TW202115281A - 積層體及其製造方法 - Google Patents

積層體及其製造方法 Download PDF

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TW202115281A
TW202115281A TW109128341A TW109128341A TW202115281A TW 202115281 A TW202115281 A TW 202115281A TW 109128341 A TW109128341 A TW 109128341A TW 109128341 A TW109128341 A TW 109128341A TW 202115281 A TW202115281 A TW 202115281A
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Taiwan
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nickel
film layer
gold
layer
plating film
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TW109128341A
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TWI745036B (zh
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古谷章
小島忠昭
鈴木広志
那賀文彰
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日商昭和電工股份有限公司
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    • 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
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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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    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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    • 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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    • B32B15/017—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of aluminium or an aluminium alloy, another layer being formed of an alloy based on a non ferrous metal other than aluminium
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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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    • 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
    • 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
    • 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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    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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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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    • 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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    • 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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    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
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Abstract

本發明之課題在於提供一種金屬材料，其能夠適用於半導體製造裝置的構成構件，且耐蝕性(特別是對於酸的耐蝕性)為優異。本發明相關的積層體具有：金屬基材、形成於前述金屬基材上的第一含鎳鍍敷被膜層、形成於前述第一含鎳鍍敷被膜層上的金鍍敷被膜層、形成於前述金鍍敷被膜層上的第二含鎳鍍敷被膜層及形成於前述第二含鎳鍍敷被膜層上的氟化鎳被膜層。

Description

積層體及其製造方法
本發明為關於積層體及其製造方法。更具體而言，關於一種適合作為半導體製造裝置等的構成構件的積層體及其製造方法。
以往以來，在半導體製造製程中，於乾式蝕刻步驟及清潔製造裝置等時，使用著氟、氯化氫、三氯化硼、三氟化氮、三氟化氯、溴化氫等的鹵素系具有強的反應性及腐蝕性的特殊氣體(以下亦稱為「腐蝕性氣體」)。
然而，前述腐蝕性氣體與環境下的水分進行反應並水解時，會產生氟化氫、草酸及氯化氫等的生成物。在使用前述腐蝕性氣體之際的閥、連接器、配管及反應膜腔室等的構成構件的金屬表面，會容易因為前述生成物而造成腐蝕，而成為問題。
迄今為止為了試圖提升耐蝕性，已進行對於金屬基材施予鎳-磷合金鍍敷來形成鎳的氟化鈍態膜的方法(例如參考專利文獻1～3)，但該等的方法有時並非充分。
進而，鍍敷表面的針孔亦可能是加速腐蝕的原因。產生針孔的要因，認為是有多種的原因，例如，於鍍敷被膜的形成時，因鍍敷反應所產生的氫氣成為氣泡而阻礙了成膜，或是，於前處理步驟中未去除殘留在基材上的雜質(氧化膜、污漬、油分等)而阻礙了成膜等。對此，專利文獻4中揭示一種手法，其於金鍍敷上形成硬質的合金鍍敷層，以提升耐磨耗性及可防止起因於氣體或水分的氧化、硫化等而造成的變色或腐蝕。 [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]日本專利第2581021號公報
[發明所欲解決之課題]
依據本發明人的研究得知，如專利文獻1～3般於鎳-磷合金鍍敷表面來形成鎳的氟化鈍態膜的方法中，會產生以鎳-磷合金鍍敷的針孔為起點的腐蝕，且對於鹽酸耐蝕性有不足之情形。又，於專利文獻4的方法中，由於最表面層為合金鍍敷，而具有無法期望耐蝕性的顯著提升之類的課題。
因此，本發明之課題在於提供一種金屬材料，其能夠適用於半導體製造裝置的構成構件，且耐蝕性(特別是對於酸的耐蝕性)為優異。 [解決課題之手段]
本發明為關於例如以下的[1]～[14]。 [1]. 一種積層體，具有：金屬基材、形成於前述金屬基材上的第一含鎳鍍敷被膜層、形成於前述第一含鎳鍍敷被膜層上的金鍍敷被膜層、形成於前述金鍍敷被膜層上的第二含鎳鍍敷被膜層及形成於前述第二含鎳鍍敷被膜層上的氟化鎳被膜層。
