TWI620835B - 錫鍍敷銅合金端子材及其製造方法 - Google Patents
錫鍍敷銅合金端子材及其製造方法 Download PDFInfo
- Publication number
- TWI620835B TWI620835B TW104126544A TW104126544A TWI620835B TW I620835 B TWI620835 B TW I620835B TW 104126544 A TW104126544 A TW 104126544A TW 104126544 A TW104126544 A TW 104126544A TW I620835 B TWI620835 B TW I620835B
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- Prior art keywords
- layer
- alloy
- plating
- tin
- less
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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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
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
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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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- 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
- 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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- 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
- 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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- 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
- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
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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
- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
- C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
- C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
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- C—CHEMISTRY; METALLURGY
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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
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
- C25D5/611—Smooth layers
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance
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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
- C25D7/00—Electroplating characterised by the article coated
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/02—Contact members
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01R13/02—Contact members
- H01R13/03—Contact members characterised by the material, e.g. plating, or coating materials
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- H01R13/02—Contact members
- H01R13/04—Pins or blades for co-operation with sockets
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C25D3/02—Electroplating: Baths therefor from solutions
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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Abstract
一種錫鍍敷銅合金端子材,其係在由銅或銅合金構成的基材表面形成有Sn系表面層,且在Sn系表面層與基材之間,從Sn系表面層起依序形成有Cu-Sn合金層/Ni層或Ni合金層的錫鍍敷銅合金端子材,Cu-Sn合金層係僅由Cu6Sn5合金的Cu的一部分取代為Ni之金屬間化合物合金所構成的層,Cu-Sn合金層的一部分係朝Sn系表面層露出而形成複數個露出部,Sn系表面層的平均厚度為0.2μm以上且0.6μm以下,Cu-Sn合金層的露出部相對於表面積的面積率為1%以上且40%以下,Cu-Sn合金層之各露出部的等效圓直徑的平均值為0.1μm以上且1.5μm以下,表面的突出山部高度Rpk為0.005μm以上且0.03μm以下,動摩擦係數為0.3以下。
Description
本發明係有關於一種有用於作為汽車或家用設備等的電氣配線之連接所使用的連接器用端子,尤為多針腳連接器用之端子的錫鍍敷銅合金端子材及其製造方法。
本案係基於2014年9月11日所申請之日本特願2014-185033,主張其優先權,將其內容援用於此。
錫鍍敷銅合金端子材係藉由在由銅合金構成的基材上實施銅鍍敷及錫鍍敷後實施回焊處理,而於表層之Sn系表面層的下層形成Cu-Sn合金層者,經常作為端子材廣泛使用。
近年來,例如在汽車方面電氣化急速進行,隨之,電力機器的電路數亦增加,因此,使用之連接器的小型‧多針腳化更形重要。若將連接器多針腳化,縱使每單一針腳的插入力較小,但插裝連接器時連接器全體仍需要較大的力,而有生產性降低之虞。因此,便有人嘗試縮小錫鍍敷銅合金材的摩擦係數來降低每單一針腳的插入
力。
舉例來說,有將基材粗化,並將Cu-Sn合金層的表面露出度予以規制者(專利文獻1),惟其有接觸電阻增大、焊料浸潤性降低等問題。又,另有將Cu-Sn合金層的平均粗糙度予以規制者(專利文獻2),惟其有為了進一步提升插拔性而無法使例如動摩擦係數成為0.3以下等問題。
再者,有在基材上依序實施鎳鍍敷、銅鍍敷、錫鍍敷,並實施回焊處理,而作成基材/Ni/CuSn/Sn之層構造者(專利文獻3),惟,以防止加熱時的接觸電阻劣化為目的,無法使動摩擦係數成為0.3以下。
於此,就連接器的插入力F,若設母端子按壓公端子的力(接觸壓力)為P、動摩擦係數為μ,由於公端子通常自上下2方向被母端子包夾,故為F=2×μ×P。為縮小此插入力F,縮小接觸壓力P係屬有效,但為確保連接器嵌合時之公‧母端子的電連接可靠度,無法一味縮小接觸壓力P,而是需要3N左右。對於多針腳連接器,亦有超過50針腳/連接器者,較理想的是連接器全體的插入力F為100N以下,可以的話為80N以下,或為70N以下,因此,就動摩擦係數μ而言,需為0.3以下。
