TWI431170B - A glossy nickel plating material, an electronic component using a glossy nickel plating material, and a method of manufacturing a glossy nickel plating material - Google Patents
A glossy nickel plating material, an electronic component using a glossy nickel plating material, and a method of manufacturing a glossy nickel plating material Download PDFInfo
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
- C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
- C25D3/16—Acetylenic compounds
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
- C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
- C25D3/18—Heterocyclic compounds
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
Description
本發明係有關於光澤鎳電鍍材料、使用光澤鎳電鍍材料的電子零件及光澤鎳電鍍材料的製造方法。The present invention relates to a glossy nickel plating material, an electronic component using a glossy nickel plating material, and a method of producing a glossy nickel plating material.
在端子、連接器等之電子零件或金屬裝飾品等的金屬基材上使用具有光澤鎳電鍍的材料。於製造光澤鎳電鍍之際所產生的問題,可舉出電鍍外觀會受到電鍍材料之表面特性的影響。譬如,在黃銅(Cu-30%Zn)條狀上進行光澤鎳電鍍時,若黃銅材料為燒鈍材料的話,則於電鍍後外觀上看不出良好的光澤,甚至有時候會出現類似模糊或光澤與模糊混合之外觀。另外,在磷青銅(Cu-8%Sn-P)條狀上進行光澤鎳電鍍時,也可確認會產生相同問題點。A material having glossy nickel plating is used on a metal substrate such as an electronic component such as a terminal or a connector or a metal ornament. The problem that arises when manufacturing glossy nickel plating is that the appearance of the plating is affected by the surface characteristics of the plating material. For example, when performing gloss nickel plating on a strip of brass (Cu-30%Zn), if the brass material is a blunt material, there is no good gloss on the appearance after plating, and sometimes it may appear similar. Blur or the appearance of a mixture of luster and blur. Further, when gloss nickel plating was performed on a strip of phosphor bronze (Cu-8% Sn-P), it was confirmed that the same problem occurred.
為了要解決如此之問題點,譬如於專利文獻1揭示有電鍍性佳之銅合金的製造方法。且其中記載著若藉由此技術特徵的話,將可縮小銅合金表面之加工變質層的厚度,特別是可形成良好的電鍍銀或電鍍銅。In order to solve such a problem, for example, Patent Document 1 discloses a method of producing a copper alloy having excellent electroplating properties. It is described that if the technical features are utilized, the thickness of the work-affected layer on the surface of the copper alloy can be reduced, and in particular, good electroplated silver or electroplated copper can be formed.
[先前技術文獻][Previous Technical Literature]
[專利文獻1]特開2007-39804號公報[Patent Document 1] JP-A-2007-39804
然而,上述之銅合金,雖然可良好適用於電鍍銀或電鍍銅,但於光澤鎳電鍍上卻很難獲得良好之光澤,仍有很多改善餘地。故,本發明之課題將提供一種具有良好外觀之光澤鎳電鍍材料,使用光澤鎳電鍍材料的電子零件及光澤鎳電鍍材料的製造方法。However, although the copper alloy described above is well suited for electroplating silver or electroplated copper, it is difficult to obtain a good gloss on glossy nickel plating, and there is still much room for improvement. Therefore, an object of the present invention is to provide a glossy nickel plating material having a good appearance, an electronic component using a glossy nickel plating material, and a method of producing a glossy nickel plating material.
本發明者們,認真檢討之結果,於進行有電鍍處理之金屬基材表面上利用形成有加工變質層,即可獲得外觀良好之光澤鎳電鍍。找出與專利文獻1相反的事實。As a result of careful review, the present inventors have obtained a gloss nickel plating having a good appearance by forming a work-affected layer on the surface of a metal substrate having a plating treatment. The fact opposite to Patent Document 1 is found.
以上述的知識為基礎所完成之本發明,於本實施形態中為光澤鎳電鍍材料,係包括:金屬基材,表面加工變質層厚度為大於等於0.2μm;及鎳電鍍層,形成於該金屬基材之表面上。The present invention, which is based on the above knowledge, is a glossy nickel plating material in the present embodiment, comprising: a metal substrate having a surface-treated metamorphic layer having a thickness of 0.2 μm or more; and a nickel plating layer formed on the metal On the surface of the substrate.
