JPH11207184A - Palladium mixed catalyst and method for providing palladium catalyst utilizing same - Google Patents
Palladium mixed catalyst and method for providing palladium catalyst utilizing sameInfo
- Publication number
- JPH11207184A JPH11207184A JP10027887A JP2788798A JPH11207184A JP H11207184 A JPH11207184 A JP H11207184A JP 10027887 A JP10027887 A JP 10027887A JP 2788798 A JP2788798 A JP 2788798A JP H11207184 A JPH11207184 A JP H11207184A
- Authority
- JP
- Japan
- Prior art keywords
- water
- soluble
- salt
- palladium
- stannous
- 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
- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 14
- 150000002940 palladium Chemical class 0.000 claims abstract description 13
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000003093 cationic surfactant Substances 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 abstract description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 abstract description 3
- 239000001103 potassium chloride Substances 0.000 abstract description 3
- 235000011164 potassium chloride Nutrition 0.000 abstract description 3
- 239000001119 stannous chloride Substances 0.000 abstract description 3
- 235000011150 stannous chloride Nutrition 0.000 abstract description 3
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 abstract description 2
- 235000011118 potassium hydroxide Nutrition 0.000 abstract description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 abstract description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 abstract description 2
- 235000011151 potassium sulphates Nutrition 0.000 abstract description 2
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 abstract description 2
- 229910000375 tin(II) sulfate Inorganic materials 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 abstract 1
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical compound [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 12
- 238000007747 plating Methods 0.000 description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 10
- 238000007772 electroless plating Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000003365 glass fiber Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- -1 and the like Substances 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000003750 conditioning effect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920002006 poly(N-vinylimidazole) polymer Polymers 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000009719 polyimide resin Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 101150003085 Pdcl gene Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- RFLFDJSIZCCYIP-UHFFFAOYSA-L palladium(2+);sulfate Chemical compound [Pd+2].[O-]S([O-])(=O)=O RFLFDJSIZCCYIP-UHFFFAOYSA-L 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、触媒核となるパラ
ジウムを析出させるための混合触媒に関し、更に詳細に
は、プリント回路基板のスルーホールやビアホール等の
微小径孔の内部や、ガラス、テフロン（登録商標）樹
脂、ＰＰＥ樹脂、ＢＴ樹脂等の触媒化が困難とされる場
所、材料等に対してもパラジウムを十分に析出させるこ
とのできる混合触媒およびこれを利用した触媒付与方法
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a mixed catalyst for precipitating palladium serving as a catalyst nucleus, and more particularly, to the inside of minute holes such as through holes and via holes in a printed circuit board, glass, and Teflon. The present invention relates to a mixed catalyst capable of sufficiently depositing palladium even in places and materials where it is difficult to catalyze (registered trademark) resin, PPE resin, BT resin, and the like, and a catalyst applying method using the mixed catalyst.
【０００２】[0002]
【従来の技術】プリント回路基板や各種電子部品の調製
においては、非電導性基材上、例えばガラスエポキシ樹
脂、紙フェノール樹脂、ポリイミド樹脂等や、セラミッ
クス等の上に銅（Ｃｕ）、ニッケル（Ｎｉ）、金（Ａ
ｕ）等の無電解めっきを施すことが多い。2. Description of the Related Art In the preparation of printed circuit boards and various electronic components, copper (Cu), nickel (Ni) (Cu), and the like are used on non-conductive substrates such as glass epoxy resin, paper phenol resin, polyimide resin, and ceramics. Ni), gold (A)
In many cases, electroless plating such as u) is performed.
