JPS62174384A - Electroless gold plating solution - Google Patents
Electroless gold plating solutionInfo
- Publication number
- JPS62174384A JPS62174384A JP1381686A JP1381686A JPS62174384A JP S62174384 A JPS62174384 A JP S62174384A JP 1381686 A JP1381686 A JP 1381686A JP 1381686 A JP1381686 A JP 1381686A JP S62174384 A JPS62174384 A JP S62174384A
- Authority
- JP
- Japan
- Prior art keywords
- gold
- plating solution
- salt
- water
- gold plating
- 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.)
- Pending
Links
- 238000007747 plating Methods 0.000 title claims abstract description 35
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 25
- 239000010931 gold Substances 0.000 title claims abstract description 25
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000008139 complexing agent Substances 0.000 claims abstract description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003002 pH adjusting agent Substances 0.000 claims abstract 6
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract 4
- 150000001447 alkali salts Chemical class 0.000 claims abstract 3
- FEBPVRFEOOTRRX-UHFFFAOYSA-L dioxido-bis(sulfanylidene)-lambda6-sulfane gold(1+) Chemical compound S(=S)(=S)([O-])[O-].[Au+].[Au+] FEBPVRFEOOTRRX-UHFFFAOYSA-L 0.000 claims abstract 3
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 3
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical group [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- ZBKIUFWVEIBQRT-UHFFFAOYSA-N gold(1+) Chemical compound [Au+] ZBKIUFWVEIBQRT-UHFFFAOYSA-N 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- -1 thiocyanate ions Chemical class 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- JAJIPIAHCFBEPI-UHFFFAOYSA-N 9,10-dioxoanthracene-1-sulfonic acid Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)O JAJIPIAHCFBEPI-UHFFFAOYSA-N 0.000 abstract 2
- 239000000758 substrate Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- KJSBBMGOSZQGIZ-UHFFFAOYSA-H [Au+3].[Au+3].[O-]S([O-])(=S)=S.[O-]S([O-])(=S)=S.[O-]S([O-])(=S)=S Chemical compound [Au+3].[Au+3].[O-]S([O-])(=S)=S.[O-]S([O-])(=S)=S.[O-]S([O-])(=S)=S KJSBBMGOSZQGIZ-UHFFFAOYSA-H 0.000 description 1
- OBITVHZFHDIQGH-UHFFFAOYSA-N [Au].[K]C#N Chemical compound [Au].[K]C#N OBITVHZFHDIQGH-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910010277 boron hydride Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002594 fluoroscopy Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003077 quantum chemistry computational method Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- YOTORACCXKJMEH-UHFFFAOYSA-L sodium;gold(1+);oxido-oxo-sulfanylidene-sulfido-$l^{6}-sulfane Chemical compound [Na+].[Au+].[O-]S([S-])(=O)=S YOTORACCXKJMEH-UHFFFAOYSA-L 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- 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
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は無電解金めつき液、詳しくは高品質の金めつき
膜を短時間に厚付は可能で、しかも毒性の低い無電解金
めつき液に関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to an electroless gold plating solution, specifically an electroless gold plating solution that can thickly deposit a high quality gold plating film in a short time and has low toxicity. Regarding plating liquid.
従来の無電解金めつき液としては、シアン化金（Ｉ）カ
リウムを金源、シアン化カリウムを錯化剤、そして水素
化ホウ素す） ＩＪウムを還元剤とするものが、よく知
られている（ブレーティング（Ｐｌａｔｉｎｇ ）第５
７巻、１９７０年、頁９１４〜９２０）。As a conventional electroless gold plating solution, one that uses potassium gold(I) cyanide as the gold source, potassium cyanide as the complexing agent, and boron hydride (IJ) as the reducing agent is well known ( Plating 5th
7, 1970, pp. 914-920).
このめっき液は１．５μｍ／時のめつき速度で厚付は可
能であるが、シアンイオンを多葉に含むので液の毒性が
高く、実用上問題があった。Although this plating solution allows thick plating at a plating rate of 1.5 μm/hour, it is highly toxic because it contains many cyanide ions, which poses a practical problem.
本発明の目的は、上記の従来の無電解金めつき液と同等
の速度で厚付は可能で、しかもそれより毒性の低い無電
解金めつき液を提供することにある。An object of the present invention is to provide an electroless gold plating solution that can be thickened at a speed equivalent to that of the conventional electroless gold plating solution and is less toxic than the conventional electroless gold plating solution.
上記目的は、水浴性金塩および錯化剤としてジチオ硫酸
金アルカリ塩およびチオシアン酸を用いることによって
達成される。The above object is achieved by using a water-bathable gold salt and an alkali gold dithiosulfate salt and thiocyanic acid as complexing agents.