本發明之光澤鎳電鍍材料,進一步於另一實施形態中,加工變質層厚度為0.25至3.0μm。Further, in another embodiment, the gloss nickel plating material of the present invention has a thickness of the processed deterioration layer of 0.25 to 3.0 μm.
本發明之光澤鎳電鍍材料,進一步於另一實施形態中,加工變質層厚度為0.3至2.0μm。Further, in another embodiment, the gloss nickel plating material of the present invention has a thickness of the processed deterioration layer of 0.3 to 2.0 μm.
本發明之光澤鎳電鍍材料,進一步於另一實施形態中,構成鎳電鍍層之鎳結晶粒子直徑為小於0.3μm。In the gloss nickel plating material of the present invention, in another embodiment, the nickel crystal particles constituting the nickel plating layer have a diameter of less than 0.3 μm.
本發明之光澤鎳電鍍材料,進一步於另一實施形態中,構成該鎳電鍍層之鎳結晶粒子直徑為0.01至0.3μm。Further, in another embodiment, the nickel electroplated material of the present invention has a nickel crystal particle diameter of 0.01 to 0.3 μm.
本發明之光澤鎳電鍍材料,進一步於另一實施形態中,金屬基材係以不鏽鋼、銅或銅合金所形成。In another embodiment of the glossy nickel plating material of the present invention, the metal substrate is formed of stainless steel, copper or a copper alloy.
本發明於另一實施形態,係使用光澤鎳電鍍材料的電子零件。In another embodiment of the invention, an electronic component of a glossy nickel plating material is used.
本發明進一步於另一實施形態中,係光澤鎳電鍍材料的製造方法,準備表面加工變質層厚度為大於等於0.2μm之金屬基材,且於該表面上形成有鎳電鍍層。According to still another embodiment of the present invention, in a method for producing a gloss nickel plating material, a metal substrate having a surface-treated altered layer thickness of 0.2 μm or more is prepared, and a nickel plating layer is formed on the surface.
於本發明之光澤鎳電鍍材料的製造方法之其中一實施形態中,構成鎳電鍍層之鎳結晶粒子直徑為小於0.01至0.3μm。In one embodiment of the method for producing a glossy nickel plating material of the present invention, the nickel crystal particles constituting the nickel plating layer have a diameter of less than 0.01 to 0.3 μm.
若藉由本發明,將可提供一種具有良好外觀之光澤鎳電鍍材料,使用光澤鎳電鍍材料的電子零件及光澤鎳電鍍材料的製造方法。According to the present invention, it is possible to provide a glossy nickel plating material having a good appearance, an electronic component using a glossy nickel plating material, and a method of producing a glossy nickel plating material.
雖無限制用於本發明之金屬基材的型態,但可舉出譬如不鏽鋼、銅或銅合金。其中可使用麻田散鐵(martensite)、亞鐵鹽(ferrite),沃斯田鐵(austenite)等材料來作為不鏽鋼。另外,雖以用於連接器或端子等電子零件的基材作為銅或銅合金,習知任意的銅或銅合金也可以,但若考慮用於電氣,電子機器之連接端子等,則最好係使用電氣傳導率較高者(譬如IACS(International Annealed Copper Standard:國際標準軟銅之導電率為100時的數值)為15至80%),譬如可舉出Cu-Sn-P(譬如磷青銅)、Cu-Zn(譬如黃銅、紅銅)、Cu-Ni-Zn(譬如洋白)、Cu-Ni-Si(銅鎳硅合金)、Cu-Fe-P合金等。另外,無特定限制金屬基材之形狀,即使板狀,條狀及壓擠品也可。Although not limited to the type of the metal substrate of the present invention, for example, stainless steel, copper or a copper alloy may be mentioned. Among them, materials such as martensite, ferrite, and austenite can be used as the stainless steel. In addition, although a base material for an electronic component such as a connector or a terminal is used as a copper or a copper alloy, any copper or copper alloy may be used. However, it is preferable to use a connection terminal for electric or electronic equipment. The system uses a higher electrical conductivity (such as IACS (International Annealed Copper Standard: the value of the international standard soft copper conductivity of 100) is 15 to 80%), such as Cu-Sn-P (such as phosphor bronze) , Cu-Zn (such as brass, copper), Cu-Ni-Zn (such as white), Cu-Ni-Si (copper-nickel-silicon alloy), Cu-Fe-P alloy. Further, the shape of the metal substrate is not particularly limited, and it may be a plate shape, a strip shape, or a compressed product.