【０００３】このような非電導性基材上に無電解めっき
を行う場合、無電解めっきすべき部分にパラジウム（Ｐ
ｄ）を析出させ、これを核として無電解めっきの析出を
開始させることが一般的である。 このようなＰｄを析
出させる方法として広く採用されている方法は、水溶性
塩である塩化パラジウム（ＰｄＣｌ2）と同じく水溶性
塩である塩化第一スズ（ＳｎＣｌ2）を混合した触媒液
（以下、「混合触媒」という）に非電導性基材を浸漬
し、第一スズイオンの還元力により、ＰｄイオンをＰｄ
金属として表面上に析出させるというものである。When electroless plating is performed on such a nonconductive substrate, palladium (P
It is common to deposit d) and use this as a nucleus to initiate the deposition of electroless plating. Such methods widely employed as a method of precipitating Pd, the catalyst solution prepared by mixing palladium chloride is a water-soluble salt stannous chloride is (PdCl 2) Like water-soluble salts (SnCl 2) (hereinafter , A "mixed catalyst") is immersed in a non-conductive substrate, and Pd ions are converted to Pd by the reducing power of stannous ions.
It is deposited on the surface as a metal.
【０００４】上記した手段で、多くの非電導性基材にＰ
ｄを析出させることができるが、Ｐｄが析出しにくい場
合も報告されつつある。 例えば、プリント回路基板に
設けられる、スルーホールやビアホールと呼ばれる微小
径孔の内部では、Ｐｄの析出が起きにくいことが知られ
ており、その解決が求められている。また、ガラスや、
テフロン樹脂、ＰＰＥ樹脂、ＢＴ樹脂等はエッチングさ
れにくく、Ｐｄが析出しにくいことが知られている。[0004] By the means described above, many non-conductive substrates are treated with P
Although d can be precipitated, it has been reported that Pd is difficult to precipitate. For example, it is known that Pd is unlikely to be deposited inside a small diameter hole called a through hole or a via hole provided in a printed circuit board, and a solution to the problem is required. Also, glass,
It is known that Teflon resin, PPE resin, BT resin and the like are hardly etched and Pd is hardly precipitated.
【０００５】このようなＰｄが析出しにくい部分あるい
は材料について、Ｐｄの析出を向上させる手段として、
コンデショナーを用いる方法が報告されている（特公昭
５９−５２７０１号、特開平４−２６７７０号、特開平
４−２６７７１号、特開平５−３２０９２３号等）。
このコンデショナーは基本的にはカチオン性界面活性
剤、例えば四級アンモニウム塩等を用いるものであり、
実際Ｐｄの析出は向上する。 しかしながら、コンデシ
ョナーを用いる方法では、また別の問題が生じる。すな
わち、後の無電解めっき工程により析出した金属被膜
と、未析出部や基材との間の密着性が低下し、場合によ
っては剥離するなどの現象が現れていた。また、早く析
出する部分と、そうでない部分の間にムラが生じるな
ど、均一性に欠けることもあった。[0005] As a means for improving the deposition of Pd in such a portion or material where Pd is unlikely to be deposited,
Methods using a conditioner have been reported (JP-B-59-52701, JP-A-4-26770, JP-A-4-26771, JP-A-5-320923, etc.).
This conditioner basically uses a cationic surfactant, such as a quaternary ammonium salt.
In fact, the precipitation of Pd is improved. However, another problem arises in the method using the conditioner. That is, the adhesion between the metal film deposited in the subsequent electroless plating step and the undeposited portion or the base material is reduced, and in some cases, a phenomenon such as peeling has appeared. In addition, uniformity may be lacking, for example, unevenness may occur between a portion that precipitates early and a portion that does not.
【０００６】[0006]
【発明が解決しようとする課題】従って、従来のコンデ
ショナーを用いた場合の欠点を解消し、十分なＰｄを析
出させる方法の開発が求められていた。Accordingly, there has been a need to develop a method of eliminating the drawbacks of using a conventional conditioner and of depositing sufficient Pd.
【０００７】[0007]
【課題を解決するための手段】本発明者らは、Ｐｄを均
一に析出させるべく、種々検討を行った結果、混合触媒
中にカリウムイオンを存在させることにより、安定にＰ
ｄが析出し、均一で連続的な触媒核皮膜が得られること
を見出し、本発明を完成した。Means for Solving the Problems The inventors of the present invention have conducted various studies in order to uniformly deposit Pd. As a result, the presence of potassium ions in the mixed catalyst allows the stable stabilization of Pd.
d was deposited, and it was found that a uniform and continuous catalyst core film was obtained, and the present invention was completed.