発明者は、金イオンと錯化剤とがつくる分子について量
子化学計算を行い、従来のシアンイオンにかわり得る錯
化剤としてチオシアンイオンが有望であることを見出し
た。またチオシアンイオンが無電解金めつき液の錯化剤
として有効であることが、釉々の実験からも確認できた
。The inventor performed quantum chemical calculations on molecules formed by gold ions and complexing agents, and found that thiocyanide ions are promising as complexing agents that can replace conventional cyanide ions. It was also confirmed through glazing experiments that thiocyanine ions are effective as complexing agents in electroless gold plating solutions.
次に本発明の無電解金めつき液の組成およびめっき条件
を示す。Next, the composition and plating conditions of the electroless gold plating solution of the present invention will be shown.
組成ニジチオ硫酸金（Ｉ）アルカリ塩（例えばナトリウ
ム塩、カリウム塩）１〜２０ ｐ／１千オジオシアン酸
イオンす化合物（例
えばナトリウム塩、カリウム塩
８＝２０ｇ／Ａ’
チオ尿素 １〜７５ｊｌ／１塩化アン
モニウム ５〜５０ ｇ７１条件：５０〜９０°
Ｃの液温で攪拌
１）Ｈ３〜１０
上記の無電解金めつき液によると１〜２μｍ／時のめつ
き速度が得られる。生じる全皮膜は緻密で、ワイヤボン
ディング性、ダイボンディング性、はんだ付は性などの
接続特性についてすぐれている。Composition Gold(I) dithiosulfate alkaline salt (e.g. sodium salt, potassium salt) 1-20 p/1,000 odiocyanate ion compound (e.g. sodium salt, potassium salt 8 = 20 g/A') Thiourea 1-75 jl/1 chloride Ammonium 5-50 g71 conditions: 50-90°
Stirring at a liquid temperature of C 1) H3 to 10 According to the above electroless gold plating solution, a plating rate of 1 to 2 μm/hour can be obtained. The resulting entire film is dense and has excellent connection properties such as wire bondability, die bondability, and solderability.
以下本発明の実施例を第１図により説明する。 Embodiments of the present invention will be described below with reference to FIG.
実施例１゜
図に示すように試験用のアルミナセラミック基板１のタ
ングステンメタライズパターン２を前処理して用いた。Example 1 As shown in the figure, a tungsten metallized pattern 2 on an alumina ceramic substrate 1 for testing was pretreated and used.
前処理は、脱脂→水洗→パラジウムによる活性化→水洗
→無電解ニッケルめつき→水洗の順に行った。無電解ニ
ッケルめっき膜は２〜３μｍの厚さであった。この基板
を次に示す組成のめつき液に、１時間浸した。Pretreatment was performed in the following order: degreasing → water washing → activation with palladium → water washing → electroless nickel plating → water washing. The electroless nickel plating film had a thickness of 2 to 3 μm. This substrate was immersed in a plating solution having the following composition for one hour.
ジチオ硫酸金（Ｉ）ナトリウム ５ ／ｌ／１チオ
シアン酸ナトリウム １０ｉ／１チオ尿素
３０．Ｆ ／ １塩化アンモニウム
１０９／１液温は８０℃に保ち、ｐＨ％５
．０とし液を攪拌した。めっき液から取り出し水洗後乾
燥した。この結果光沢のある金めつき膜が得られた。膜
厚は１４μｍであり、従来のシアンイオンを錯化剤とす
る無電解金めつき液と同等の速度であった。Sodium gold(I) dithiosulfate 5/l/1 Sodium thiocyanate 10i/1 Thiourea
30. F/ammonium monochloride
109/1 Keep the liquid temperature at 80℃, pH%5
．． The solution was stirred. It was taken out from the plating solution, washed with water, and then dried. As a result, a shiny gold-plated film was obtained. The film thickness was 14 μm, and the speed was equivalent to that of a conventional electroless gold plating solution using cyan ions as a complexing agent.
次に実施例１で得られた金めつき膜の評価を以下の方法
で行った。Next, the gold-plated film obtained in Example 1 was evaluated by the following method.
（１） ワイヤボンディング性
直径２５μｍのＡｌワイヤを約１５０°Ｃｔこ加熱した
モデル基板の金めつき膜上に圧接した。冷却後６ｇの荷
重をワイヤに加えて引張り、ワイヤがモデル基板から剥
れなかったものを良品とした。(1) Wire bonding property An Al wire with a diameter of 25 μm was pressure-bonded onto the gold-plated film of a model substrate heated to about 150°C. After cooling, a load of 6 g was applied to the wire and the wire was pulled, and those in which the wire did not peel off from the model board were considered good products.
（２） ダイボンディング性
４５０°Ｃで窒素雰囲気中シリコンペレットをスクラブ
しながら行い、Ｘｉｌ透視で金−シＩＪ 。(2) Die bonding properties: Performed at 450°C while scrubbing the silicon pellet in a nitrogen atmosphere, and inspected with gold-shield IJ using XIl fluoroscopy.
コン共晶で９０％以上濡れているものを良品とした。Those that were 90% or more wet with Con eutectic were considered good products.
