JP4716760B2 - Gold plating solution and gold plating method - Google Patents
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Description
本発明は、金めっき液および金めっき方法に関する。 The present invention relates to a gold plating solution and a gold plating method.
金めっきは、多くの電子部品に施されている。金めっき膜は、酸化しにくく、耐食性にも優れ、配線の保護膜として適しているからである。
一方、カーボンナノファイバーは、導電性、伝熱性、および強度に優れることから、種々の用途が開発されている。
特開２００４−２５３２２９には、金めっき膜中にカーボンナノファイバーを含ませ、接点部材として用いる技術が開示されている。
On the other hand, since carbon nanofibers are excellent in conductivity, heat conductivity, and strength, various applications have been developed.
Japanese Patent Laid-Open No. 2004-253229 discloses a technique in which carbon nanofibers are included in a gold plating film and used as a contact member.
ところで、上記特開２００４−２５３２２９に示されている金めっき液は、シアン系の金めっき液であり、環境に負荷を与える課題がある。
そこで、本発明は、非シアン系のもので、環境への負荷を軽減でき、また、カーボンナノファイバーを好適に膜中に取り込める金めっき液およびこれを用いた金めっき方法を提供するものである。
By the way, the gold plating solution shown by the said Unexamined-Japanese-Patent No. 2004-253229 is a cyan-type gold plating solution, and there exists a subject which gives a load to an environment.
Therefore, the present invention provides a gold plating solution that is non-cyan, can reduce the burden on the environment, and can suitably incorporate carbon nanofibers into the film, and a gold plating method using the same. .
本発明に係る金めっき液は、塩化金酸塩を主体とする非シアン系金めっき液において、トリメチルステアリルアンモニウムクロリドからなる界面活性剤とカーボンナノファイバーとを含むことを特徴とする。
トリメチルステアリルアンモニウムクロリドを０．０２〜５ｇ／ｌ、カーボンナノファイバーを０．１〜１０ｇ／ｌ含むことを特徴とする。
The gold plating solution according to the present invention is a non-cyanide gold plating solution mainly composed of chloroaurate, and contains a surfactant composed of trimethylstearyl ammonium chloride and carbon nanofibers.
It is characterized by containing 0.02 to 5 g / l of trimethylstearyl ammonium chloride and 0.1 to 10 g / l of carbon nanofibers .
本発明に係る金めっき方法は、上記金めっき液を用い、被めっき物に電解金めっきを行うことを特徴とする。
被めっき物が、コネクタ、その他の電子部品であることを特徴とする。
極性を反転させるサイクルを複数回繰り返す逆電流法によりめっきを行うと好適である。
The gold plating method according to the present invention is characterized in that electrolytic gold plating is performed on an object to be plated using the gold plating solution.
The object to be plated is a connector or other electronic component.
Plating is preferably performed by a reverse current method in which a cycle for reversing the polarity is repeated a plurality of times .
本発明によれば、非シアン系の金めっき液であって、環境への負荷を軽減できるとともに、カーボンナノファイバーを金めっき皮膜中に取り込むことができ、電子部品の金めっきに用いて好適である。 According to the present invention, it is a non-cyanide gold plating solution that can reduce the burden on the environment and can incorporate carbon nanofibers into the gold plating film, which is suitable for use in gold plating of electronic components. is there.
以下本発明における最良の実施の形態を詳細に説明する。
本発明に係る金めっき液は、塩化金酸塩を主体とする非シアン系金めっき液において、トリメチルステアリルアンモニウムクロリドからなるカチオン系界面活性剤とカーボンナノファイバーとを含むことを特徴とするものである。
塩化金酸塩としては、塩化金酸ナトリウムが好適であり、亜硫酸ナトリウム等の亜硫酸塩を添加することにより、亜硫酸金錯体を形成する。
また、必要に応じて、2,2´−ビピリジル：（Ｃ5Ｈ4Ｎ）2などの安定剤を添加するとよい。
上記非シアン系の基本金めっき液は公知のものである。各成分の添加量としては、塩化金酸塩が０．０５Ｍ程度、亜硫酸塩が０．５Ｍ程度、安定剤が１００ｐｐｍ程度が好適であるが、もちろんこれに限定されるものではない。
The best mode of the present invention will be described in detail below.
A gold plating solution according to the present invention is a non-cyanide gold plating solution mainly composed of chloroaurate, and includes a cationic surfactant composed of trimethylstearyl ammonium chloride and carbon nanofibers. is there.