[2]. 如前述[1]之積層體，其中，前述金鍍敷被膜層的針孔係以鎳單質(elemental substance)的金屬來封孔，且前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔係以金單質的金屬來封孔。 [3]. 如前述[1]或[2]之積層體，其中，前述金屬基材包含選自由不鏽鋼、鐵、鋁、鋁合金、銅及銅合金所組成之群組之至少1種的金屬。
[4]. 如前述[1]～[3]中任一項之積層體，其中，於前述金屬基材與前述第一含鎳鍍敷被膜層之間，及於前述金鍍敷被膜層與前述第二含鎳鍍敷被膜層之間具有鎳觸擊電鍍層。 [5]. 如前述[1]～[4]中任一項之積層體，其中，前述第一含鎳鍍敷被膜層包含磷濃度為8質量%以上未滿10質量%的鎳-磷合金鍍敷層，且前述第二含鎳鍍敷被膜層包含磷濃度為10質量%以上12質量%以下的鎳-磷合金鍍敷層。
[6]. 如前述[1]～[5]中任一項之積層體，其中，前述金鍍敷被膜層從前述第一含鎳鍍敷被膜層側起依序包含取代型金鍍敷被膜層及還原型金鍍敷被膜層。 [7]. 如前述[1]～[6]中任一項之積層體，其中，前述氟化鎳被膜層的厚度為70nm以上。
[8]. 一種積層體的製造方法，包含：於金屬基材上形成第一含鎳鍍敷被膜層之步驟(A)、於前述第一含鎳鍍敷被膜層上形成金鍍敷被膜層之步驟(B)、於前述金鍍敷被膜層上形成第二含鎳鍍敷被膜層之步驟(C)及於前述第二含鎳鍍敷被膜層上形成氟化鎳被膜層之步驟(D)。
[9]. 如前述[8]之積層體的製造方法，其中，於前述步驟(C)與前述步驟(D)之間包含步驟(X)，該步驟(X)係藉由以溫度250℃以上之條件下來將步驟(C)所得到的積層體進行加熱處理，而將前述金鍍敷被膜層的針孔以鎳單質的金屬來封孔，且將前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔以金單質的金屬來封孔。
[10]. 如前述[8]或[9]之積層體的製造方法，其中，前述步驟(D)係在氟氣濃度8體積%以上及溫度250℃以上的環境下來進行。 [11]. 如前述[8]～[10]中任一項之積層體的製造方法，其中，於前述步驟(A)之前及前述步驟(C)之前，包含以電流密度3～20A/dm2 之條件下來對於金屬基材施予鎳觸擊電鍍處理之步驟。
[12]. 如前述[8]～[11]中任一項之積層體的製造方法，其中，前述步驟(A)包含形成磷濃度為8質量%以上未滿10質量%的鎳-磷合金鍍敷層之步驟，且前述步驟(C)包含形成磷濃度為10質量%以上12質量%以下的鎳-磷合金鍍敷層之步驟。
[13]. 如前述[8]～[12]中任一項之積層體的製造方法，其中，前述步驟(B)包含形成取代型金鍍敷被膜層之步驟(b1)，與於該步驟(b1)之後形成還原型金鍍敷被膜層之步驟(b2)。 [14]. 一種半導體製造裝置的構成構件，其係由如前述[1]～[7]中任一項之積層體所組成。 [發明的效果]
依據本發明可提供一種耐蝕性(特別是對於酸的耐蝕性)為優異的積層體。
[實施發明之最佳形態]
以下，對於本發明的一實施形態來具體地進行說明。 本發明的一實施形態的積層體具有：金屬基材、形成於前述金屬基材上的第一含鎳鍍敷被膜層、形成於前述第一含鎳鍍敷被膜層上的金鍍敷被膜層、形成於前述金鍍敷被膜層上的第二含鎳鍍敷被膜層及形成於前述第二含鎳鍍敷被膜層上的氟化鎳被膜層。
又，本發明的一實施形態的積層體，較佳為前述金鍍敷被膜層的針孔係以鎳單質的金屬來封孔，且前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔係以金單質的金屬來封孔。
本發明的一實施形態的積層體的製造方法，包含：於金屬基材上形成第一含鎳鍍敷被膜層之步驟(A)、於前述第一含鎳鍍敷被膜層上形成金鍍敷被膜層之步驟(B)、於前述金鍍敷被膜層上形成第二含鎳鍍敷被膜層之步驟(C)及於前述第二含鎳鍍敷被膜層上形成氟化鎳被膜層之步驟(D)。