【０００８】すなわち、本発明は、水溶性パラジウム
塩、水溶性第一スズ塩および水溶性カリウム塩を含有す
る混合触媒液を提供するものである。また、本発明の別
の目的は、非電導性基材をカチオン性界面活性剤を含有
するコンデショナー液に浸漬し、次いでこれを上記混合
触媒液で処理することを特徴とするパラジウム触媒付与
方法を提供するものである。[0008] That is, the present invention provides a mixed catalyst solution containing a water-soluble palladium salt, a water-soluble stannous salt and a water-soluble potassium salt. Another object of the present invention is to provide a method for applying a palladium catalyst, which comprises immersing a non-conductive substrate in a conditioner solution containing a cationic surfactant, and then treating this with the mixed catalyst solution. To provide.
【０００９】[0009]
【発明の好ましい実施形態】本発明の混合触媒は、従来
から広く使用されている水溶性パラジウム塩と水溶性第
一スズ塩に、水溶性のカリウム塩を加えることにより調
製される。DETAILED DESCRIPTION OF THE INVENTION The mixed catalyst of the present invention is prepared by adding a water-soluble potassium salt to a water-soluble palladium salt and a water-soluble stannous salt which have been widely used in the past.
【００１０】水溶性パラジウム塩としては、水溶液中で
容易に解離し、パラジウムイオンを放出しうるものが好
ましく、例えば、塩化パラジウム（ＰｄＣｌ2）、硫酸
パラジウム（ＰｄＳＯ4）等が挙げられる。 また、第一
スズ塩としても水溶液中で容易に解離し、第一スズイオ
ンとなるもの、例えば塩化第一スズ、硫酸第一スズ等が
利用できる。As the water-soluble palladium salt, those which can be easily dissociated in an aqueous solution and release palladium ions are preferable, and examples thereof include palladium chloride (PdCl 2 ) and palladium sulfate (PdSO 4 ). Also, as stannous salts, those which readily dissociate in an aqueous solution and become stannous ions, for example, stannous chloride, stannous sulfate and the like can be used.
【００１１】一方、水溶性カリウム塩としては、塩化カ
リウム、硫酸カリウム、水酸化カリウム等が利用でき
る。On the other hand, as the water-soluble potassium salt, potassium chloride, potassium sulfate, potassium hydroxide and the like can be used.
【００１２】本発明の混合触媒における水溶性パラジウ
ム塩と水溶性第一スズ塩の濃度は、従来と同様としても
良いが、より触媒活性を挙げるためには水溶性パラジウ
ム塩の配合量を増やすことが好ましい。 この場合の配
合量はそれぞれ、０.０１〜１０ｍｍｏｌ／ｌ、０.５〜
５００ｍｍｏｌ／ｌ程度で、それらの配合比率は、例え
ば、モル比で１：１〜１：１００程度とすることが望ま
しい。 このように水溶性第一スズ濃度を低下させるこ
とにより触媒活性が高くなるのは、析出物中のＰｄの純
度が高くなるためと解される。[0012] The concentrations of the water-soluble palladium salt and the water-soluble stannous salt in the mixed catalyst of the present invention may be the same as those in the prior art. Is preferred. In this case, the compounding amounts are 0.01 to 10 mmol / l and 0.5 to 10 mmol / l, respectively.
It is desirable that the mixing ratio is, for example, about 1: 1 to 1: 100 in a molar ratio of about 500 mmol / l. It is understood that the reason why the catalytic activity is increased by reducing the concentration of the water-soluble stannous is that the purity of Pd in the precipitate is increased.
【００１３】また、本発明の混合触媒における水溶性カ
リウム塩の濃度は、１０ｍｍｏｌ以上溶解可能な量（４
０００ｍｍｏｌ）の範囲であり、水溶性パラジウム塩と
水溶性第一スズ塩の合計に対して、モル比で１：１〜１
００：１程度とすることが好ましい。[0013] The concentration of the water-soluble potassium salt in the mixed catalyst of the present invention is 10 mmol or more that can be dissolved (4
000 mmol) in a molar ratio of 1: 1 to 1 with respect to the total of the water-soluble palladium salt and the water-soluble stannous salt.