（３）はんだ付は性
４６０°Ｃで空気中１５分間モデル基板を加熱後、金め
つき膜に、すんだディップを行い、膜表面が９５％以上
はんだで濡れているものを良品とした。(3) Soldering After heating the model board in air at 460°C for 15 minutes, the gold-plated film was dipped, and those with 95% or more of the film surface wet with solder were considered good.
（４）異常析出
金めつきしたモデル基板の表面を光学顕微鏡で観察し、
メタライズ層表面以外での金の析出のないものを良品と
した。(4) Observing the surface of the model substrate plated with abnormally deposited gold using an optical microscope,
Those with no gold precipitation on areas other than the surface of the metallized layer were considered to be non-defective.
以上の方法を用いて、実施例１によるサンプル２０個を
評価したところ、すべて良品と判定された。When 20 samples according to Example 1 were evaluated using the above method, all of them were determined to be non-defective.
本発明によれば、接続特性のすぐれた金めつき皮膜を、
短時間にしかも安全性の高い方法で形成できるので、金
めつきプロセスの効率化およびめっき設備の簡略化に大
きな効果がある。According to the present invention, a gold-plated film with excellent connection characteristics,
Since it can be formed in a short time and in a highly safe manner, it has great effects on increasing the efficiency of the gold plating process and simplifying the plating equipment.
図は本発明の実施例に用いた試験用モデルセラミック基
板の正面図である。The figure is a front view of a test model ceramic substrate used in an example of the present invention.
Claims (1)
からなる無電解金めつき液において、水溶性金塩がジチ
オ硫酸金（ I ）アルカリ塩であり、錯化剤がチオシア
ン酸イオンであり、ｐＨ調整剤が塩化アンモニウムであ
り、還元剤がチオ尿素であることを特徴とする無電解金
めつき液。 ２、水溶性金塩、錯化剤、ＰＨ調整剤、還元剤および水
からなる無電解金めつき液において、水溶性金塩がジチ
オ硫酸金（ I ）アルカル塩であり、錯化剤がチオシア
ン酸イオンであり、ｐＨ調整剤が無電解金めつき液のＰ
Ｈが３．０〜１０．０となるだけの量の塩化アンモニウ
ムとその他のｐＨ調整剤の混合物であり、還元剤がチオ
尿素であることを特徴とする無電解金めつき液。[Claims] 1. In an electroless gold plating solution comprising a water-soluble gold salt, a complexing agent, a pH adjuster, a reducing agent, and water, the water-soluble gold salt is an alkali salt of gold(I) dithiosulfate. An electroless gold plating solution characterized in that the complexing agent is thiocyanate ion, the pH adjusting agent is ammonium chloride, and the reducing agent is thiourea. 2. In an electroless gold plating solution consisting of a water-soluble gold salt, a complexing agent, a PH adjuster, a reducing agent, and water, the water-soluble gold salt is a dithiosulfate gold (I) alkal salt, and the complexing agent is a thiocyanide. It is an acid ion, and the pH adjuster is P in the electroless gold plating solution.
An electroless gold plating solution characterized in that it is a mixture of ammonium chloride and other pH adjusting agents in an amount sufficient to give H of 3.0 to 10.0, and the reducing agent is thiourea.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1381686A JPS62174384A (en) | 1986-01-27 | 1986-01-27 | Electroless gold plating solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1381686A JPS62174384A (en) | 1986-01-27 | 1986-01-27 | Electroless gold plating solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62174384A true JPS62174384A (en) | 1987-07-31 |
Family
ID=11843800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1381686A Pending JPS62174384A (en) | 1986-01-27 | 1986-01-27 | Electroless gold plating solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62174384A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5302256A (en) * | 1991-06-25 | 1994-04-12 | Learonal Japan Inc. | Immersion tin/lead alloy plating bath |
| JP2009030721A (en) * | 2007-07-26 | 2009-02-12 | Panasonic Electric Works Co Ltd | Motor mounting structure |
| WO2014072969A1 (en) * | 2012-11-09 | 2014-05-15 | Ben Gurion University Of The Negev Research And Development Authority | Gold nanostructures and processes for their preparation |
-
1986
- 1986-01-27 JP JP1381686A patent/JPS62174384A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5302256A (en) * | 1991-06-25 | 1994-04-12 | Learonal Japan Inc. | Immersion tin/lead alloy plating bath |
| JP2009030721A (en) * | 2007-07-26 | 2009-02-12 | Panasonic Electric Works Co Ltd | Motor mounting structure |
| WO2014072969A1 (en) * | 2012-11-09 | 2014-05-15 | Ben Gurion University Of The Negev Research And Development Authority | Gold nanostructures and processes for their preparation |
| US10895013B2 (en) | 2012-11-09 | 2021-01-19 | Ben Gurion University Of The Negev Research And Development Authority | Gold nanostructures and processes for their preparation |
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