As the chloroaurate, sodium chloroaurate is suitable, and a gold sulfite complex is formed by adding a sulfite such as sodium sulfite.
If necessary, a stabilizer such as 2,2′-bipyridyl: (C 5 H 4 N) 2 may be added.
The non-cyan basic gold plating solution is known. The addition amount of each component is preferably about 0.05 M chloroaurate, about 0.5 M sulfite, and about 100 ppm stabilizer, but is not limited to this.
トリメチルステアリルアンモニウムクロリドからなる界面活性剤の添加量は０．０２〜５ｇ／ｌ、カーボンナノファイバーの添加量は０．１〜１０ｇ／ｌが好適である。
界面活性剤は、その他のカチオン系界面活性剤および／またはノニオン系界面活性剤を用いることができる。
The addition amount of the surfactant made of trimethylstearyl ammonium chloride is preferably 0.02 to 5 g / l, and the addition amount of the carbon nanofiber is preferably 0.1 to 10 g / l.
As the surfactant, other cationic surfactants and / or nonionic surfactants can be used .
カチオン系界面活性剤としては、トリメチルステアリルアンモニウムクロリド：Ｃ21Ｈ46ＣｌＮ、ベンジルオクタデシルジメチルアンモニウムクロリド：Ｃ27Ｈ50ＣｌＮ、ジアリルジメチルアンモニウムクロリド２０％：［（ＣＨ2ＣＨＣＨ2）2Ｎ（ＣＨ3）2］Ｃｌ、塩化ベンザルコニウム：［Ｃ6Ｈ5ＣＨ2Ｎ（ＣＨ3）2Ｒ］Ｃｌを用いることができる。特にトリメチルステアリルアンモニウムクロリドを用いると、カーボンナノファイバーが金めっき液中で均一に分散し、また、電解めっきを行った際、金めっき膜中へのカーボンナノファイバーの取り込み量も多く、好適であった。 Examples of the cationic surfactant include trimethyl stearyl ammonium chloride: C 21 H 46 ClN, benzyl octadecyl dimethyl ammonium chloride: C 27 H 50 ClN, diallyl dimethyl ammonium chloride 20%: [(CH 2 CHCH 2 ) 2 N (CH 3 ) 2 ] Cl, benzalkonium chloride: [C 6 H 5 CH 2 N (CH 3 ) 2 R] Cl can be used. In particular, when trimethylstearyl ammonium chloride is used, the carbon nanofibers are uniformly dispersed in the gold plating solution, and the amount of carbon nanofibers incorporated into the gold plating film is large when electrolytic plating is performed. It was.
また、ノニオン系界面活性剤としては、ポリオキシエチレン(2)ノニルフェニルエーテル：（Ｃ9Ｈ19−Ｃ6Ｈ4Ｏ−（Ｃ2Ｈ4Ｏ）2Ｈ、ポリアクリル酸５０００、ポリオキシエチレン(23)ラウリルエーテル：Ｃ12Ｈ25（ＯＣＨ2ＣＨ2）23ＯＨ、ポリエチレングリコール２０００：ＨＯ（ＣＨ2ＣＨ2Ｏ）nＨを用いることができる。
なお、これらの界面活性剤は単独でも、併用してもよい。
As the nonionic surfactant, polyoxyethylene (2) nonylphenyl ether: (C 9 H 19 -C 6 H 4 O- (C 2 H 4 O) 2 H, polyacrylic acid 5000, polyoxyethylene (23) Lauryl ether: C 12 H 25 (OCH 2 CH 2 ) 23 OH, polyethylene glycol 2000: HO (CH 2 CH 2 O) n H can be used.
These surfactants may be used alone or in combination.