[專利文獻1]日本特開2007-100220號公報
[專利文獻2]日本特開2007-636324號公報
[專利文獻3]日本專利第4319247號公報
以往,有人開發出表面之摩擦阻力經降低的端子材。惟,若為嵌合公、母端子的連接端子時,兩者不常使用相同的材料物種,尤其是公端子係廣泛使用以黃銅為基材的廣用之附有錫鍍敷之端子材。因此,僅有母端子使用低插入力端子材,仍有降低插入力之效果較小等問題。
本發明係有鑑於前述之課題而完成者,係以提供一種對於使用廣用之錫鍍敷端子材的端子亦可降低嵌合時之插入力的錫鍍敷銅合金端子材為目的。
本案發明人等致力進行研究的結果,終至瞭解到:表層的Sn層較薄,使下層的Cu-Sn合金層僅有一小部分朝該表面露出對於動摩擦係數的降低係屬有利。然而,因Sn層變薄,導致電連接特性降低。因此,吾人發現,若將Cu-Sn合金層作成陡峭的凹凸形狀,並將表層附近作成Sn層與Cu-Sn合金層的複合構造,則可控制於限制Cu-Sn合金層之露出的範圍而抑制電連接特性的降低,
同時位於較硬之Cu-Sn合金層之間的較柔軟的Sn可發揮潤滑劑之作用而降低動摩擦係數,可得低插入力端子材。惟,若將此低插入力端子材僅用於端子的其中一者,而另一者採用廣用之錫鍍敷材時,降低摩擦係數之效果減半。其原因在於,使Cu-Sn合金層的一部分朝表面露出時,朝表面露出之Cu-Sn合金層與Sn層間產生段差,較硬的Cu-Sn合金層形成凸部,因此,若僅用於端子的其中一者,則會產生削下另一者之廣用之錫鍍敷材的較柔軟的Sn系表面層的所謂的磨料磨損之故。於此等見解之下,採用以下之解決手段。
本發明之錫鍍敷銅合金端子材係在由銅或銅合金構成的基材上的表面形成有Sn系表面層,且在該Sn系表面層與前述基材之間,從前述Sn系表面層起依序形成有Cu-Sh合金層/Ni層或Ni合金層的錫鍍敷銅合金端子材,前述Cu-Sn合金層係僅由Cu6Sn5合金的Cu的一部分取代為Ni之金屬間化合物合金所構成的層,前述Cu-Sn合金層的一部分係朝前述Sn系表面層的表面露出而形成複數個露出部,前述Sn系表面層的平均厚度為0.2μm以上且0.6μm以下,前述Cu-Sn合金層的前述露出部相對於前述錫鍍敷銅合金端子材之表層的表面積的面積率為1%以上且40%以下,前述Cu-Sn合金層之前述各露出部的等效圓直徑的平均值為0.1μm以上且1.5μm以下,前述錫鍍敷銅合金端子材之表面的突出山部高度Rpk為0.005μm以上且0.03μm以下,動摩擦係數為0.3以下。
藉由使錫鍍敷銅合金端子材之表面的突出山部高度Rpk成為0.005μm以上且0.03μm以下,使Sn系表面層的平均厚度成為0.2μm以上且0.6μm以下,使Cu-Sn合金層的露出部相對於錫鍍敷銅合金端子材之表層的表面積的面積率成為1~40%,使Cu-Sn合金層之各露出部的等效圓直徑的平均值成為0.1μm以上且1.5μm以下,可實現錫鍍敷銅合金端子材的動摩擦係數為0.3以下。此時,透過Cu的一部分取代為Ni之(Cu,Ni)6Sn5合金的存在,Cu-Sn合金層的表面便形成微細的凹凸形狀,而抑制於限制錫鍍敷銅合金端子材的突出山部高度Rpk及Cu-Sn合金層之露出部的面積率的範圍。
使錫鍍敷銅合金端子材之表面的突出山部高度Rpk成為0.03μm以下的原因在於,若超過0.03μm則會產生較硬之Cu-Sn合金層削下滑動對象材料之較柔軟的Sn層的所謂的磨料磨損,使摩擦阻力變大之故。使錫鍍敷銅合金端子材的突出山部高度Rpk成為0.005μm以上的原因在於,當Cu-Sn合金層朝Sn系表面層的表面露出時,在Sn系表面層與Cu-Sn合金層的露出部之間會產生段差之故。
使Sn系表面層的平均厚度成為0.2μm以上且0.6μm以下的原因在於,若未達0.2μm時會導致焊料浸潤性的降低、電連接可靠度的降低;超過0.6μm時則無法使表層形成Sn層與Cu-Sn合金層的複合構造,僅由Sn占據而導致動摩擦係數增大之故。更佳之Sn系表面層的平均
厚度為0.3μm~0.5μm。
Cu-Sn合金層的露出部相對於錫鍍敷銅合金端子材的表面積的面積率若未達1%時無法使動摩擦係數成為0.3以下;若超過40%,則焊料浸潤性等的電連接特性會降低。更佳之面積率為2%~20%。
Cu-Sn合金層之各露出部的等效圓直徑的平均值若未達0.1μm時,無法使Cu-Sn合金層的露出部的面積率成為1%以上;超過1.5μm時,則位於較硬之Cu-Sn合金層之間的較柔軟的Sn無法充分發揮作為潤滑劑之作用,而無法使動摩擦係數成為0.3以下。更佳之等效圓直徑為0.2μm~1.0μm。
