layers only obtained by electroless plating
    • C—CHEMISTRY; METALLURGY
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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
    • C—CHEMISTRY; METALLURGY
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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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    • C23C18/1689—After-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
    • C23C18/1601—Process or apparatus
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    • C23C18/1692—Heat-treatment
    • C23C18/1696—Control of atmosphere
    • 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
    • C23C18/1848—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by electrochemical pretreatment
    • 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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    • 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
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    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • 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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    • C—CHEMISTRY; METALLURGY
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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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    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract

本發明之課題在於提供可適用於半導體製造裝置之構成構件，耐蝕性優異之金屬材料。本發明之層合體具有金屬基材、形成於前述金屬基材上之含鎳鍍敷被膜層、形成於前述含鎳鍍敷被膜層上之金鍍敷被膜層，且前述金鍍敷被膜層之針孔藉由厚度8nm以上之氟化鈍態被膜封孔。

Description

層合體及其製造方法
本發明有關層合體及其製造方法。更具體而言，有關適合作為半導體製造裝置等之構成構件之層合體及其製造方法。
以往，以半導體製造製程，於乾蝕刻步驟及製造裝置之清潔等中，使用氟、氯化氫、三氯化硼、三氟化氮、三氟化氯、溴化氫等之鹵素系之反應性及腐蝕性強的特殊氣體(以下亦稱為「腐蝕性氣體」)。
然而，前述腐蝕性氣體與環境下之水分反應而水解時，產生氟化氫、草酸及氯化氫等之生成物。前述生成物由於容易腐蝕使用前述腐蝕性氣體之際之閥、接頭、配管及反應腔室等之構成構件的金屬表面，故成為問題。
另一方面，鍍敷表面之針孔亦可能成為腐蝕進行之原因。針孔之發生要因認為係例如因鍍敷反應產生之氫氣於鍍敷被膜形成時成為泡而阻礙成膜，且殘留於基材之雜質(氧化膜、污物、油分等)於前處理等步驟無法去除而阻礙成膜等之複數種原因。
迄今，為了實現耐腐蝕性之提高，而對金屬基材實施鎳-磷合金鍍敷，進行形成鎳之氟化鈍態被膜之方法(例如參考專利文獻1~3)，但該等方法有不充分之情況。
又，亦有對金屬基材實施鎳-鎢合金鍍敷，利用藉由氟化反應而生成之WF6 之標準生成焓之形成低溫且厚膜之鎳的氟化鈍態被膜之方法，但就電解鍍敷法之方面可適用之構件受到限制而有制約(參考專利文獻4)。 [先前技術文獻] [專利文獻]
專利文獻1：日本專利第2954716號公報 專利文獻2：日本專利第3094000號公報 專利文獻3：日本特開2004-360066號公報 專利文獻4：日本特開2008-056978號公報
[發明欲解決之課題]
本發明係欲解決如上述以往技術所伴隨之問題者，而提供可適用於半導體製造裝置之構成構件，進而耐蝕性優異之金屬材料，以及提供前述金屬材料之製造方法。 [用以解決課題之手段]
本發明有關例如以下之[1]~[12]。 [1] 一種層合體，其具有金屬基材、形成於前述金屬基材上之含鎳鍍敷被膜層、及形成於前述含鎳鍍敷被膜層上之金鍍敷被膜層，且前述金鍍敷被膜層之針孔藉由厚度8nm以上之氟化鈍態被膜封孔。
[2] 如前述[1]之層合體，其中前述金屬基材含有選自不鏽鋼、鐵、鋁、鋁合金、銅及銅合金所成之群之至少1種金屬。
[3] 如前述[1]或[2]之層合體，其中於前述金屬基材與前述含鎳鍍敷被膜層之間具有鎳噴擊層。 [4] 如前述[1]至[3]中任一項之層合體，其中前述含鎳鍍敷被膜層自前述金屬基材側起依序含有：磷濃度為8質量%以上且未達10質量%之鎳-磷合金鍍敷層(1)及磷濃度為10質量%以上12質量%以下之鎳-磷合金鍍敷層(2)。
[5] 如前述[1]至[4]中任一項之層合體，其中前述金鍍敷被膜層自前述含鎳鍍敷被膜層側起依序含有取代型金鍍敷被膜層及還原型金鍍敷被膜層。
[6] 一種半導體製造裝置之構成構件，其係由如前述[1]至[5]中任一項之層合體而成。 [7] 一種層合體之製造方法，其包含：於金屬基材上形成含鎳鍍敷被膜層之步驟(A)，於前述含鎳鍍敷被膜層上形成金鍍敷被膜層之步驟(B)，及於前述金鍍敷被膜層之針孔，形成厚度8nm以上之氟化鈍態被膜之封孔處理步驟(C)。
[8] 如前述[7]之層合體之製造方法，其中前述封孔處理步驟(C)係於氟化氣體濃度8體積%以上及溫度100~150℃之環境下進行。 [9] 如前述[7]或[8]之層合體之製造方法，其中前述金屬基材含有選自不鏽鋼、鐵、鋁、鋁合金、銅及銅合金所成之群之至少1種金屬。
[10] 如前述[7]至[9]中任一項之層合體之製造方法，其中於前述步驟(A)之前，包含對金屬基材以電流密度5~20 A/dm2 之條件實施鎳噴擊處理之步驟。
