JPS6341998B2 - - Google Patents
Info
- Publication number
- JPS6341998B2 JPS6341998B2 JP14872881A JP14872881A JPS6341998B2 JP S6341998 B2 JPS6341998 B2 JP S6341998B2 JP 14872881 A JP14872881 A JP 14872881A JP 14872881 A JP14872881 A JP 14872881A JP S6341998 B2 JPS6341998 B2 JP S6341998B2
- Authority
- JP
- Japan
- Prior art keywords
- silver
- nickel
- plating
- silver plating
- nickel alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 40
- 238000007747 plating Methods 0.000 claims description 40
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 37
- 229910052709 silver Inorganic materials 0.000 claims description 35
- 239000004332 silver Substances 0.000 claims description 35
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 17
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 239000010931 gold Substances 0.000 claims description 7
- -1 alkali metal citrate Chemical class 0.000 claims description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 4
- 150000002344 gold compounds Chemical class 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 206010040844 Skin exfoliation Diseases 0.000 description 5
- 238000002845 discoloration Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910000833 kovar Inorganic materials 0.000 description 3
- XTFKWYDMKGAZKK-UHFFFAOYSA-N potassium;gold(1+);dicyanide Chemical compound [K+].[Au+].N#[C-].N#[C-] XTFKWYDMKGAZKK-UHFFFAOYSA-N 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001508 potassium citrate Substances 0.000 description 2
- 229960002635 potassium citrate Drugs 0.000 description 2
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 2
- 235000011082 potassium citrates Nutrition 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 229920000298 Cellophane Polymers 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical class [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Landscapes
- Electroplating Methods And Accessories (AREA)
Description
【発明の詳細な説明】
本発明はニツケル又はニツケル合金の銀めつき
方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for silver plating nickel or nickel alloys.
従来、ニツケル又はニツケル合金（例えば
42Alloy―Ni42％、Fe残部、Kcvar―Ni29％、
コバール17％、Fe残部）を銀めつきするには、
素地に対する銀めつきの密着性が悪いのでこれを
向上させるため、素地に銅又は銀ストライクめつ
きを施す必要がある。そして銅ストライクめつき
を施した場合には、置換反応によつて銅ストライ
クめつき面に銀が析出し易いので置換防止剤で銀
ストライクめつき面を処理して置換防止を行なう
必要もあつた。更に、ニツケル又はニツケル合金
が電気、電子部品、例えばICリードフレームの
ような場合には、銀めつき後の工程で錫めつき、
半田その他の処理を行なうのでこの後工程に於け
る錫めつきや半田の「のり」を良くしておくため
銀本めつき処理で部分的に銀めつきした部分以外
のいわば余分な銅ストライクめつき、銀ストライ
クめつきを剥離処理にて剥離除去する必要があつ
た。従つて、従来のニツケル又はニツケル合金の
銀めつき方法では、銀本めつき処理の前にストラ
イクめつき、置換防止処理（銅ストライクめつき
した場合のみ）が、そして又銀本めつき処理後に
ストライクに対する剥離処理が、それぞれ不可欠
で銀めつき処理が複雑になるという不都合があつ
た。更に剥離処理を行なえば銀本めつきを施した
近辺を剥離することになつて品質が低下するとい
う不都合もあつた。 Traditionally, nickel or nickel alloys (e.g.
42Alloy-Ni42%, Fe balance, Kcvar-Ni29%,
To silver plate Kovar (17%, Fe balance),
Since the adhesion of silver plating to the substrate is poor, in order to improve this, it is necessary to apply copper or silver strike plating to the substrate. When copper strike plating is applied, silver tends to precipitate on the copper strike plating surface due to a substitution reaction, so it is necessary to treat the silver strike plating surface with a substitution inhibitor to prevent substitution. . Furthermore, when nickel or nickel alloy is used for electrical or electronic parts, such as IC lead frames, tin plating is performed in the process after silver plating.