於進行有鎳電鍍層之金屬基材表面上,具有加工變質層為大於等於0.2μm的厚度。若加工變質層為小於0.2μm,則形成於該表面之鎳電鍍所有組織或局部會變粗大,無法獲得一良好外觀之電鍍。所謂加工變質層乃藉由輾壓加工或拋光輪研磨等產生於金屬表面之結晶粒細微層。加工變質層的厚度最好為0.25至3.0μm,0.3至2.0μm為更佳。On the surface of the metal substrate on which the nickel plating layer is applied, the work-affected layer has a thickness of 0.2 μm or more. If the affected layer is less than 0.2 μm, all the structures or portions of the nickel plating formed on the surface become coarse, and a good appearance plating cannot be obtained. The so-called work-affected layer is a fine layer of crystal grains which is produced on the surface of the metal by press processing or polishing wheel polishing. The thickness of the work-affected layer is preferably 0.25 to 3.0 μm, more preferably 0.3 to 2.0 μm.
另外,於製造光澤鎳電鍍材料時,雖使用含有光澤劑之電鍍於金屬基材上來形成電鍍保護膜,但如上述所言,依據金屬基材表面的狀態有時候鎳電鍍的外觀不會很光澤。那是因為鎳電鍍具有容易受到基材的金屬結晶影響之特性。譬如,若金屬基材的結晶粒較為粗大,則電鍍的結晶粒也會變大,結果電鍍表面的凹凸也變大。故,電鍍外觀就變為不光澤。另外,若金屬基材的結晶粒較為細微,電鍍組織也變為細微,則電鍍表面就變為平滑。故,電鍍的外觀就變為光澤。In addition, in the production of a glossy nickel plating material, although a plating resist is formed by plating on a metal substrate using a gloss agent, as described above, depending on the state of the surface of the metal substrate, sometimes the appearance of nickel plating is not very glossy. . That is because nickel plating has characteristics that are easily affected by metal crystallization of the substrate. For example, when the crystal grains of the metal substrate are coarse, the crystal grains to be plated are also increased, and as a result, the unevenness of the plating surface is also increased. Therefore, the appearance of the plating becomes dull. Further, when the crystal grains of the metal substrate are fine and the plating structure is fine, the plating surface becomes smooth. Therefore, the appearance of plating becomes gloss.
(光澤鎳電鍍)(Gloss nickel plating)
本發明之光澤鎳電鍍材料,係於上述之加工過之金屬基材表面形成一鎳電鍍層。此鎳電鍍層係利用具有對應於金屬基材表面之金屬結晶粒大小的結晶粒直徑(小於0.3μm)所構成。此鎳電鍍層,如上述所言由於結晶粒直徑較為細微,故具有良好的光澤。另外,構成鎳電鍍層之鎳的結晶粒直徑最好為0.01至0.3μm。The glossy nickel plating material of the present invention is formed by forming a nickel plating layer on the surface of the processed metal substrate. This nickel plating layer is composed of a crystal grain diameter (less than 0.3 μm) having a metal crystal grain size corresponding to the surface of the metal substrate. This nickel plating layer has a good luster as described above because the crystal grain diameter is fine. Further, the crystal grains constituting the nickel plating layer preferably have a crystal grain diameter of 0.01 to 0.3 μm.
雖鎳電鍍層係以鎳所構成,但其中也含有極微量之有機光澤劑成分。此是因為光澤劑成分在電鍍步驟上有微量被滲入到保護膜。Although the nickel plating layer is made of nickel, it also contains a very small amount of organic luster component. This is because the gloss component is slightly infiltrated into the protective film during the plating step.
另外,本發明之端子,連接器等電子零件,係以上述光澤鎳電鍍材料所構成。Further, the electronic component such as the terminal or the connector of the present invention is composed of the above-mentioned glossy nickel plating material.