[11] 如前述[7]至[10]中任一項之層合體之製造方法，其中前述步驟(A)包含形成磷濃度為8質量%以上且未達10質量%之鎳-磷合金鍍敷層(1)之步驟(a1)，及於該步驟(a1)之後，形成磷濃度為10質量%以上12質量%以下之鎳-磷合金鍍敷層(2)之步驟(a2)。
[12] 如前述[7]至[11]中任一項之層合體之製造方法，其中前述步驟(B)包含形成取代型金鍍敷被膜層之步驟(b1)，及於該步驟(b1)之後，形成還原型金鍍敷被膜層之步驟(b2)。 [發明效果]
依據本發明，提供耐腐蝕性尤其對酸之耐腐蝕性優異之層合體。
以下針對本發明之一實施形態具體說明。 本發明之一實施形態之層合體具有金屬基材、形成於前述金屬基材上之含鎳鍍敷被膜層、及形成於前述含鎳鍍敷被膜層上之金鍍敷被膜層，且前述金鍍敷被膜層之針孔藉由厚度8nm以上之氟化鈍態被膜封孔。
本發明一實施形態之層合體之製造方法包含：於金屬基材上形成含鎳鍍敷被膜層之步驟(A)，於前述含鎳鍍敷被膜層上形成金鍍敷被膜層之步驟(B)，及於前述金鍍敷被膜層之針孔，形成厚度8nm以上之氟化鈍態被膜之封孔處理步驟(C)。
[金屬基材] 本發明一實施形態使用之金屬基材係至少表面由金屬所成之基材。作為前述金屬基材並未特別限定，舉例為半導體製造裝置之構成構件中一般使用之金屬，較佳為不鏽鋼、鐵、鋁、鋁合金、銅及銅合金。
前述金屬基材由於與含鎳鍍敷被膜層之密著性強固，故作為步驟(A)之前處理，亦可實施脫脂、酸洗淨或鎳噴擊處理等之對應於基材之處理。鎳噴擊處理係使用含鎳鍍敷液之預鍍敷處理，且鎳噴擊處理之電流密度較佳為5~20 A/dm2 ，更佳為5~10 A/dm2 。且鎳噴擊處理時間較佳為5秒以上5分鐘以下。
[含鎳鍍敷被膜層] 含鎳鍍敷被膜層係藉由步驟(A)形成於前述金屬基材上。又對前述金屬基材實施鎳噴擊處理之情況，金屬基材與鎳鍍敷被沒膜層之間具有鎳噴擊層。
基於耐腐蝕性提高之觀點，含鎳鍍敷被膜層較佳含有磷，較佳自前述金屬基材側起依序含有：磷濃度為8質量%以上且未達10質量%之鎳-磷合金鍍敷層(1)及磷濃度為10質量%以上12質量%以下之鎳-磷合金鍍敷層(2)。
含鎳鍍敷被膜層中之鎳含量，於將含鎳鍍敷被膜全體設為100質量%時，較佳為80質量%以上，更佳為85~95質量%，特佳為88~92質量%。藉由使鎳含量為前述範圍，可增加被膜層中之磷比例，可發揮優異之耐腐蝕性。又，若層合磷濃度改變之無電解鎳-磷合金鍍敷被膜，則由於針孔缺陷形成於不同位置而成膜，故外部干擾不易直接到達基材，可期待耐腐蝕性提高。
＜步驟(A)＞ 含鎳鍍敷被膜層可使用含有鎳鹽、作為還原劑之磷化合物之無電解鍍敷浴形成於金屬基材上。作為鎳鹽舉例為例如硫酸鎳、氯化鎳、乙酸鎳、碳酸鎳等。作為磷化合物舉例為例如亞磷酸鈉、亞磷酸鉀等。
前述步驟(A)較佳包含形成鎳-磷合金鍍敷層(1)之步驟(a1)，及於該步驟(a1)之後，形成鎳-磷合金鍍敷層(2)之步驟(a2)。
前述鎳-磷合金鍍敷層(1)之成膜速度較佳為20~30 μm/h(小時)，更佳為22~25 μm/h(小時)，前述鎳-磷合金鍍敷層(2)之成膜速度較佳為10 ~15 μm/h(小時)，更佳為11~13 μm/h(小時)。藉由如此形成鎳-磷合金鍍敷層(1)及(2)，可提高耐腐蝕性。鎳-磷合金鍍敷層(1)及(2)之膜厚均較佳為5μm以上，更佳為7~25μm，基於不易發生針孔之被膜性能及成本之觀點，又更佳為10~20μm。
[金鍍敷被膜層] 金鍍敷被膜層係藉由步驟(B)形成於前述含鎳鍍敷被膜層上。
金鍍敷被膜層中之金含量，於將金鍍敷被膜層全體設為100質量%之情況，較佳為90質量%以上，更佳為99質量%以上，特佳為99.9質量%以上。藉由將金含量設為前述範圍，本發明一實施形態之層合體之耐腐蝕性穩定。金含量係藉由雜質定量法求出，亦即將金鍍敷以王水溶解，以原子吸光分析及高頻感應耦合電漿(ICP)發光分光分析測定。