此外,就Sn系表面層,已知若縮小動摩擦係數測定時的垂直荷重則動摩擦係數會增大,但本發明品,即使降低垂直荷重,動摩擦係數亦幾無變化,使用於小型端子亦可發揮其效果。
在本發明之錫鍍敷銅合金端子材中,前述Cu-Sn合金層中的Ni含有率宜為1at%以上且25at%以下。將Ni含有率規定為1at%以上的原因在於,若未達1at%時,無法形成Cu6Sn5合金的Cu的一部分取代為Ni之金屬間化合物合金,而無法構成陡峭的凹凸形狀之故;規定為25at%以下的原因在於,若超過25at%,則有Cu-Sn合金層的形狀變得過於微細的傾向,若Cu-Sn合金層變得過於微細,則有無法使動摩擦係數成為0.3以下的情形。
本發明之錫鍍敷銅合金端子材的製造方法係
製造藉由在由銅合金構成的基材上,依序實施鎳鍍敷或鎳合金鍍敷、銅鍍敷及錫鍍敷後,實施回焊處理,而於前述基材上形成Ni層或Ni合金層/Cu-Sn合金層/Sn系表面層的錫鍍敷銅合金端子材之方法,其中將藉前述鎳鍍敷或鎳合金鍍敷形成的第1鍍敷層厚度作成0.05μm以上且1.0μm,將藉前述銅鍍敷形成的第2鍍敷層厚度作成0.05μm以上且0.20μm以下,將藉前述錫鍍敷形成的第3鍍敷層厚度作成0.5μm以上且1.0μm以下,前述回焊處理係具有將各鍍敷層以20~75℃/秒的升溫速度加熱至240~300℃之峰值溫度的加熱步驟;達到前述峰值溫度後,以30℃/秒以下的冷卻速度冷卻2~15秒的一次冷卻步驟;及在一次冷卻後以100~300℃/秒的冷卻速度冷卻的二次冷卻步驟。
諸如前述,藉由對基材實施鎳鍍敷或鎳合金鍍敷,於回焊處理後形成(Cu,Ni)6Sn5合金,藉此,Cu-Sn合金層的凹凸變得更陡峭而能夠使動摩擦係數成為0.3以下。
藉鎳鍍敷或鎳合金鍍敷形成的第1鍍敷層厚度若未達0.05μm時,(Cu,Ni)6Sn5合金所含有的Ni含有率變小,無法形成陡峭的凹凸形狀之Cu-Sn合金層;超過1.0μm時則不易實施彎曲加工等。此外,欲使Ni層或Ni合金層具有作為防止Cu從基材的擴散之障壁層的機能而提升耐熱性時,藉鎳鍍敷或鎳合金鍍敷形成的第1鍍敷層厚度較佳作成0.1μm以上。鎳鍍敷或鎳合金鍍敷所使用的
金屬不限定於純Ni,亦可為Ni-Co或Ni-W等的Ni合金。
藉銅鍍敷形成的第2鍍敷層厚度若未達0.05μm時,(Cu,Ni)6Sn5合金所含有的Ni含有率變大,Cu-Sn合金層的形狀變得過於微細;超過0.20μm時,則(Cu,Ni)6Sn5合金所含有的Ni含有率變小,無法形成陡峭的凹凸形狀之Cu-Sn合金層。
藉錫鍍敷形成的第3鍍敷層厚度若未達0.5μm時,回焊後的Sn系表面層會變薄而損及電連接特性;超過1.0μm時,則Cu-Sn合金層朝前述Sn系表面層的表面之露出部的面積率會變小而不易使動摩擦係數成為0.3以下。
在回焊處理中,加熱步驟中的升溫速度若未達20℃/秒時,在鍍錫熔融前的期間,Cu原子在Sn的粒界中優先性地擴散而於粒界附近,金屬間化合物異常生長,而無法形成陡峭的凹凸形狀之Cu-Sn合金層。另一方面,升溫速度超過75℃/秒時,金屬間化合物未能充分生長,在其後的冷卻無法獲得所期望的金屬間化合物合金。
又,加熱步驟中的峰值溫度若未達240℃時,Sn無法均勻地熔融;峰值溫度超過300℃時,則金屬間化合物劇烈地生長,Cu-Sn合金層的凹凸變大,因而不佳。
再者,在冷卻步驟中,藉由設置冷卻速度較小的一次冷卻步驟,使Cu原子在Sn粒內平穩地擴散,而以所期望的金屬間化合物構造生長。此一次冷卻步驟的冷
卻速度若超過30℃/秒,金屬間化合物因受劇烈冷卻的影響而無法充分地生長,使Cu-Sn合金層無法朝表面露出。冷卻時間未達2秒亦同樣地無法使金屬間化合物生長。冷卻時間超過15秒時,Cu6Sn5合金的生長會過度地進行而粗大化,根據銅鍍敷層的厚度,在Cu-Sn合金層下形成Ni-Sn化合物層,使Ni層的障壁性降低。此一次冷卻步驟係適用空氣冷卻。
於此一次冷卻步驟後,藉由二次冷卻步驟急速冷卻而以所期望的構造完成金屬間化合物合金的生長。此二次冷卻步驟的冷卻速度未達100℃/秒時,金屬間化合物進一步進行,而無法獲得所期望的金屬間化合物形狀。
根據本發明,由於其動摩擦係數小,而能夠提供一種可兼具低接觸電阻、良好的焊料浸潤性及低插拔性,而且在低荷重下亦有其效果而最適合小型端子的錫鍍敷銅合金端子材。尤其是在使用於汽車及電子零件等的端子中,在要求接合時的低插入力、穩定的接觸電阻、良好的焊料浸潤性的部位有其優勢。