めっき液のｐＨは、７（中性）〜アルカリ側とし、例えばｐＨ８前後に調整するとよい。浴温は、室温〜９０℃とし、例えば６０℃程度がよい。電流密度は０．１〜５０ｍＡ／ｃｍ2とし、例えば５ｍＡ／ｃｍ2程度がよい。陽極は白金めっきを行ったチタン製（メッシュ）のものなどが好適である。
コネクタその他の電子部品等の被めっき物に電解めっきを行うことによって、金めっき膜によりカーボンナノファイバーが取り込まれためっき皮膜を得ることができる。
金めっき皮膜中にカーボンナノファイバーが取り込まれることによって、例えばコネクタや接点の場合、導電性が向上し、接触抵抗が減少し、チャタリングなども減少することが期待できる。
なお、極性を反転させるサイクルを複数回繰り返す逆電流法によりめっきを行うようにするとより好適に金めっきを行うことができる。
また、界面活性剤やカーボンナノファイバーは、金めっきを行う直前に、上記の基本めっき液に添加するようにしてもよい。
The pH of the plating solution is 7 (neutral) to the alkali side, and may be adjusted to about pH 8, for example. The bath temperature is from room temperature to 90 ° C., for example, about 60 ° C. is preferable. The current density was set to 0.1~50mA / cm 2, for example, it is about 5 mA / cm 2. The anode is preferably made of titanium (mesh) plated with platinum.
By performing electrolytic plating on an object to be plated such as a connector or other electronic component, a plating film in which carbon nanofibers are taken in by a gold plating film can be obtained.
By incorporating carbon nanofibers into the gold plating film, for example, in the case of connectors and contacts, it can be expected that conductivity is improved, contact resistance is reduced, and chattering is also reduced.
Note that gold plating can be performed more suitably if plating is performed by the reverse current method in which a cycle for reversing the polarity is repeated a plurality of times.
Moreover, you may make it add surfactant and carbon nanofiber to said basic plating solution just before performing gold plating.
次の基本金めっき液を作成した。
塩化金酸（III）ナトリウム ＮａＡｕＣｌ4・２Ｈ2Ｏ ０．０５Ｍ
亜硫酸ナトリウム Ｎａ2ＳＯ3 ０．５Ｍ
2,2´-ビピリジル （Ｃ5Ｈ4Ｎ）2 ０．１ｇ／ｌ
この基本金めっき浴を用いて、次の条件により金めっきを行った際の金めっき膜の表面のＳＥＭ写真を図１（ａ）、（ｂ）に示す。光沢めっき皮膜が得られている。図１（ａ）は２０００倍、図１（ｂ）は５０００倍のものである（以下の図も、（ａ）は２０００倍、（ｂ）は５０００倍である）。
電流密度：５ｍＡ／ｃｍ2、ｐＨ：８、浴温度：６０℃、クーロン量：９．４６Ｃ、被めっき電極の面積：２ｃｍ2、非めっき物：ニッケルめっきを行った銅板
The following basic gold plating solution was prepared.
Sodium chloroaurate (III) NaAuCl 4 · 2H 2 O 0.05M
Sodium sulfite Na 2 SO 3 0.5M
2,2′-bipyridyl (C 5 H 4 N) 2 0.1 g / l
FIGS. 1A and 1B show SEM photographs of the surface of the gold plating film when gold plating is performed under the following conditions using this basic gold plating bath. A bright plating film is obtained. 1 (a) is 2000 times and FIG. 1 (b) is 5000 times (the following figures are also 2000 times and (b) is 5000 times).
Current density: 5 mA / cm 2 , pH: 8, bath temperature: 60 ° C., Coulomb amount: 9.46 C, area of electrode to be plated: 2 cm 2 , non-plated material: copper plate subjected to nickel plating
上記基本金めっき液に、トリメチルステアリルアンモニウムクロリドを１ｇ／ｌ、カーボンナノファイバー（以下ＣＮＴという）を２ｇ／ｌ添加した金めっき液を調整し、上記と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図２（ａ）、（ｂ）に示す。多数の金めっき粒子が寄り集まった比較的大きな粒子にＣＮＴの端部が埋没して取り込まれ、ＣＮＴの他端側が突出して他の粒子に取り込まれた構造のものとなっている。ＣＮＴが取り込まれたことで、金めっき皮膜は、比較的に荒い表面状態の黒っぽい色の皮膜となっている。取り込まれたＣＮＴ量は、金めっき皮膜量に対して、数vol％〜１０vol％程度で、多量のＣＮＴが取り込まれている。 A gold plating solution prepared by adding 1 g / l of trimethylstearyl ammonium chloride and 2 g / l of carbon nanofiber (hereinafter referred to as CNT) to the above basic gold plating solution, and performing gold plating under the same plating conditions as above SEM photographs of the surface of the plating film are shown in FIGS. 2 (a) and 2 (b). The structure is such that the end of the CNT is buried and taken in relatively large particles in which a large number of gold plating particles are gathered, and the other end of the CNT protrudes and is taken in by other particles. Since the CNTs are taken in, the gold plating film is a blackish film with a relatively rough surface state. The amount of CNT taken in is about several vol% to 10 vol% with respect to the amount of the gold plating film, and a large amount of CNT is taken in.