金鍍敷被膜之厚度，基於不易產生針孔之被膜性能及成本之觀點，較佳為0.1μm~1μm，更佳為0.2~ 0.9μm，特佳為0.3~0.8μm。貴金屬鍍敷被膜若厚則針孔減少，係以往技術已知，雖期待高的耐腐蝕性，但由於價格昂貴故較佳為適當厚度。
＜步驟(B)＞ 作為前述金鍍敷被膜層之形成方法並未特別限定，但較佳為無電解金鍍敷法。無電解金鍍敷法較佳進行取代型金鍍敷之後，進行還原型金鍍敷。亦即，前述步驟(B)較佳包含形成取代型金鍍敷被膜層之步驟(b1)，及於該步驟(b1)之後，形成還原型金鍍敷被膜層之步驟(b2)。
取代型金鍍敷係自鎳被膜溶解出鎳，藉由此時釋出之電子使溶液中之金離子還原為金鍍敷被膜而析出。還原型金鍍敷係溶液中之金離子藉由因還原劑之氧化反應而釋出之電子而被還原，析出金鍍敷被膜。
作為無電解金鍍敷液舉例為包含例如氰化金鉀、氯化金、亞硫酸金、硫代硫酸金等之鍍敷浴等，作為還原劑舉例為例如氫氧化鈉、二甲基胺硼烷、六亞甲基四胺、具有碳數3以上之烷基與複數胺基之鏈狀聚胺等。
取代型金鍍敷較佳於50~90℃實施3~7分鐘，更佳於65~75℃實施3~7分鐘，還原型金鍍敷較佳於55~65℃實施7~15分鐘，更佳於58~62℃實施7~15分鐘，可形成金鍍敷被膜層。
[氟化鈍態被膜] 前述金鍍敷被膜層表面藉由步驟(C)之氟化處理，而使前述金鍍敷被膜層之針孔以氟化鈍態被膜予以封孔。
氟化鈍態被膜於圖1(b)中，僅形成於鎳-磷合金鍍敷層(2b)露出面。亦即僅於氟化鈍態被膜5之上下方向成長而形成，不形成於金鍍敷被膜層3之針孔內部側面或金鍍敷被膜層3之最表面，且不超過金鍍敷被膜層3之上端。
氟化鈍態被膜之厚度通常為8nm以上，較佳為10~20nm，更佳為12~18nm。藉由使氟化鈍態被膜之厚度為上述範圍，使氟化鈍態被膜之耐久性等成為實用上適用者。又，此處所謂氟化鈍態被膜之厚度係所得層合體之層合方向之長度，例如圖1(b)中於氟化鈍態被膜5之上下方向之長度。
＜步驟(C)＞ 步驟(C)係使用氟化氣體使自經過前述步驟(A)及(B)之金鍍敷被膜層之針孔露出之含鎳鍍敷被膜層表面強制氟化，形成氟化鈍態被膜，進行針孔封孔處理。
步驟(C)係於氟化氣體濃度較佳為8體積%以上，更佳10~25體積%之環境下進行，氟化溫度較佳為100 ~150℃，更佳為105~145℃，更佳為110~140℃。
所謂氟化氣體係作為氟化處理使用之氣體，為選自氟(F2 )、三氟化氯(ClF3 )及氟化氮(NF3 )所成之群中之至少1種氣體，或該氣體以惰性氣體稀釋之氣體的總稱。
例如，使用三氟化氯之情況，以60~100℃熱分解產生氟自由基，該自由基可利用於氟化反應。又，使用三氟化氮之情況，藉由電漿能分解產生氟自由基，該自由基可利用於氟化反應。
作為伴隨前述氟化氣體之稀釋氣體舉例為氮氣、氬氣等之惰性氣體，較佳為氮氣。 將前述氟化氣體稀釋而使用之情況，其濃度可根據反應條件適當設定。例如氟之情況下，考慮成本等，較佳以10%左右之濃度使用。
金屬基材為不鏽鋼之情況，較佳於150~190℃，更佳於155~175℃，為鋁合金之情況，較佳於140~160℃，更佳於145~155℃氟化。藉由成膜溫度為前述範圍，無電解鎳-合金鍍敷與金鍍敷之熱擴散之均衡良好。
氟化處理時間係隨形成之氟化鈍態被膜之厚度而異，但為了發揮優異之耐腐蝕性，較佳為20~100小時，更佳為30~80小時。 [實施例]
以下基於實施例更具體說明本發明，但本發明不限定於該等實施例。