The ratio is preferably set to about 00: 1.
【００１４】本発明の触媒液は、直接使用できるタイプ
とすることもできるが、用時に希釈する濃縮タイプのも
のとすることも可能である。後者の場合の各成分の配合
割合は、希釈した場合に上記濃度となるようにすること
が好ましい。The catalyst solution of the present invention may be of a type which can be used directly, or may be of a concentrated type which is diluted at the time of use. In the latter case, it is preferable that the mixing ratio of each component is adjusted to the above concentration when diluted.
【００１５】かくして得られる本発明の混合触媒は、従
来のＰｄ／Ｓｎ混合触媒と同様に使用できるが、特にい
わゆるコンデショニング処理した後に使用することによ
りより優れた触媒付与効果を与えることができる。The mixed catalyst of the present invention thus obtained can be used in the same manner as a conventional mixed catalyst of Pd / Sn. Particularly, when used after so-called conditioning treatment, a more excellent effect of providing a catalyst can be provided.
【００１６】すなわち、セラミックスやガラス等の無機
基材や、ガラスエポキシ樹脂、紙フェノール樹脂、ポリ
イミド樹脂テフロン樹脂、ＰＰＥ樹脂、ＢＴ樹脂等の高
分子基材等の非電導性基材を、常法に従ってアルカリ脱
脂、次いでカチオン性界面活性剤を有効成分として含む
コンデショナー液に浸漬し、更に予備浸漬液に浸漬した
後、本発明の混合触媒液で処理することにより、パラジ
ウムによる優れた触媒活性が得られる。That is, non-conductive base materials such as inorganic base materials such as ceramics and glass, and polymer base materials such as glass epoxy resin, paper phenol resin, polyimide resin Teflon resin, PPE resin, BT resin, etc. Excellent catalysis by palladium is obtained by immersing in a conditioner solution containing a cationic surfactant as an active ingredient, followed by immersion in a preliminary immersion solution, followed by treatment with the mixed catalyst solution of the present invention. Can be
【００１７】上記方法において用いられるコンデショナ
ー液の例としては、有効成分として、ポリビニルイミダ
ゾール、アルキルアンモニウムクロライド等を利用した
ものが挙げられ、また、予備浸漬液としては、濃塩酸、
塩化ナトリウム等の水溶液が挙げられる。Examples of the conditioner liquid used in the above method include those using polyvinyl imidazole, alkylammonium chloride or the like as an active ingredient, and concentrated hydrochloric acid,
An aqueous solution such as sodium chloride is given.
【００１８】上記のようにして触媒化した後、促進処理
液に浸漬し、無電解めっきを行うことにより、良好な無
電解めっき皮膜が得られる。 促進処理液としては、硫
酸、ホウフッ化水素酸等の水溶液を利用することができ
る。After catalyzing as described above, a good electroless plating film can be obtained by immersing in an accelerating treatment solution and performing electroless plating. As the accelerated treatment liquid, an aqueous solution of sulfuric acid, borofluoric acid, or the like can be used.
【００１９】また無電解めっきとしては、目的に応じて
無電解銅めっき、無電解ニッケルめっき、無電解金めっ
き等を採用することができ、その工程も一般的な方法、
条件で実施できる。As the electroless plating, electroless copper plating, electroless nickel plating, electroless gold plating, or the like can be adopted according to the purpose.
It can be implemented under conditions.
【００２０】以上の本発明方法において採用される各工
程の好ましい条件をまとめて示せば次の通りである。The preferred conditions of each step employed in the above method of the present invention are summarized below.