又，本發明的一實施形態的積層體的製造方法，較佳為於前述步驟(C)與前述步驟(D)之間包含步驟(X)，該步驟(X)係藉由以溫度250℃以上及2小時以上之條件下來將步驟(C)所得到的積層體進行加熱處理，而將前述金鍍敷被膜層的針孔以鎳單質的金屬來封孔，且將前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔以金單質的金屬來封孔。
[金屬基材] 使用於本發明的一實施形態的金屬基材係至少表面由金屬所組成的基材。作為前述金屬基材並無特別限定，可舉出一般使用於半導體製造裝置的構成構件中的金屬，較佳為不鏽鋼、鐵、鋁、鋁合金、銅及銅合金。
為了使前述金屬基材與含鎳鍍敷被膜層的密著性成為堅固，作為步驟(A)的前處理，可因應基材來施予脫脂、酸洗淨或鎳觸擊電鍍處理等的處理。鎳觸擊電鍍(strike plating)處理係使用含鎳鍍敷浴的預備性鍍敷處理，鎳觸擊電鍍處理時的電流密度較佳為3～20A/dm2 ，又較佳為6～10A/dm2 。又，鎳觸擊電鍍處理的時間較佳為1分鐘以上5分鐘以下。
[第一含鎳鍍敷被膜層] 藉由步驟(A)，而於前述金屬基材上形成第一含鎳鍍敷被膜層。尚，若對於前述金屬基材施予鎳觸擊電鍍處理時，於金屬基材與第一鎳鍍敷被膜層之間具有鎳觸擊電鍍層。
就提升耐蝕性之觀點而言，含鎳鍍敷被膜層較佳為含有磷，以包含磷濃度為8質量%以上未滿10質量%的鎳-磷合金鍍敷層為較佳。
將含鎳鍍敷被膜層整體設為100質量%時，第一含鎳鍍敷被膜層中的鎳含量較佳為80質量%以上，又較佳為85～95質量%，特佳為90～92質量%。藉由使鎳含量成為前述範圍，被膜層中的磷的比率會增加，而可發揮優異的耐蝕性。
＜步驟(A)＞ 可使用包含鎳鹽與作為還原劑的磷化合物的無電解鍍敷浴，而於金屬基材上形成前述第一含鎳鍍敷被膜層。作為鎳鹽，可舉例如硫酸鎳、氯化鎳、乙酸鎳、碳酸鎳等。作為磷化合物，可舉例如次亞磷酸鈉、次亞磷酸鉀等。
前述第一鎳-磷合金鍍敷層的成膜速度較佳為20～30μm/h(小時)，又較佳為22～25μm/h(小時)。第一鎳-磷含有鍍敷被膜層之膜厚較佳為5μm以上，以7～25μm為又較佳，就不易產生針孔的被膜性能及成本之觀點而言，以9～20μm為更佳。
[金鍍敷被膜層] 藉由步驟(B)，而於前述含鎳鍍敷被膜層上形成金鍍敷被膜層。將金鍍敷被膜整體層整體設為100質量%時，金鍍敷被膜中的金含量較佳為90質量%以上，又較佳為99質量%以上，特佳為99.9質量%以上。藉由使金含量成為前述範圍，本申請案發明的積層體的耐蝕性為穩定。金含量係可藉由雜質定量法來求出，即，使用王水來將金鍍敷溶解，並以原子吸光分析及感應耦合電漿質譜(ICP)發光分光分析來進行測量。
就不易產生針孔的被膜性能及成本之觀點而言，金鍍敷被膜的厚度較佳為0.1μm～2μm，又較佳為0.2～1.5μm，特佳為0.3～0.8μm。依據以往的技術，已知當貴金屬鍍敷被膜增厚時針孔將會減少，而可期待高的耐蝕性，但以設定為適當的厚度為佳，因為價格會變得昂貴之緣故。
＜步驟(B)＞ 作為前述金鍍敷被膜層的形成方法並無特別限定，較佳為無電解金鍍敷法(electroless gold plating)。無電解金鍍敷法較佳為於進行取代型(substitution type)金鍍敷後，再進行還原型(reduction type)金鍍敷。即，前述步驟(B)較佳為包含形成取代型金鍍敷被膜層之步驟(b1)，與於該步驟(b1)之後形成還原型金鍍敷被膜層之步驟(b2)。
取代型金鍍敷如下：鎳從鎳被膜中溶解出來，藉由此時所放出的電子來還原溶液中的金離子，而以金鍍敷被膜來進行析出。還原型金鍍敷如下：藉由還原劑的氧化反應中所放出的電子來還原溶液中的金離子，而析出金鍍敷被膜。
作為無電解金鍍敷液，可舉出包含例如氰化金鉀、氯化金、亞硫酸金、硫代硫酸金等的鍍敷浴等；作為還原劑，可舉例如氫氧化鈉、二甲胺硼烷、六亞甲基四胺、具有碳數3個以上的烷基與複數胺基的鏈狀聚胺等。
藉由將取代金鍍敷較佳設為50～90℃、進行3～7分鐘，又較佳設為65～75℃、進行3～7分鐘，將還原型金鍍敷較佳設為55～65℃、進行7～15分鐘，又較佳設為58～62℃、進行7～15分鐘來實施，而可形成金鍍敷被膜層。
[第二含鎳鍍敷被膜層] 藉由步驟(C)，而於前述金鍍敷被膜層上形成第二含鎳鍍敷被膜層。尚，若對於前述金鍍敷被膜層施予鎳觸擊電鍍處理時，於金鍍敷被膜層與第二鎳鍍敷被膜層之間具有鎳觸擊電鍍層。