(光澤鎳電鍍材料的製造方法)(Manufacturing method of gloss nickel plating material)
首先,準備一以不鏽鋼,銅或銅合金等所形成之金屬基材。其次,再利用譬如輾壓、光軋機(skinpass)輾壓、拋光輪研磨、刷研磨而於金屬基材表面形成一加工變質層。加工的條件譬如調整輾壓加工度,拋光輪研磨時之壓力或時間讓加工變質層厚度為大於等於0.2μm。加工變質層的觀察係利用FIB(Focused Ion Beam:聚焦離子束)來進行剖面觀察再確認加工成功與否。First, a metal substrate formed of stainless steel, copper or a copper alloy or the like is prepared. Next, a work-affected layer is formed on the surface of the metal substrate by, for example, rolling, skinpass rolling, polishing wheel grinding, and brush grinding. The processing conditions are, for example, adjusting the degree of press working, and the pressure or time during polishing of the polishing wheel is such that the thickness of the processed metamorphic layer is 0.2 μm or more. The observation layer for processing the metamorphic layer is subjected to cross-sectional observation using FIB (Focused Ion Beam) to confirm the success of the processing.
其次,準備一光澤鎳電鍍浴槽。用於光澤鎳電鍍浴槽的光澤鎳電鍍液,具有水溶性鎳鹽,pH緩衝劑,光澤劑。Next, prepare a gloss nickel plating bath. A glossy nickel plating bath for a glossy nickel plating bath with a water soluble nickel salt, a pH buffer, and a gloss.
於此,水溶性鎳鹽譬如可舉出硫酸鎳、氯化鎳等,此等添加總計250至350g/L。Here, examples of the water-soluble nickel salt include nickel sulfate, nickel chloride, and the like, and the addition thereof is 250 to 350 g/L in total.
pH緩衝劑可舉出譬如硼酸、檸檬酸等,此等添加總計35至45g/L。The pH buffer may, for example, be boric acid, citric acid or the like, and these additions are 35 to 45 g/L in total.
光澤劑,可舉出譬如糖精、1-4丁炔二醇(1,4-butynediol),此等添加總計0.1至2g/L。As the glossing agent, for example, saccharin, 1,4-butynediol, and the like are added in a total amount of 0.1 to 2 g/L.
光澤鎳電鍍液為水溶液,pH值最好調整為3至5,調整到3.8至4.2為更佳。The gloss nickel plating solution is an aqueous solution, and the pH is preferably adjusted to 3 to 5, preferably to 3.8 to 4.2.
另外,光澤鎳電鍍液最好使用浴槽溫度為40至60℃,45至50℃為更佳。Further, the gloss nickel plating solution is preferably used at a bath temperature of 40 to 60 ° C, more preferably 45 to 50 ° C.
若光澤鎳電鍍液的pH值及浴槽溫度不在上述範圍,則會有電鍍速度變慢或容易產生外觀不良等問題。If the pH of the gloss nickel plating solution and the bath temperature are out of the above range, there is a problem that the plating speed is slow or the appearance is poor.
其次,將上述表面加工過的金屬基材既定時間浸漬於光澤電鍍浴槽內,即可獲得一具有光澤的光澤鎳電鍍基材。此時,於金屬基材表面,結晶粒子直徑最好小於1μm,且由於會形成厚度為0.01至0.2μm的加工變質層,因此形成於該表面之之電鍍層的金屬結晶粒子直徑也會變為較為細緻。故,所形成之電鍍層表面也會較為平滑而可獲得良好的光澤。Next, the surface-processed metal substrate is immersed in a gloss plating bath for a predetermined period of time to obtain a glossy gloss nickel plating substrate. At this time, the diameter of the crystal particles is preferably less than 1 μm on the surface of the metal substrate, and since a work-affected layer having a thickness of 0.01 to 0.2 μm is formed, the diameter of the metal crystal particles of the plating layer formed on the surface also becomes More detailed. Therefore, the surface of the formed plating layer is also smoother and a good gloss can be obtained.
以下為本發明之實施例,但此等實施例乃為更佳清楚明白本發明而提供,並非用以限制本發明。The following are examples of the invention, but are provided to provide a better understanding of the invention and are not intended to limit the invention.