Since soldering and other treatments are performed, in order to improve tin plating and solder "glue" in subsequent processes, extra copper strike metal is used in areas other than the partially silvered areas in the silver plating process. It was necessary to remove the silver strike plating using a peeling process. Therefore, in the conventional silver plating method for nickel or nickel alloy, strike plating and displacement prevention treatment (only when copper strike plating is performed) are performed before the silver main plating process, and then after the silver main plating process. There was an inconvenience that a stripping process for each strike was necessary, making the silver plating process complicated. Furthermore, if a peeling treatment was performed, the area near where the silver plating was applied would be peeled off, resulting in an inconvenience in that the quality would deteriorate.
本発明はこのような従来の銀めつき方法に着目
してなされたもので、銅や銀のストライクめつき
を行なうことなく直接ニツケル又はニツケル合金
の素地に銀めつき処理を行なうことのできる銀め
つき方法を提供せんとするものである。 The present invention has been made by focusing on such conventional silver plating methods, and is a silver plating method that can directly silver plate a nickel or nickel alloy substrate without performing strike plating with copper or silver. The purpose is to provide a plating method.
そして具体的には、本発明はニツケル又はニツ
ケル合金の素地を、クエン酸４〜15ｇ／、クエ
ン酸アルカリ金属塩40〜120ｇ／、水溶性金化
合物20〜85p.p.m（金属金として）、を含む前処理
液中で電解処理し、次いで直接銀めつき処理する
ことを特徴とするニツケル又はニツケル合金の銀
めつき方法に係るものである。 Specifically, the present invention prepares a base of nickel or nickel alloy by adding 4 to 15 g of citric acid, 40 to 120 g of alkali metal citrate, and 20 to 85 p.pm of a water-soluble gold compound (as metallic gold). This invention relates to a method for silver plating nickel or a nickel alloy, which is characterized by electrolytically treating nickel or a nickel alloy in a pretreatment solution containing the present invention, and then directly silver plating the nickel or nickel alloy.
以下、本発明の詳細を述べる。先ず本発明では
以下の組成よりなる前処理液を用いてニツケル又
はニツケル合金の素地を前処理するものである。 The details of the present invention will be described below. First, in the present invention, a nickel or nickel alloy substrate is pretreated using a pretreatment liquid having the following composition.
クエン酸 ４〜150ｇ／
クエン酸アルカリ金属塩 40〜120ｇ／
水溶性金化合物 20〜85p.p.m（金属金として）
前処理の操作条件では、例えば以下の条件が好
適である。Citric acid 4-150g/Alkali metal citrate 40-120g/Water-soluble gold compound 20-85p.pm (as metallic gold) As for the operating conditions for pretreatment, the following conditions are suitable, for example.
温 度 50〜65℃
時 間 10〜30秒
電 圧 ３〜7v
上記組成の前処理液、上記の操作条件で、ニツ
ケル又はニツケル合金の素地を（−）、前処理液
を（＋）として電解前処理しておけば密着性が向
上して銅乃至銀のストライクめつきを施すことな
く、直接素地に銀めつき処理を施すことができる
ものである。 Temperature: 50 to 65℃ Time: 10 to 30 seconds Voltage: 3 to 7V Electrolyze with the pretreatment liquid of the above composition and the above operating conditions, with the nickel or nickel alloy substrate as (-) and the pretreatment liquid as (+). Pretreatment improves adhesion and allows silver plating to be applied directly to the substrate without performing copper or silver strike plating.