実施例１と同様の金めっき液を用い、逆電流法を用いて金めっきを行った。その他のめっき条件は実施例１と同一である。めっきシステムは、北斗電工（株）による電気化学測定システム「ＨＺ−３０００」を使用した。
逆電流法は、初期安定期３０秒間は電流を流さず、その後は、図３に示すように、５ｍＡ／ｃｍ2で３０秒間めっきをして、次いで３０秒間電流を流さず安定させ、次に逆方向に（極性を反転させて）２４０ｍＡ／ｃｍ2で５秒間電流を流してめっき皮膜を溶かし、次に３０秒間電流を流さずに安定させる。このサイクルを３１回繰り返して行った（析出９．４６Ｃ狙い）。得られた金めっき膜の表面のＳＥＭ写真を図４（ａ）、（ｂ）に示す。図２のものに比較すると、金めっき粒子が寄り集まった粒子は小さくなり、また、露出していたＣＮＴ表面にも金めっき粒子が付着し、樹枝状となっていて、さらに平坦さが増加した。
なお、電流反転時間は上記に限られず、数ｍ秒、あるいは数μ秒サイクルで電流を反転するパルスめっきであってもよい。
Using the same gold plating solution as in Example 1, gold plating was performed using the reverse current method. Other plating conditions are the same as those in Example 1. As a plating system, an electrochemical measurement system “HZ-3000” by Hokuto Denko Co., Ltd. was used.
In the reverse current method, no current is passed for 30 seconds in the initial stable period, and thereafter, as shown in FIG. 3, plating is performed at 5 mA / cm 2 for 30 seconds, then the current is stabilized for 30 seconds, and then, In the opposite direction (with polarity reversed), current is applied at 240 mA / cm 2 for 5 seconds to dissolve the plating film, and then stabilized without current for 30 seconds. This cycle was repeated 31 times (precipitation 9.46C aim). 4A and 4B show SEM photographs of the surface of the obtained gold plating film. Compared with that of FIG. 2, the particles with gold plating particles gathered smaller, and the gold plating particles adhered to the exposed CNT surface, forming a dendritic shape, and the flatness increased further. .
The current reversal time is not limited to the above, and pulse plating that reverses the current in a cycle of several milliseconds or several microseconds may be used.
上記基本金めっき液に、ベンジルオクタデシルメチルアンモニウムクロリドを１ｇ／ｌ、ＣＮＴを２ｇ／ｌ添加した金めっき液を調整し、実施例１と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図５（ａ）、（ｂ）に示す。取り込み量は少ないがＣＮＴが金めっき皮膜に取り込まれている。 The surface of the gold plating film prepared by preparing a gold plating solution in which 1 g / l of benzyloctadecylmethylammonium chloride and 2 g / l of CNT were added to the above basic gold plating solution and gold plating was performed under the same plating conditions as in Example 1. The SEM photograph of is shown in FIGS. 5 (a) and 5 (b). Although the amount of incorporation is small, CNT is incorporated into the gold plating film.
上記基本金めっき液に、塩化ベンザルコニウムを２ｇ／ｌ、ＣＮＴを２ｇ／ｌ添加した金めっき液を調整し、実施例１と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図６（ａ）、（ｂ）に示す。取り込み量は少ないがＣＮＴが金めっき皮膜に取り込まれている。 A gold plating solution prepared by adding 2 g / l benzalkonium chloride and 2 g / l CNT to the above basic gold plating solution was prepared, and the surface of the gold plating film subjected to gold plating under the same plating conditions as in Example 1 was prepared. SEM photographs are shown in FIGS. 6 (a) and 6 (b). Although the amount of incorporation is small, CNT is incorporated into the gold plating film.
上記基本金めっき液に、ジアリルジメチルアンモニウムクロリド２０％を５ｇ／ｌ、ＣＮＴを２ｇ／ｌ添加した金めっき液を調整し、実施例１と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図７（ａ）、（ｂ）に示す。取り込み量は少ないがＣＮＴが金めっき皮膜に取り込まれている。 A gold plating solution prepared by adding gold plating solution in which diallyldimethylammonium chloride 20% and 5 g / l CNT were added to the above basic gold plating solution and gold plating was performed under the same plating conditions as in Example 1 was performed. The SEM photograph of the surface is shown in FIGS. 7 (a) and 7 (b). Although the amount of incorporation is small, CNT is incorporated into the gold plating film.