【００２１】 工 程 温 度 浸漬時間 備 考 アルカリ脱脂 ５０〜７０℃ ２〜１０分 コンデショニング ２０〜６０℃ １〜５分 予備浸漬 ２０〜３０℃ １〜５分 後水洗なし 触媒付与 ２０〜６０℃ ２〜１０分 促進処理 ２０〜６０℃ ２〜１０分Process Temperature Immersion time Remarks Alkaline degreasing 50 to 70 ° C 2 to 10 minutes Conditioning 20 to 60 ° C 1 to 5 minutes Pre-soaking 20 to 30 ° C 1 to 5 minutes No post-washing Catalyst applied 20 to 60 ° C 2 to 10 minutes Acceleration treatment 20 to 60 ° C 2 to 10 minutes
【００２２】以上説明した本発明の混合触媒を利用して
触媒化することにより、通常の非電導性基材上はもとよ
り、一般に無電解めっきを析出させることが困難とされ
ている微小径孔の内部や、エッチングされにくい材質上
にも良好に無電解めっきを行うことができる。By catalyzing using the mixed catalyst of the present invention described above, not only the usual non-conductive substrate but also the fine pores which are generally difficult to deposit electroless plating are considered. Electroless plating can be satisfactorily performed on the inside or on a material that is not easily etched.
【００２３】[0023]
【実施例】次に実施例を挙げ、本発明を更に詳しく説明
するが、本発明はこれら実施例等になんら制約されるも
のではない。EXAMPLES Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
【００２４】実 施 例 １ 直径５μｍのガラス繊維を試料とし、これを表１の工程
で前処理した後、表２に示す組成の触媒液を用いて触媒
付与した。 この触媒液での触媒付与は、浴温２５℃、
浸漬時間５分の条件でおこなった。 触媒付与処理後、
５０ｍｌ／ｌの濃硫酸液を用いて２５℃で５分間促進処
理を行い、更に下記条件で無電解銅めっきを施し、無電
解銅めっきの析出状態を走査型電子顕微鏡（ＳＥＭ）で
調べた。この結果、均一なフィルム状の無電解銅めっき
被膜が析出したことが認められた。Example 1 A glass fiber having a diameter of 5 μm was used as a sample, pretreated in the steps shown in Table 1, and then catalyzed using a catalyst solution having the composition shown in Table 2. The catalyst is applied with this catalyst solution at a bath temperature of 25 ° C.
The immersion time was 5 minutes. After the catalyst application treatment,
Acceleration treatment was performed at 25 ° C. for 5 minutes using a 50 ml / l concentrated sulfuric acid solution, and further, electroless copper plating was performed under the following conditions, and the deposition state of the electroless copper plating was examined by a scanning electron microscope (SEM). As a result, it was confirmed that a uniform film-like electroless copper plating film was deposited.
【００２５】前処理工程：Pretreatment step:
【表１】 * ＯＰ−１４４（荏原ユージライト(株)製） ３０ｇ
／ｌ ** ポリビニルイミダゾール ２ｇ／ｌ + 濃塩酸 ３００ｍｌ／ｌ[Table 1] * OP-144 (manufactured by EBARA Eugelight Co., Ltd.) 30 g
/ L ** polyvinyl imidazole 2g / l + concentrated hydrochloric acid 300ml / l
【００２６】混 合 触 媒 液：Mixing catalyst solution:
【表２】 [Table 2]
【００２７】無電解銅めっき： （ 使 用 浴 ）Electroless copper plating: (use bath)
【表３】 [Table 3]
【００２８】（ 作 業 条 件 ） ｐＨ １２.９ 温度 ２５℃ 浸漬時間 １０分(Working conditions) pH 12.9 Temperature 25 ° C Immersion time 10 minutes
【００２９】実 施 例 ２ 混合触媒液の組成を表４に示すものに代える以外は実施
例１と同様にしてガラス繊維上に無電解銅めっきを行っ
た。この結果、実施例１と同様の均一なフィルム状の無
電解銅めっき被膜が得られた。Example 2 Electroless copper plating was performed on glass fibers in the same manner as in Example 1 except that the composition of the mixed catalyst solution was changed to that shown in Table 4. As a result, a uniform film-like electroless copper plating film as in Example 1 was obtained.