[實施例1] ＜步驟(A)＞ 於加工成縱15mm橫15mm厚1mm之試驗片尺寸之不鏽鋼(SUS316L)表面，實施脫脂、酸洗淨及鎳噴擊處理作為前處理。前述酸洗淨係使用鹽酸作為洗淨劑，於室溫進行25秒。實施該鎳噴擊處理之不鏽鋼表面，使用無電解鎳-磷鍍敷藥劑「NIMUDEN(商標)NSX」(上村工業(股)製)，於鍍敷溫度90℃、pH4.5~4.8之條件下，以成膜速度10μm/ 25分鐘，形成成膜時之磷含量為8質量%以上且未達10質量%之無電解鎳-磷合金鍍敷被膜層(1)。其次，使用無電解鎳-磷鍍敷藥劑「NIMUDEN(商標)HDX」(上村工業(股)製)，以成膜速度10μm/25分鐘，形成成膜時之磷含量為10質量%以上12質量%以下之無電解鎳-磷合金鍍敷被膜層(2)。藉此，於實施鎳噴擊處理之不鏽鋼上形成合計20μm厚之含鎳鍍敷被膜層。
＜步驟(B)＞ 依序使用2種無電解金鍍敷液「FLASH GOLD NC(取代型)」及「SELF GOLD OTK-IT(還原型)」(均為奧野製藥工業(股)製)，於步驟(A)形成之含鎳鍍敷被膜層上，分別依據進行取代型鍍敷溫度70℃之5分鐘處理及還原型鍍敷溫度60℃之10分鐘處理，形成合計0.6μm厚之金鍍敷被膜層。
＜步驟(C)＞ 將於步驟(A)及(B)形成之具有含鎳鍍敷被膜層及金鍍敷被膜層之不鏽鋼安裝於常壓氣相流通式反應爐之內部，將爐內溫度升溫至115℃。隨後將大氣以氮氣置換，接著導入以氮氣稀釋之10體積%氟氣將反應爐內之氮氣置換為10體積%氟氣。完全置換後，該狀態保持36小時，將施工金鍍敷時產生之針孔所致之基底無電解鎳-磷被膜之露出部分強制氟化，形成氟化鈍態被膜。所得氟化鈍態被膜以W-SEM「JSM-IT200」(日本電子股(製))分析之結果，確認氟化鈍態被膜之膜厚為10nm。又，此處所謂氟化鈍態被膜之膜厚係所得層合體之層方向長，例如圖1(b)中之氟化鈍態被膜5之上下方向之長度。
[實施例2] 實施例1之步驟(C)中使用經氮氣稀釋之10體積%氟氣之強制氟化時間變更為72小時以外，以與實施例1同樣之方法，形成氟化鈍態被膜。所得氟化鈍態被膜以與實施例1同樣求出膜厚之結果，確認為13nm。
[實施例3] 替代實施例1中之不鏽鋼(SUS316L)而使用鋁合金(A5052)，實施脫脂、活性化處理、酸洗淨及鋅取代處理作為前處理後，與實施例1同樣之方法實施步驟(A)及(B)。
前述活性化處理使用酸性氟化銨與硝酸之混合酸作為處理劑，於室溫進行30秒。前述酸洗淨係使用硝酸作為洗淨劑，於室溫進行25秒。前述鋅取代處理係使用鋅酸鹽浴作為處理劑，於室溫進行25秒。又，前述酸洗淨及前述鋅取代處理係以上述條件分別各進行2次。
上述步驟(C)中除了強制氟化溫度設為105℃以外，與實施例2同樣，於金鍍敷被膜上形成氟化鈍態被膜。所得氟化鈍態被膜與實施例1同樣求出膜厚之結果，確認為10nm。
[比較例1] 僅實施實施例1之步驟(A)，於不鏽鋼表面形成含鎳鍍敷被膜層合計20μm。
[比較例2] 實施實施例1之步驟(A)及(B)後，使具有含鎳鍍敷被膜層及金鍍敷被膜層之不鏽鋼板於大氣中露出，形成自然氧化被膜。所得自然氧化被膜與實施例1同樣求出膜厚之結果，確認為7nm。
[比較例3] 實施實施例1之步驟(A)後，進行以下處理。將具有含鎳鍍敷被覆層之不鏽鋼安裝於常壓氣相流通式反應爐之內部，將爐內溫度升溫至300℃。隨後將大氣以氮氣置換，接著導入100體積%氧氣將氮氣置換為氧氣。完全置換後，該狀態保持12小時。其次導入以氮氣稀釋之10體積%氟氣，該狀態保持12小時，藉此於含鎳鍍敷被膜層上形成氟化鎳(NiF2 )膜。隨後，為了實現成膜穩定化而注入氮氣12小時。
[評價] 針對上述實施例1~3及比較例1~3所得之金屬基材表面上之被膜，以下述方法進行評價。評價結果示於表1。