(範例1:實施例1至10)(Example 1: Examples 1 to 10)
準備一厚度為0.65mm的黃銅板來作為金屬基材。於黃銅板表面藉由拋光輪研磨來形成如表1所示厚度之加工變質層。此變質層的厚度乃使用FIB來觀看。A brass plate having a thickness of 0.65 mm was prepared as a metal substrate. The surface of the brass plate was ground by a polishing wheel to form a work-affected layer having a thickness as shown in Table 1. The thickness of this metamorphic layer is viewed using FIB.
另外,藉由FIB來觀看構成金屬基材之加工變質層的金屬結晶粒子直徑。Further, the diameter of the metal crystal particles constituting the work-affected layer of the metal substrate was observed by FIB.
接著,準備一含有以下成分之光澤電鍍液的光澤電鍍浴槽。Next, a gloss plating bath containing the gloss plating solution of the following components was prepared.
NiSO4 ‧6H2 O 250g/lNiSO 4 ‧6H 2 O 250g/l
NiCl2 ‧6H2 O 50g/lNiCl 2 ‧6H 2 O 50g/l
硼酸 40糖精 2g/lBoric acid 40 saccharin 2g/l
1-4丁炔二醇 0.2g/l1-4 butynediol 0.2g/l
其次,將表面加工過的黃銅板經過脫脂、酸洗後,浸漬到電鍍浴槽再以電流密度為5A/dm2 來形成電鍍層。光澤電鍍浴槽設定pH值為4.0,溫度為45℃。Next, the surface-processed brass plate was degreased, pickled, and then immersed in an electroplating bath to form a plating layer at a current density of 5 A/dm 2 . The gloss plating bath was set to a pH of 4.0 and a temperature of 45 °C.
第1圖為表示實施例3之黃銅基材、加工變質層級鎳電鍍層的放大剖面圖。Fig. 1 is an enlarged cross-sectional view showing a brass base material and a modified graded nickel plating layer of Example 3.
比較例1至5,首先準備一與實施例相同的銅箔。其次,準備與實施例相同的電鍍浴槽,於此不對該黃銅板表面進行加工,或輕輕地以刷研磨等之輕微加工來進行電鍍。電鍍電流及浴槽溫度也設定成與實施例相同。In Comparative Examples 1 to 5, first, a copper foil similar to that of the Example was prepared. Next, the same plating bath as in the embodiment was prepared, and the surface of the brass plate was not processed, or the plating was lightly performed by light processing such as brush polishing. The plating current and bath temperature were also set to be the same as in the examples.
(評估)(assessment)
利用FIB來觀察構成鎳電鍍層之鎳結晶粒子直徑的剖面。The FIB was used to observe the profile of the diameter of the nickel crystal particles constituting the nickel plating layer.
對鎳電鍍層的光澤進行外觀觀察。使用光澤度計(日本電色工業製反射濃度計ND-1)來進行外觀評估,若測定值超過1.8就評估為○,若測定值位於1.6至1.8,則就評估為△,若測定值低於1.6就評估為×。The appearance of the nickel plating layer was observed. The appearance was evaluated using a gloss meter (Nippon Denshoku Industrial Reflectance Meter ND-1). If the measured value exceeds 1.8, the evaluation is ○. If the measured value is between 1.6 and 1.8, the evaluation is △, if the measured value is low. It is evaluated as × at 1.6.
表1為表示範例1及範例2的結果Table 1 shows the results of Example 1 and Example 2.
第1圖為表示實施例3之黃銅基材、加工變質層及鎳電鍍層的放大剖面圖。Fig. 1 is an enlarged cross-sectional view showing a brass base material, a work-affected layer and a nickel plated layer of Example 3.
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JP6141708B2 (en) * | 2013-07-09 | 2017-06-07 | 三菱伸銅株式会社 | Plated copper alloy plate with excellent gloss |
JP6805547B2 (en) * | 2015-09-18 | 2020-12-23 | アイシン精機株式会社 | Press fit terminal |
CN105543921A (en) * | 2015-12-28 | 2016-05-04 | 上海运安制版有限公司 | Nickel plating non-grinding process for production of printing roller |
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