【００３０】混 合 触 媒 液 ：[0030] Mixed catalyst solution:
【表４】 [Table 4]
【００３１】比 較 例 実施例１の混合触媒液組成中の塩化カリウムを、同モル
（３.５モル）となる濃度の塩化ナトリウムよび塩化リ
チウムに代える以外は実施例１と同様にしてガラス繊維
上に無電解銅めっきを行った。この結果、共に無電解銅
めっき被膜が完全にガラス繊維上につき回らず、不十分
なものであった。Comparative Example Glass fiber was prepared in the same manner as in Example 1 except that potassium chloride in the mixed catalyst liquid composition of Example 1 was replaced with sodium chloride and lithium chloride at the same molar concentration (3.5 mol). Electroless copper plating was performed thereon. As a result, in both cases, the electroless copper plating film did not completely cover the glass fiber and was insufficient.
【００３２】上記の結果より明らかなように、水溶性カ
リウム塩を利用する本発明の混合触媒は、従来触媒化が
困難とされてきた素材に対しても触媒付与することが可
能となるものであり、これにより電子回路等の基板とし
て利用する素材の範囲を拡張することができる。 以 上As is clear from the above results, the mixed catalyst of the present invention using a water-soluble potassium salt can provide a catalyst even to a material which has been conventionally difficult to catalyze. Yes, this makes it possible to expand the range of materials used as substrates for electronic circuits and the like. that's all
Claims (5)
および水溶性カリウム塩を含有する混合触媒。1. A mixed catalyst comprising a water-soluble palladium salt, a water-soluble stannous salt and a water-soluble potassium salt.
を、モル比で１：１〜１：１００の割合で含有する請求
項第１項記載の混合触媒。2. The mixed catalyst according to claim 1, wherein the water-soluble palladium salt and the water-soluble stannous salt are contained in a molar ratio of 1: 1 to 1: 100.
ム塩と水溶性第一スズ塩の合計量に対し、モル比で１：
１〜１００：１の割合で含有する請求項第１項または第
２項記載の混合触媒。3. The molar ratio of the water-soluble potassium salt to the water-soluble palladium salt and the water-soluble stannous salt is 1: 1:
3. The mixed catalyst according to claim 1, wherein the mixed catalyst is contained in a ratio of 1 to 100: 1.
第３項の何れかの項記載の混合触媒。4. The mixed catalyst according to claim 1, further comprising hydrochloric acid.
含有するコンデショナー液に浸漬し、次いでこれを水溶
性パラジウム塩、水溶性第一スズ塩および水溶性カリウ
ム塩を含有する混合触媒の水溶液で処理することを特徴
とするパラジウム触媒付与方法。5. A non-conductive substrate is immersed in a conditioner solution containing a cationic surfactant, and then immersed in a mixed catalyst containing a water-soluble palladium salt, a water-soluble stannous salt and a water-soluble potassium salt. A method for applying a palladium catalyst, comprising treating with an aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10027887A JPH11207184A (en) | 1998-01-27 | 1998-01-27 | Palladium mixed catalyst and method for providing palladium catalyst utilizing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10027887A JPH11207184A (en) | 1998-01-27 | 1998-01-27 | Palladium mixed catalyst and method for providing palladium catalyst utilizing same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11207184A true JPH11207184A (en) | 1999-08-03 |
Family
ID=12233413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10027887A Pending JPH11207184A (en) | 1998-01-27 | 1998-01-27 | Palladium mixed catalyst and method for providing palladium catalyst utilizing same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11207184A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007138218A (en) * | 2005-11-16 | 2007-06-07 | Hitachi Chem Co Ltd | Liquid catalyst concentrate for electroless plating, and plating catalyst providing method using the same |
| JP2007302985A (en) * | 2006-05-15 | 2007-11-22 | Shinko Electric Ind Co Ltd | Electroless plating method and electroless plating pretreatment agent |
-
1998
- 1998-01-27 JP JP10027887A patent/JPH11207184A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007138218A (en) * | 2005-11-16 | 2007-06-07 | Hitachi Chem Co Ltd | Liquid catalyst concentrate for electroless plating, and plating catalyst providing method using the same |
| JP2007302985A (en) * | 2006-05-15 | 2007-11-22 | Shinko Electric Ind Co Ltd | Electroless plating method and electroless plating pretreatment agent |
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