就提升耐蝕性之觀點而言，含鎳鍍敷被膜層較佳為含有磷，以包含磷濃度為10質量%以上12質量%以下的鎳-磷合金鍍敷層為較佳。
將含鎳鍍敷被膜層整體設為100質量%時，第二含鎳鍍敷被膜層中的鎳含量較佳為80質量%以上，又較佳為85～95質量%，特佳為90～92質量%。藉由使鎳含量成為前述範圍，被膜層中的磷的比率會增加，而可發揮優異的耐蝕性。又，當積層磷濃度為改變的無電解鎳-磷合金鍍敷被膜時，由於在成膜之同時會於不同的位置形成針孔欠陥，而使得外在干擾(disturbance)不易直接到達基材，故可期待提升耐蝕性。
＜步驟(C)＞ 可使用包含鎳鹽與作為還原劑的磷化合物的無電解鍍敷浴，而於金屬基材上形成前述第二含鎳鍍敷被膜層。作為鎳鹽，可舉例如硫酸鎳、氯化鎳、乙酸鎳、碳酸鎳等。作為磷化合物，可舉例如次亞磷酸鈉、次亞磷酸鉀等。
前述第二鎳-磷合金鍍敷層的成膜速度較佳為10～15μm/h(小時)，又較佳為11～13μm/h(小時)。第二鎳-磷合金鍍敷被膜層之膜厚係分別較佳為5μm以上，以7～25μm為又較佳，就不易產生針孔的被膜性能及成本之觀點而言，以10～20μm為更佳。
[封孔處理] 封孔處理係藉由下述之方式來進行：將前述金鍍敷被膜層的針孔以鎳單質的金屬來封孔，且將前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔以金單質的金屬來封孔。
＜步驟(X)＞ 步驟(X)係於前述步驟(C)與後述之步驟(D)之間，藉由將步驟(C)所得到的積層體進行加熱處理來使金屬熱擴散，而將前述金鍍敷被膜層的針孔以鎳單質的金屬來封孔，且將前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔以金單質的金屬來進行封孔處理。可藉由能量分散式X射線分析(EDS)來確認金及鎳單質的存在。 加熱條件較佳為250℃以上進行2小時以上，又較佳為300～350℃進行2～6小時。
[氟化鎳被膜層] 於前述第二含鎳鍍敷被膜層上形成氟化鎳被膜層。氟化鎳被膜層為鈍態被膜。藉由步驟(D)來將前述第二含鎳鍍敷被膜層表面進行氟化處理，而於前述含鎳鍍敷被膜層上形成作為鈍態被膜的氟化鎳被膜層。
氟化鎳被膜層的厚度較佳為70nm以上，又較佳為80～200nm，更佳為100～150nm。藉由使氟化鎳被膜層的厚度成為前述範圍，金鍍敷被膜層與第二含鎳鍍敷被膜層的密著性將會提升。
＜步驟(D)＞ 步驟(D)係在經過前述步驟(A)～(C)及因應所需的前述步驟(X)後，以氟氣將前述含鎳鍍敷被膜層表面進行氟化來形成氟化鎳被膜層。
步驟(D)係以氟氣濃度較佳為8體積%以上，又較佳為10體積%以上的環境下來進行。成膜溫度係佳為250℃以上，又較佳為300℃以上。又，氟化處理時間較佳為2小時以上。作為與氟氣為同伴的氣體，可舉出氮氣等的惰性氣體。於本發明的一實施形態中，藉由上述反應條件，可得到由更厚膜的氟化鎳所組成的氟化鈍態膜，可依據構件的使用目的，藉由調節鎳合金鍍敷皮膜的厚度、反應溫度、反應時間來任意地調整氟化鎳被膜之膜厚。尚，上述反應溫度係指以熱電偶來測量反應爐內的氣體環境的溫度之涵義。 [實施例]
以下為依據實施例來更具體地說明本發明，但本發明並非被限定於該等實施例。積層體的各層(不包括氟化鎳被膜層)的膜厚係由重量的增加部分、層面積與已知的密度來算出。氟化鎳被膜層之膜厚係藉由X射線光電子分光法(XPS)並依後述的方法來算出。
[實施例1] ＜步驟(A)＞ 作為前處理，對於不鏽鋼(SUS316L)的表面施予脫脂、酸洗淨及鎳觸擊電鍍處理。使用無電解鎳-磷鍍敷藥劑「Nimuden(商標)NSX」(上村工業(股)製)，以鍍敷溫度90℃、pH4.5～4.8之條件下進行鍍敷時間25分鐘，而於已施予該鎳觸擊電鍍處理的不鏽鋼的表面上，來形成成膜時的磷含量為8質量%以上未滿10質量%的第一含鎳鍍敷被膜層(膜厚：10μm)。
＜步驟(B)＞ 依序使用2種類的無電解金鍍敷液「Flashgold NC(取代型)」及「Selfgold OTK-IT(還原型)」(皆為奥野製藥工業(股)製)，分別依序進行取代型鍍敷以溫度70℃、5分鐘、及還原型鍍敷以溫度60℃、10分鐘的處理，而於步驟(A)所形成的第一含鎳鍍敷被膜層上形成合計0.6μm厚的金鍍敷被膜層。