1‧‧‧基臺
12‧‧‧公端子試片
13‧‧‧母端子試片
14‧‧‧載重
15‧‧‧測力計
第1圖為表示實施例3、比較例4、比較例10之X射線繞射圖形的圖。
第2圖為實施例3之錫鍍敷銅合金端子材之剖面的STEM像。
第3圖為沿著第2圖之白線部分的EDS分析圖。
第4圖為比較例4之錫鍍敷銅合金端子材之剖面的STEM像。
第5圖為沿著第4圖之白線部分的EDS分析圖。
第6圖為比較例10之錫鍍敷銅合金端子材之剖面的STEM像。
第7圖為沿著第6圖之白線部分的EDS分析圖。
第8圖為概念性地表示供測定動摩擦係數之裝置的正面圖。
茲說明本發明一實施形態之錫鍍敷銅合金端子材。
本實施形態之錫鍍敷銅合金端子材係在由銅或銅合金構成的基材上的表面形成有Sn系表面層,且在Sn系表面層與前述基材之間,從Sn系表面層起依序形成有Cu-Sn合金層/Ni層或Ni合金層。
基材只要是由銅或銅合金構成者,則其組成不特別限定。
Ni層或Ni合金層係由純Ni、Ni-Co或Ni-W等的Ni合金所構成的層。
Cu-Sn合金層係僅由Cu6Sn5合金的Cu的一部
分取代為Ni之金屬間化合物合金所構成的層,其一部分係朝Sn系表面層的表面露出而形成複數個露出部。
此等層係如後述,藉由在基材上依序實施鎳鍍敷、銅鍍敷、錫鍍敷並實施回焊處理而形成者,在Ni層或Ni合金層上形成有Cu-Sn合金層。
於此錫鍍敷銅合金端子材中,重要的是朝表面露出之Cu-Sn合金層呈微細且與Sn系表面層的段差較小而呈平滑,藉Cu-Sn合金層的露出部及Sn系表面層形成的錫鍍敷銅合金端子材之表面的突出山部高度Rpk係作成0.005μm以上且0.03μm以下。突出山部高度Rpk為以JISB0671-2定義之位於粗糙度曲線之芯部上的突出山部的平均高度,係透過以雷射顯微鏡進行測定來求得。
Sn系表面層的平均厚度為0.2μm以上且0.6μm以下,Cu-Sn合金層的一部分(露出部)係朝此Sn系表面層的表面露出。而且,形成為露出部相對於錫鍍敷銅合金端子材的表面積的面積率為1%以上且40%以下,Cu-Sn合金層之各露出部的等效圓直徑的平均值為0.1μm以上且1.5μm以下。
此種構造之錫鍍敷銅合金端子材,透過存在有僅由Cu的一部分取代為Ni之(Cu,Ni)6Sn5合金所構成的Cu-Sn合金層,而形成表層較硬之Cu-Sn合金層與較柔軟之Sn系表面層的複合構造,該較硬之Cu-Sn合金層的一部分(露出部)係朝Sn系表面層些微露出而形成複數個露出部,存在於各露出部之周圍的較柔軟的Sn係發揮
潤滑劑之作用,而實現0.3以下之較低的動摩擦係數。由於該Cu-Sn合金層之各露出部的面積率係限制在相對於錫鍍敷銅合金端子材的表面積為1%以上且40%以下的範圍,故不會損及Sn系表面層所具有之優良的電連接特性。
此時,Cu-Sn合金層中的Ni含有率係設為1at%以上且25at%以下。將Ni含有率規定為1at%以上的原因在於,若未達1at%時,無法形成Cu6Sn5合金的Cu的一部分取代為Ni之金屬間化合物合金,而無法構成陡峭的凹凸形狀之故;規定為25at%以下的原因在於,若超過25at%,則有Cu-Sn合金層的形狀變得過於微細的傾向,若Cu-Sn合金層變得過於微細,則有無法使動摩擦係數成為0.3以下的情形。
使Sn系表面層的平均厚度成為0.2μm以上且0.6μm以下的原因在於,若未達0.2μm時會導致焊料浸潤性的降低、電連接可靠度的降低;超過0.6μm時則無法使表層形成Sn層與Cu-Sn合金層的複合構造,僅由錫占據而導致動摩擦係數增大之故。更佳之Sn系表面層的平均厚度為0.3μm~0.5μm。
端子材的表面之Cu-Sn合金層的露出部的面積率若未達1%時無法使動摩擦係數成為0.3以下;若超過40%,則焊料浸潤性等的電連接特性會降低。更佳之面積率為2%~20%。
Cu-Sn合金層之各露出部的等效圓直徑的平均
值若未達0.1μm時,無法使露出部的面積率成為1%以上;超過1.5μm時,則位於較硬之Cu-Sn合金層之間的較柔軟的錫(Sn)無法充分發揮作為潤滑劑之作用,而無法使動摩擦係數成為0.3以下。更佳之等效圓直徑為0.2μm~1.0μm。
此外,就Sn系表面層,已知若縮小動摩擦係數測定時的垂直荷重則動摩擦係數會增大,但本發明品,即使降低垂直荷重,動摩擦係數亦幾無變化,使用於小型端子亦可發揮其效果。
其次,就此端子材的製造方法加以說明。