そして、この電解前処理に次いで6μ銀めつき
したニツケル合金に種々の耐熱テスト（例えば大
気中で480℃、５分又は360℃、２時間）を施した
ところ変色もふくれも全然見当らず、光沢ニツケ
ルから無光沢ニツケルのもの全部に本発明方法が
有効であることがその他の種々のテストより判明
した。このことはニツケル又はニツケル合金であ
れば42Alloy、コバールを問わずどのような素地
にも適応できることを意味している。更に、銀め
つきを施した部分の近辺を分析したところ、銀の
析出は検出されず銀めつきがその周囲に全く置換
していないことも確認できた。 Following this electrolytic pretreatment, the 6μ silver-plated nickel alloy was subjected to various heat resistance tests (for example, 480°C for 5 minutes in the air or 360°C for 2 hours), and no discoloration or blistering was observed. Various other tests have shown that the method of the present invention is effective for all types of nickel, from nickel to matte nickel. This means that it can be applied to any substrate, whether it is nickel or nickel alloy, 42Alloy, or Kovar. Furthermore, when the area around the silver-plated area was analyzed, no silver precipitation was detected, and it was confirmed that the silver plating had not replaced the surrounding area at all.
以下に実施例を示す。 Examples are shown below.
〔実施例 １〕
前処理液組成
クエン酸 ４ｇ／
クエン酸カリウム 45ｇ／
金シアン化カリ 20p.p.m（金属金として）
操作条件
温 度 50℃
時 間 30秒
電 圧 6V
以上の条件で、予めニツケルメツキしたコネク
ターに電解前処理を施し次いで6μ銀めつきを施
した。このコネクターに市販のセロハンテープ
〔商品名〕を張付け剥離テストを行なつたが銀め
つき膜は全く剥離せず密着性の向上していること
が確認できた。更に480℃、５分間の耐熱テスト
を施したが、変色やふくれは皆無であつた。[Example 1] Pre-treatment liquid composition Citric acid 4g/Potassium citrate 45g/Potassium gold cyanide 20p.pm (as metal gold) Operating conditions Temperature 50°C Time 30 seconds Voltage 6V or above, nickel plated in advance The prepared connector was subjected to electrolytic pretreatment and then 6μ silver plating was applied. Commercially available cellophane tape (trade name) was attached to this connector and a peel test was performed, but the silver plating film did not peel off at all, confirming that the adhesion had improved. Furthermore, a heat resistance test was conducted at 480°C for 5 minutes, but there was no discoloration or blistering.
又、同じコネクターにつき、本発明の前処理を
施さず銀めつきしたものに剥離テストを行なつた
ところ銀めつき膜は容易に剥離した。 Further, when a peel test was conducted on the same connector, which was silver-plated without being subjected to the pretreatment of the present invention, the silver-plated film was easily peeled off.
〔実施例 ２〕
前処理液組成
クエン酸 15ｇ／
クエン酸ナトリウム 80ｇ／
金シアン化カリ 80p.p.m（金属金として）
操作条件
温 度 65℃
時 間 10秒
電 圧 3V
以上の条件でコバール材ICリードフレームを
電解前処理して6μ銀めつきを施し、実施例１と
同様の剥離テストと360℃で２時間の耐熱テスト
を行なつたところ、銀めつきは全然剥離せず、又
変色やふくれも生じなかつた。[Example 2] Pretreatment liquid composition Citric acid 15g / Sodium citrate 80g / Potassium gold cyanide 80p.pm (as metal gold) Operating conditions Temperature 65℃ Time 10 seconds Voltage Kovar material IC under conditions of 3V or more The lead frame was electrolytically pretreated and plated with 6μ silver, and a peel test similar to that in Example 1 and a heat resistance test at 360°C for 2 hours were conducted.The silver plating did not peel off at all, and there was no discoloration or discoloration. No blistering occurred.