＜步驟(C)＞ 與步驟(A)以相同方式，來對於步驟(B)所形成的金鍍敷被膜層的表面施予鎳觸擊電鍍處理。使用無電解鎳-磷鍍敷藥劑「Nimuden(商標)HDX」(上村工業(股)製)，以鍍敷時間50分鐘，於已施予該鎳觸擊電鍍處理的金鍍敷被膜層的表面上，形成成膜時的磷含量為10質量%以上12質量%以下的第二含鎳鍍敷被膜層(膜厚：10μm)。
＜步驟(X)＞ 將具有步驟(A)、步驟(B)及步驟(C)所形成的第一含鎳鍍敷被膜層、金鍍敷被膜層及第二含鎳鍍敷被膜層的不鏽鋼，安裝在常壓氣相流通式反應爐的內部，使爐內溫度升溫至300℃並維持該狀態2小時。
加熱後，以能量分散式X射線分析(EDS)來分析該不鏽鋼之結果，確認第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔係以金單質的金屬來封孔，金鍍敷被膜層的針孔係以鎳單質的金屬來封孔。
＜步驟(D)＞ 步驟(X)之後，以氮氣來取代前述常壓氣相流通式反應爐內部的大氣，接下來導入100體積%氧氣，以氧氣來完全取代氮氣，並維持該狀態12小時。接下來，將氧氣取代成氮氣後，導入10體積%氟氣(剩下90體積%為氮氣)，維持該狀態12小時來形成氟化鎳被膜層。進而，將氮氣流通12小時，使得成膜穩定化。對於所得到的最表面層為氟化鎳被膜的不鏽鋼，藉由X射線光電子分光法(XPS)所檢測出的F及Ni量比來確認氟化鎳的存在。由F及Ni的濺鍍時間及已知的濺鍍速率2.4nm/min(SiO2 換算)，來求出氟化鎳被膜的厚度時為103nm。
[實施例2] 與實施例1相同地實施步驟(A)後，於實施例1的步驟(B)中，除了將金的還原鍍敷處理變更成20分鐘以外，以與實施例1相同的方法來形成1.2μm厚的金鍍敷被膜層。之後，與實施例1相同地實施步驟(C)、步驟(X)及步驟(D)。與實施例1相同地求出氟化鎳被膜的厚度時為103nm。
[實施例3] 於實施例1中使用鋁合金(A5052)來替代不鏽鋼(SUS316L)，作為前處理施予脫脂、活性化處理、酸洗淨及鋅取代處理。之後，以與實施例1相同的方法來實施步驟(A)、步驟(B)、步驟(C)、步驟(X)及步驟(D)。與實施例1相同地求出氟化鎳被膜的厚度時為103nm。尚，前述活性化處理係使用酸性氟化銨與硝酸的混酸來作為處理劑，並以室溫下進行30秒鐘。前述酸洗淨係使用硝酸來作為洗淨劑，並以室溫下進行25秒鐘。前述鋅取代處理係使用鋅酸鹽浴(zincate bath)來作為處理劑，並以室溫下進行25秒鐘。又，依據上述條件分別各進行2次的前述酸洗淨及前述鋅取代處理。
[比較例1] 作為前處理，對於不鏽鋼(SUS316L)的表面施予脫脂、酸洗淨及鎳觸擊電鍍處理。使用無電解鎳-磷鍍敷藥劑「Nimuden(商標)NSX」(上村工業(股)製)，以鍍敷溫度90℃、pH4.5～4.8之條件下、成膜速度10μm/25分鐘，於已施予該鎳觸擊電鍍處理的不鏽鋼的表面上，形成成膜時的磷含量為8質量%以上未滿10質量%的第一含鎳鍍敷被膜層。接下來，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/50分鐘來形成成膜時的磷含量為10質量%以上12質量%以下的第二含鎳鍍敷被膜層。據此，於已施予鎳觸擊電鍍處理的不鏽鋼上，形成合計20μm厚的含鎳鍍敷被膜層。之後，依據與實施例1相同的方法來實施步驟(D)，於已施予鎳觸擊電鍍處理的不鏽鋼的表面形成含鎳鍍敷被膜層及氟化鎳被膜層。
[比較例2] 於比較例1中，使用鋁合金(A5052)替代不鏽鋼(SUS316L)來作為金屬基材，作為前處理施予脫脂、活性化處理、酸洗淨及鋅取代處理後，與比較例1相同地形成無電解鎳-磷合金鍍敷被膜層及氟化鎳被膜層。
[比較例3] 於實施例1中僅實施步驟(A)、步驟(B)及步驟(C)，換言之，未實施步驟(X)及步驟(D)，而於不鏽鋼上形成第一含鎳鍍敷被膜層、金鍍敷被膜層及第二含鎳鍍敷被膜層。
[評估] 對於上述實施例1～3及比較例1～3中所得到的金屬基材表面上的被膜來進行鹽酸耐蝕試驗。將評估結果表示於表1中。