作為基材,係準備由銅或Cu-Ni-Si系等的銅合金構成的板材。藉由對此板材實施脫脂、酸洗等的處理而使表面成清潔後,依序實施鎳鍍敷、銅鍍敷、錫鍍敷。
鎳鍍敷只要使用一般的鎳鍍敷浴即可,可使用例如以硫酸(H2SO4)與硫酸鎳(NiSO4)為主成分的硫酸浴。鍍敷浴的溫度係採20℃以上且50℃以下、電流密度係採1~30A/dm2以下。藉此鎳鍍敷形成之鎳鍍敷層的膜厚(第1鍍敷層厚度)係作成0.05μm以上且1.0μm以下。此係因第1鍍敷層厚度若未達0.05μm時,(Cu,Ni)6Sn5合金所含有的Ni含有率變小,無法形成陡峭的凹凸形狀之Cu-Sn合金層;第1鍍敷層厚度超過1.0μm時則不易實施彎曲加工等之故。
銅鍍敷只要使用一般的銅鍍敷浴即可,可使用例如以硫酸銅(CuSO4)及硫酸(H2SO4)為主成分的
硫酸銅浴。鍍敷浴的溫度係採20~50℃、電流密度係採1~30A/dm2以下。藉此銅鍍敷形成之銅鍍敷層的膜厚(第2鍍敷層厚度)係作成0.05μm以上且0.20μm以下。此係因第2鍍敷層厚度若未達0.05μm時,(Cu,Ni)6Sn5合金所含有的Ni含有率變大,Cu-Sn合金層的形狀變得過於微細;第2鍍敷層厚度超過0.20μm時,則(Cu,Ni)6Sn5合金所含有的Ni含有率變小,無法形成陡峭的凹凸形狀之Cu-Sn合金層之故。
作為用於形成錫鍍敷層的鍍敷浴,只要使用一般的錫鍍敷浴即可,可使用例如以硫酸(H2SO4)與硫酸錫(SnSO4)為主成分的硫酸浴。鍍敷浴的溫度係採15~35℃、電流密度係採1~30A/dm2。藉此錫鍍敷形成之錫鍍敷層的膜厚(第3鍍敷層厚度)係作成0.5μm以上且1.0μm以下。第3鍍敷層厚度若未達0.5μm時,回焊後的Sn系表面層會變薄而損及電連接特性;第3鍍敷層厚度超過1.0μm時,則Cu-Sn合金層朝端子材的表面之露出部的面積率會變小而不易使動摩擦係數成為0.3以下。
實施各鍍敷處理後,進行加熱來進行回焊處理。
回焊處理係採用具有:在形成CO還原性氣體環境的加熱爐內,將鍍敷後之處理材(基材)以20~75℃/秒的升溫速度加熱3~15秒至240~300℃之峰值溫度的加熱步驟;達到該峰值溫度後,以30℃/秒以下的冷卻速度冷卻2~15秒的一次冷卻步驟;及在一次冷卻後以
100~300℃/秒的冷卻速度冷卻0.5~5秒的二次冷卻步驟之處理。一次冷卻步驟係藉由空氣冷卻,二次冷卻步驟則藉由使用10~90℃的水的水冷卻來進行。
藉由在還原性氣體環境下進行此回焊處理,可防止在錫鍍敷表面生成熔融溫度較高的錫氧化物皮膜,而能以更低的溫度且更短的時間實施回焊處理,更容易製作所期望的金屬間化合物構造。又,藉由將冷卻步驟設為二階段,並設置冷卻速度較小的一次冷卻步驟,可使Cu原子在Sn粒內平穩地擴散,而以所期望的金屬間化合物構造生長。而且,藉由在隨後進行急速冷卻來停止金屬間化合物合金的生長,可固定在所期望的構造。
以高電流密度電析而得的Cu與Sn其穩定性較低,在室溫下亦會發生合金化或結晶粒的增大化,而不易以回焊處理作成所期望的金屬間化合物構造。因此,較理想的是在鍍敷處理後迅速進行回焊處理。具體而言,需在15分鐘以內,較理想為5分鐘以內進行回焊。鍍敷後的放置時間過短雖然不會造成問題,但在一般的處理線上,以構成而言係取約1分鐘後。
以板厚0.25mm之科森系(Cu-Ni-Si系)銅合金板為基材,依序實施鎳鍍敷、銅鍍敷、錫鍍敷,再實施回焊處
理而製成各母端子試片用之試料。鎳鍍敷、銅鍍敷及錫鍍敷的鍍敷條件在實施例、比較例中均相同,係如表1所示。表1中,Dk為陰極的電流密度,ASD為A/dm2的簡稱。
實施過鍍敷處理後的回焊處理係於實施最後的錫鍍敷處理後的1分鐘後進行,以各種的條件進行加熱步驟、一次冷卻步驟、二次冷卻步驟。將各試驗條件及所得之各試料的鍍敷層的厚度彙整於表2。
針對回焊後之此等試料,測定Sn系表面層的平均厚度、(Cu,Ni)6Sn5合金中的Ni含有率、Cu6Sn5合金以外之合金層的存在、突出山部高度Rpk、Cu-Sn合金層之露出部在Sn系表面上的面積率、露出部的等效圓直徑的平均值,並評定動摩擦係數、焊料浸潤性、光澤度、電性可靠度(接觸電阻)。
Sn系表面層的厚度係以SII NanoTechnology股份有限公司製螢光X射線膜厚計(SFT9400)測定。最初測定回焊後之試料的總Sn系表面層的厚度後,對例如Leybold股份有限公司製之L80等的純Sn進行蝕刻並予以浸漬於由不會腐蝕Cu-Sn合金層之成分所構成的鍍敷被膜剝離用之蝕刻液數分鐘,藉此去除Sn系表面層,使其