〔実施例 ３〕
前処理液
クエン酸 10ｇ／
クエン酸カリウム 80ｇ／
金シアン化カリ 40p.p.m（金属金として）
操作条件
温 度 60℃
時 間 20秒
電 圧 6V
以上の条件で、42Alloy材の半導体のリード線
を電解前処理し、次いで6μ銀めつきを施した。
このリード線に90゜の折り曲げテストを行なつた
が銀めつきの剥離はなく、又360℃で２時間の耐
熱テストを施したが変色やふくれの発生は皆無で
あつた。[Example 3] Pretreatment liquid citric acid 10g/potassium citrate 80g/potassium gold cyanide 40p.pm (as metal gold) Operating conditions Temperature 60°C Time 20 seconds Voltage 6V or higher conditions The semiconductor lead wires were electrolytically pretreated and then plated with 6μ silver.
This lead wire was subjected to a 90° bending test, but no peeling of the silver plating was observed, and a heat resistance test at 360°C for 2 hours showed no discoloration or blistering.
以上説明してきたように、本発明によれば、ニ
ツケル又はニツケル合金の素地を、クエン酸４〜
15ｇ／、クエン酸アルカリ金属塩40〜120ｇ／
、水溶性金化合物20〜85p.p.m（金属金とし
て）、を含む前処理液中で電解処理し、次いで直
接銀めつき処理することとしたため、ニツケル又
はニツケル合金の素地に銅乃至は銀ストライクめ
つきすることが全く不要となり前処理液による前
処理のみでいわば銀めつきをじか付けすることが
可能でしかもストライクめつきのみならず置換防
止処理、剥離処理も不要とすることができて従来
の銀めつき方法に比べ処理工程を格段に単純化且
つ短縮化できて銀めつきのめつき処理効率を非常
に向上することができ且つ大幅なコストダウンを
期待することができる。そして剥離処理の省略に
より銀めつきのロスがなくなりしかも品質が安定
するという効果もある。 As explained above, according to the present invention, the base material of nickel or nickel alloy is
15g/, citric acid alkali metal salt 40-120g/
, a water-soluble gold compound of 20 to 85 p.pm (as metallic gold) was electrolytically treated in a pretreatment solution, and then directly silver-plated, so a copper or silver strike was applied to the nickel or nickel alloy base. There is no need for plating at all, and it is possible to directly apply silver plating just by pre-treatment with a pre-treatment liquid.In addition to eliminating the need for strike plating, displacement prevention treatment and peeling treatment can also be eliminated. Compared to conventional silver plating methods, the processing steps can be significantly simplified and shortened, the plating processing efficiency of silver plating can be greatly improved, and a significant cost reduction can be expected. Omitting the peeling process also has the effect of eliminating silver plating loss and stabilizing quality.
Claims (1)
酸４〜15ｇ／、クエン酸アルカリ金属塩40〜
120ｇ／、水溶性金化合物20〜85p.p.m（金属金
として）、を含む前処理液中で電解処理し、次い
で直接銀めつき処理することを特徴とするニツケ
ル又はニツケル合金の銀めつき方法。1. Add 4 to 15 g of citric acid and 40 to 40 g of alkali metal citrate to the base of nickel or nickel alloy.
A method for silver plating nickel or nickel alloy, characterized by electrolytically treating it in a pretreatment solution containing 120 g/water-soluble gold compound and 20 to 85 p.pm (as metallic gold), and then directly silver plating it. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14872881A JPS5852497A (en) | 1981-09-22 | 1981-09-22 | Silver plating method for nickel or nickel alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14872881A JPS5852497A (en) | 1981-09-22 | 1981-09-22 | Silver plating method for nickel or nickel alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5852497A JPS5852497A (en) | 1983-03-28 |
| JPS6341998B2 true JPS6341998B2 (en) | 1988-08-19 |
Family
ID=15459278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14872881A Granted JPS5852497A (en) | 1981-09-22 | 1981-09-22 | Silver plating method for nickel or nickel alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5852497A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5858295A (en) * | 1981-09-30 | 1983-04-06 | Electroplating Eng Of Japan Co | Pretreating solution for silver plating, silver plating method and substrate |
-
1981
- 1981-09-22 JP JP14872881A patent/JPS5852497A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5852497A (en) | 1983-03-28 |
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