＜鹽酸耐蝕試驗＞ 將長15mm×寬15mm×厚度1mm的試片，以25℃浸漬於35質量%鹽酸溶液中5小時。依據浸漬前後的質量減少量[mg/dm2 ]，利用下述基準來評估鹽酸耐蝕性。 (評估基準) A：未滿0.1mg/dm2 B：0.1mg/dm2 以上、未滿3.0mg/dm2 C：3.0mg/dm2 以上、未滿10.0mg/dm2 D：10.0mg/dm2 以上
Figure 02_image001
表1中，SUS表示不鏽鋼(SUS316L)，Al表示鋁合金(A5052)。
1:金屬基材 2:第一含鎳鍍敷被膜層 3:金鍍敷被膜層 4:第二含鎳鍍敷被膜層 5:氟化鎳被膜層 6:針孔 7:針孔被封孔處理的部位
[圖1]表示封孔處理前後的積層體的概略圖((a)：封孔處理前、(b)：封孔處理後)。
1:金屬基材
2:第一含鎳鍍敷被膜層
3:金鍍敷被膜層
4:第二含鎳鍍敷被膜層
5:氟化鎳被膜層
6:針孔
7:針孔被封孔處理的部位

Claims (14)

  1. 一種積層體，具有： 金屬基材、 形成於前述金屬基材上的第一含鎳鍍敷被膜層、 形成於前述第一含鎳鍍敷被膜層上的金鍍敷被膜層、 形成於前述金鍍敷被膜層上的第二含鎳鍍敷被膜層及 形成於前述第二含鎳鍍敷被膜層上的氟化鎳被膜層。
  2. 如請求項1之積層體，其中，前述金鍍敷被膜層的針孔係以鎳單質的金屬來封孔，且 前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔係以金單質的金屬來封孔。
  3. 如請求項1或2之積層體，其中，前述金屬基材包含選自由不鏽鋼、鐵、鋁、鋁合金、銅及銅合金所組成之群組之至少1種的金屬。
  4. 如請求項1～3中任一項之積層體，其中，於前述金屬基材與前述第一含鎳鍍敷被膜層之間，及於前述金鍍敷被膜層與前述第二含鎳鍍敷被膜層之間具有鎳觸擊電鍍層。
  5. 如請求項1～4中任一項之積層體，其中，前述第一含鎳鍍敷被膜層包含磷濃度為8質量%以上未滿10質量%的鎳-磷合金鍍敷層，且前述第二含鎳鍍敷被膜層包含磷濃度為10質量%以上12質量%以下的鎳-磷合金鍍敷層。
  6. 如請求項1～5中任一項之積層體，其中，前述金鍍敷被膜層從前述第一含鎳鍍敷被膜層側起依序包含取代型金鍍敷被膜層及還原型金鍍敷被膜層。
  7. 如請求項1～6中任一項之積層體，其中，前述氟化鎳被膜層的厚度為70nm以上。
  8. 一種積層體的製造方法，包含： 於金屬基材上形成第一含鎳鍍敷被膜層之步驟(A)、 於前述第一含鎳鍍敷被膜層上形成金鍍敷被膜層之步驟(B)、 於前述金鍍敷被膜層上形成第二含鎳鍍敷被膜層之步驟(C)及 於前述第二含鎳鍍敷被膜層上形成氟化鎳被膜層之步驟(D)。
  9. 如請求項8之積層體的製造方法，其中，於前述步驟(C)與前述步驟(D)之間包含步驟(X)，該步驟(X)係藉由以溫度250℃以上之條件下來將步驟(C)所得到的積層體進行加熱處理，而將前述金鍍敷被膜層的針孔以鎳單質的金屬來封孔，且將前述第一含鎳鍍敷被膜層及第二含鎳鍍敷被膜層的針孔以金單質的金屬來封孔。
  10. 如請求項8或9之積層體的製造方法，其中，前述步驟(D)係在氟氣濃度8體積%以上及溫度250℃以上的環境下來進行。
  11. 如請求項8～10中任一項之積層體的製造方法，其中，於前述步驟(A)之前及前述步驟(C)之前，包含以電流密度3～20A/dm2 之條件下來對於金屬基材施予鎳觸擊電鍍處理之步驟。
  12. 如請求項8～11中任一項之積層體的製造方法，其中，前述步驟(A)包含形成磷濃度為8質量%以上未滿10質量%的鎳-磷合金鍍敷層之步驟，且 前述步驟(C)包含形成磷濃度為10質量%以上12質量%以下的鎳-磷合金鍍敷層之步驟。
  13. 如請求項8～12中任一項之積層體的製造方法，其中，前述步驟(B)包含形成取代型金鍍敷被膜層之步驟(b1)，與於該步驟(b1)之後形成還原型金鍍敷被膜層之步驟(b2)。
  14. 一種半導體製造裝置的構成構件，其係由如請求項1～7中任一項之積層體所組成。
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