下層的Cu-Sn合金層露出並測定換算成純Sn之Cu-Sn合金層的厚度後,將(總Sn系表面層的厚度-換算成純Sn之Cu-Sn合金層的厚度)定義為Sn系表面層的厚度。
在Cu-Sn合金層中,針對(Cu,Ni)6Sn5合金中的Ni含有率,以藉由剖面STEM像之觀察及EDS分析的面分析鑑定出合金的位置,並以點分析求出(Cu,Ni)6Sn5合金中之Ni的含有率。就Cu6Sn5合金以外之合金層的有無,係以藉由剖面STEM像之觀察及EDS分析的面分析鑑定出合金的位置,並藉由深度方向的線分析求出Cu6Sn5合金以外之合金層的有無。又,除剖面觀察外,就更廣範圍之Cu6Sn5合金以外之合金層的有無,係藉由浸漬於錫鍍敷被膜剝離用之蝕刻液而去除Sn系表面層,使其下層的Cu-Sn合金層露出後,測定使用CuKα線的X射線繞射圖形來判定。測定條件如下:
PANalytical製:MPD1880HR
使用管球:Cu Kα線
電壓:45kV
電流:40mA
表面的突出山部高度Rpk係利用KEYENCE股份有限公司製雷射顯微鏡(VK-X200),以物鏡150倍(測定視野96μm×72μm)之條件,由在長邊方向取5點、在短邊方向取5點共計10點所測得之Rpk的平均值來求取。
Cu-Sn合金層的露出部的面積率及等效圓直徑
係將表面氧化膜去除後,藉由掃描離子顯微鏡觀察100×100μm之區域來求取。在測定原理上,由於係將存在於最表面起至約20nm之深度區域的Cu6Sn5合金假想為白色,因此,使用影像處理軟體,計算各個白色區域的面積,算出白色區域的面積相對於測定區域之總面積的比率作為Cu-Sn合金層的露出部的面積率。
又,將具有與各露出部(白色區域)的面積同等面積的圓的直徑作為各露出部的等效圓直徑,算出其平均值。等效圓直徑係指在粒徑分布的測定中,針對粒子形狀不規則的粒子,將換算成具有與觀察到的該粒子的面積同等面積的圓的直徑所得之值視為粒子的直徑者。
以板厚0.25mm之銅合金板(C2600、Cu:70質量%-Zn:30質量%)作為基材,依序實施銅鍍敷、錫鍍敷,再實施回焊處理而製成公端子試片用之試料。回焊後之Sn系表面層的厚度為0.6μm,無Cu-Sn合金層的露出。
使用該公端子試片、與以表2之各條件所製作的各母端子試片來測定動摩擦係數。將各試料作成板狀的公端子試片與呈內徑1.5mm之半球狀的母端子試片,模擬嵌合型之連接器的公端子與母端子的接點部,利用Trinity-Lab股份有限公司製之摩擦測定機(μV1000),測定兩試片間的摩擦力並求出動摩擦係數。
根據第8圖加以說明,在水平的基臺11上固
定公端子試片12,於其上載置母端子試片13的半球凸面使鍍敷面彼此接觸,對母端子試片13藉由載重14施加500gf的荷重P而按壓公端子試片12。在施加此荷重P的狀態下,藉由測力計15測定將公試片12以滑動速度80mm/分朝箭號所示之水平方向拉伸10mm時的摩擦力F。由該摩擦力F的平均值Fav與荷重P求出動摩擦係數(=Fav/P)。
就焊料浸潤性,係將各試料切成寬10mm,使用松脂系活性助焊劑以彎月圖法測定零點交叉時間。(使其浸漬於焊料浴溫230℃的Sn-37%Pb焊料,以浸漬速度2mm/sec、浸漬深度2mm、浸漬時間10sec之條件測定)將焊料零點交叉時間為3秒以下者評為良,將超過3秒的情形評為不良。
光澤度係利用日本電色工業股份有限公司製光澤度計(型號:PG-1M),依據JIS Z 8741,以入射角60度進行測定。
為評定電性可靠度,而於大氣中,在160℃下加熱500小時,並測定接觸電阻。測定方法係依據JIS-C-5402,藉由4端子接觸電阻試驗機(山崎精機研究所製:CRS-113-AU),以滑動式(1mm)測定0到50g的荷重變化-接觸電阻,以取荷重為50g時的接觸電阻值來評定。
將此等測定結果、評定結果示於表3。
由此表3可明瞭,在實施例中動摩擦係數均小至0.3以下,焊料浸潤性良好、光澤度亦高且外觀良好,接觸電阻也顯示為10mΩ以下。尤其是藉由鎳鍍敷形成厚度0.1μm以上之鎳鍍敷層的實施例1至4及7,8,均顯示出低至4mΩ以下的接觸電阻。
相對於此,就比較例1,3,5,7,9,12,因Cu-Sn合金層的露出部的面積率未達1%,故動摩擦係數為0.3以上。就比較例2、6,因露出部的面積率超過40%,焊料浸潤性、光澤度差。就比較例4,由於Cu6Sn5合金中不含Ni,且可確認Cu3Sn合金的存在,故露出部的等效圓直徑的平均值超過1.5μm,因此,動摩擦係數超過0.3。