上記基本金めっき液に、ポリオキシエチレン(2)ノニルフェニルエーテルを２ｇ／ｌ、ＣＮＴを２ｇ／ｌ添加した金めっき液を調整し、実施例１と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図８（ａ）、（ｂ）に示す。取り込み量は少ないがＣＮＴが金めっき皮膜に取り込まれている。 A gold plating solution prepared by adding 2 g / l of polyoxyethylene (2) nonylphenyl ether and 2 g / l of CNT to the above basic gold plating solution was prepared, and gold was plated under the same plating conditions as in Example 1. SEM photographs of the surface of the plating film are shown in FIGS. Although the amount of incorporation is small, CNT is incorporated into the gold plating film.
上記基本金めっき液に、ポリアクリル酸（ＰＡ）５０００（分子量）を０．５ｇ／ｌ、ＣＮＴを２ｇ／ｌ添加した金めっき液を調整し、実施例１と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図９（ａ）、（ｂ）に示す。取り込み量は少ないがＣＮＴが金めっき皮膜に取り込まれている。 A gold plating solution prepared by adding 0.5 g / l of polyacrylic acid (PA) 5000 (molecular weight) and 2 g / l of CNT to the above basic gold plating solution is prepared, and gold plating is performed under the same plating conditions as in Example 1. 9A and 9B show SEM photographs of the surface of the gold plating film performed. Although the amount of incorporation is small, CNT is incorporated into the gold plating film.
上記基本金めっき液に、ポリオキシエチレン(23)ラウリルエーテルを２ｇ／ｌ、ＣＮＴを２ｇ／ｌ添加した金めっき液を調整し、実施例１と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図１０（ａ）、（ｂ）に示す。取り込み量は少ないがＣＮＴが金めっき皮膜に取り込まれている。 A gold plating solution prepared by adding a gold plating solution prepared by adding 2 g / l polyoxyethylene (23) lauryl ether and 2 g / l CNT to the above basic gold plating solution, and performing gold plating under the same plating conditions as in Example 1 SEM photographs of the film surface are shown in FIGS. 10 (a) and 10 (b). Although the amount of incorporation is small, CNT is incorporated into the gold plating film.
上記基本金めっき液に、ポリエチレングリコール２０００を２ｇ／ｌ、ＣＮＴを２ｇ／ｌ添加した金めっき液を調整し、実施例１と同一のめっき条件で金めっきを行った金めっき膜の表面のＳＥＭ写真を図１１（ａ）、（ｂ）に示す。取り込み量は少ないがＣＮＴが金めっき皮膜に取り込まれている。 A gold plating solution prepared by adding 2 g / l of polyethylene glycol 2000 and 2 g / l of CNT to the above basic gold plating solution was prepared, and an SEM of the surface of the gold plating film subjected to gold plating under the same plating conditions as in Example 1 Pictures are shown in FIGS. 11 (a) and 11 (b). Although the amount of incorporation is small, CNT is incorporated into the gold plating film.
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| CN105420771A (en) * | 2015-12-23 | 2016-03-23 | 苏州市金星工艺镀饰有限公司 | Environment-friendly cyanide-free gilding electroplating liquid |
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| JP4934765B2 (en) * | 2005-12-28 | 2012-05-16 | 国立大学法人信州大学 | Gold plating film and manufacturing method thereof |
| JP5066743B2 (en) * | 2008-01-29 | 2012-11-07 | 三菱電機株式会社 | Plating method and plated product provided with plating film produced by the method |
| JP2015014019A (en) * | 2013-07-03 | 2015-01-22 | パナソニック株式会社 | Surface treatment method of electrical contact, electrical contact member, connector and contact treatment agent |
| JP6664200B2 (en) * | 2015-11-25 | 2020-03-13 | 日本ゼオン株式会社 | Manufacturing method of composite material |
| JP2019002034A (en) * | 2017-06-13 | 2019-01-10 | 国立大学法人信州大学 | Copper/monolayer carbon nanotube composite plating method |
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| JP2006249484A (en) | 2006-09-21 |
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