＜鹽酸耐腐蝕試驗＞ 將縱15mm×橫15mm×厚1mm之試驗片於35質量%鹽酸溶液中於25℃浸漬5小時。基於浸漬前後之質量減少量[mg/dm2 ]，以下述基準評價鹽酸耐腐蝕性。 (評價基準) A：未達0.1 mg/dm2 B：0.1 mg/dm2 以上且未達3 mg/dm2 C：3 mg/dm2 以上
[表1]
   實施例1 實施例2 實施例3 比較例1 比較例2 比較例3
金屬基材 SUS SUS Al SUS SUS SUS
含鎳鍍敷被膜層 有 有 有 有 有 有
金鍍敷被膜層 有 有 有 無 有 無
封孔處理之有無 有 有 有 無 有 無
氟化鈍態被膜厚[nm] 10 13 10 - - -
自然氧化被膜厚[nm] - - - - 7 -
NiF2 處理 無 無 無 無 無 有
鹽酸耐腐蝕性 B A B C C C
表中，SUS表示不鏽鋼(SUS316L)，Al表示鋁合金(A5052)。
1:金屬基材 2:含鎳鍍敷被膜層 2a:鎳-磷合金鍍敷層(1) 2b:鎳-磷合金鍍敷層(2) 3:金鍍敷被膜層 4:針孔 5:氟化鈍態被膜
[圖1]顯示封孔處理前後之層合體的概略圖((a)：封孔處理前，(b)：封孔處理後)。
1:金屬基材
2:含鎳鍍敷被膜層
2a:鎳-磷合金鍍敷層(1)
2b:鎳-磷合金鍍敷層(2)
3:金鍍敷被膜層
4:針孔
5:氟化鈍態被膜

Claims (12)

  1. 一種層合體，其具有金屬基材、形成於前述金屬基材上之含鎳鍍敷被膜層、及形成於前述含鎳鍍敷被膜層上之金鍍敷被膜層，且前述金鍍敷被膜層之針孔藉由厚度8nm以上之氟化鈍態被膜封孔。
  2. 如請求項1之層合體，其中前述金屬基材含有選自不鏽鋼、鐵、鋁、鋁合金、銅及銅合金所成之群之至少1種金屬。
  3. 如請求項1或2之層合體，其中於前述金屬基材與前述含鎳鍍敷被膜層之間具有鎳噴擊層。
  4. 如請求項1或2之層合體，其中前述含鎳鍍敷被膜層自前述金屬基材側起依序含有：磷濃度為8質量%以上且未達10質量%之鎳-磷合金鍍敷層(1)及磷濃度為10質量%以上12質量%以下之鎳-磷合金鍍敷層(2)。
  5. 如請求項1或2之層合體，其中前述金鍍敷被膜層自前述含鎳鍍敷被膜層側起依序含有取代型金鍍敷被膜層及還原型金鍍敷被膜層。
  6. 一種半導體製造裝置之構成構件，其係由如請求項1至5中任一項之層合體而成。
  7. 一種層合體之製造方法，其包含：於金屬基材上形成含鎳鍍敷被膜層之步驟(A)，於前述含鎳鍍敷被膜層上形成金鍍敷被膜層之步驟(B)，及 於前述金鍍敷被膜層之針孔，形成厚度8nm以上之氟化鈍態被膜之封孔處理步驟(C)。
  8. 如請求項7之層合體之製造方法，其中前述封孔處理步驟(C)係於氟化氣體濃度8體積%以上及溫度100~150。℃之環境下進行。
  9. 如請求項7或8之層合體之製造方法，其中前述金屬基材含有選自不鏽鋼、鐵、鋁、鋁合金、銅及銅合金所成之群之至少1種金屬。
  10. 如請求項7或8之層合體之製造方法，其中於前述步驟(A)之前，包含對金屬基材以電流密度5~20A/dm2之條件實施鎳噴擊處理之步驟。
  11. 如請求項7或8之層合體之製造方法，其中前述步驟(A)包含形成磷濃度為8質量%以上且未達10質量%之鎳-磷合金鍍敷層(1)之步驟(a1)，及於該步驟(a1)之後，形成磷濃度為10質量%以上12質量%以下之鎳-磷合金鍍敷層(2)之步驟(a2)。
  12. 如請求項7或8之層合體之製造方法，其中前述步驟(B)包含形成取代型金鍍敷被膜層之步驟(b1)，及於該步驟(b1)之後，形成還原型金鍍敷被膜層之步驟(b2)。
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