比較例8、11係偏離回焊條件,Rpk超過0.03μm而產生磨料磨損,因此動摩擦係數超過0.3。比較
例10因偏離回焊條件,而形成Ni3Sn4合金的結果,Ni層的障壁性降低致接觸電阻超過9mΩ。
第1圖為實施例3與比較例4,10之25度至46度的X射線繞射圖形。比較此等圖形可知,實施例3僅檢測出基材之Cu、底鍍敷層之Ni及Cu6Sn5合金的峰,惟比較例10在31.7度附近檢測出Ni3Sn4合金的峰,比較例4在37.8度附近檢測出Cu3Sn合金的峰。又,就實施例3與比較例10,由於Cu6Sn5合金的峰朝高角度側位移,可知Cu6Sn5合金中的Cu的一部分取代為Ni。
第2圖及第3圖為實施例3之試料的剖面STEM像與EDS分析結果,(a)為Ni層、(b)為由(Cu,Ni)6Sn5合金構成的Cu-Sn合金層、(c)為錫層。
第4圖、第5圖為比較例4的剖面STEM像與EDS分析結果,(a)為Ni層、(b)為Cu3Sn合金層、(c)為(Cu,Ni)6Sn5合金層、(d)為錫層。
第6圖、第7圖為比較例10的剖面STEM像與EDS線分析結果,(a)為Ni層、(b)為(Ni,Cu)3Sn4合金層、(c)為(Cu,Ni)6Sn5合金層、(d)為錫層。
比較此等照片及圖可知,若為實施例者,在Ni層與錫層之間僅形成僅由含有Ni之Cu6Sn5合金((Cu,Ni)6Sn5合金)所構成的Cu-Sn合金層。另一方面,就比較例4,可知在Cu6Sn5合金層與Ni層的界面形成Cu3Sn合金層,且Cu6Sn5合金中不含Ni,Cu-Sn合金層的凹凸亦較粗糙地呈平緩。又,就比較例10,可知在含有
Ni之Cu6Sn5合金層與Ni層的界面形成有含Cu的Ni3Sn4合金層。
由於動摩擦係數小,而能夠提供一種可兼具低接觸電阻、良好的焊料浸潤性及低插拔性,而且在低荷重下亦有其效果而最適合小型端子的錫鍍敷銅合金端子材。尤其是在使用於汽車及電子零件等的端子中,在要求接合時的低插入力、穩定的接觸電阻、良好的焊料浸潤性的部位有其優勢。
Claims (2)
- 一種錫鍍敷銅合金端子材,其係在由銅或銅合金構成的基材上的表面形成有Sn系表面層,且在該Sn系表面層與前述基材之間,從前述Sn系表面層起依序形成有Cu-Sn合金層/Ni層或Ni合金層的錫鍍敷銅合金端子材,其特徵為:前述Cu-Sn合金層係僅由Cu6Sn5合金的Cu的一部分取代為Ni之金屬間化合物合金所構成的層,前述Cu-Sn合金層的一部分係朝前述Sn系表面層的表面露出而形成複數個露出部,前述Sn系表面層的平均厚度為0.2μm以上且0.6μm以下,前述Cu-Sn合金層的前述露出部相對於前述錫鍍敷銅合金端子材之表層的表面積的面積率為1%以上且40%以下,前述Cu-Sn合金層之前述各露出部的等效圓直徑的平均值為0.1μm以上且1.5μm以下,前述錫鍍敷銅合金端子材之表面的突出山部高度Rpk為0.005μm以上且0.03μm以下,動摩擦係數為0.3以下,前述Cu-Sn合金層中的Ni含有率為1at%以上且25at%以下。
- 一種錫鍍敷銅合金端子材的製造方法,其係製造藉由在由銅合金構成的基材上,依序實施鎳鍍敷或鎳合金 鍍敷、銅鍍敷及錫鍍敷後,實施回焊處理,而於前述基材上形成Ni層或Ni合金層/Cu-Sn合金層/Sn系表面層的錫鍍敷銅合金端子材之方法,其特徵為:將藉前述鎳鍍敷或鎳合金鍍敷形成的第1鍍敷層厚度作成0.05μm以上且1.0μm,將藉前述銅鍍敷形成的第2鍍敷層厚度作成0.05μm以上且0.20μm以下,將藉前述錫鍍敷形成的第3鍍敷層厚度作成0.5μm以上且1.0μm以下,前述回焊處理係具有將各鍍敷層以20~75℃/秒的升溫速度加熱至240~300℃之峰值溫度的加熱步驟;達到前述峰值溫度後,以30℃/秒以下的冷卻速度冷卻2~15秒的一次冷卻步驟;及在一次冷卻後以100~300℃/秒的冷卻速度冷卻的二次冷卻步驟。
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CN108914123A (zh) * | 2018-07-27 | 2018-11-30 | 苏州瑞沁精密机械有限公司 | 一种金属零件表面防腐蚀处理方法 |
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