JP2014180666A - 無電解金属化用の安定触媒 - Google Patents
無電解金属化用の安定触媒 Download PDFInfo
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- JP2014180666A JP2014180666A JP2014051891A JP2014051891A JP2014180666A JP 2014180666 A JP2014180666 A JP 2014180666A JP 2014051891 A JP2014051891 A JP 2014051891A JP 2014051891 A JP2014051891 A JP 2014051891A JP 2014180666 A JP2014180666 A JP 2014180666A
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- Prior art keywords
- catalyst
- copper
- solution
- metal
- ring
- Prior art date
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- Granted
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- 238000001465 metallisation Methods 0.000 title description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 57
- 239000002184 metal Substances 0.000 claims abstract description 57
- 239000000758 substrate Substances 0.000 claims abstract description 51
- 229930182486 flavonoid glycoside Natural products 0.000 claims abstract description 24
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 16
- 229910000510 noble metal Inorganic materials 0.000 claims description 15
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- 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 7
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- VMDSWYDTKFSTQH-UHFFFAOYSA-N sodium;gold(1+);dicyanide Chemical compound [Na+].[Au+].N#[C-].N#[C-] VMDSWYDTKFSTQH-UHFFFAOYSA-N 0.000 description 1
- DTNJZLDXJJGKCM-UHFFFAOYSA-K sodium;trichlorogold Chemical compound [Na].Cl[Au](Cl)Cl DTNJZLDXJJGKCM-UHFFFAOYSA-K 0.000 description 1
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- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical compound [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
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- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
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- 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
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- 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
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- 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
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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Abstract
【解決手段】貴金属及びフラボノイド誘導体の安定化剤のナノ粒子の水性触媒が、非導電性基板に金属を無電解的にめっきするために使用される。そのような基板には、プリント回路板が含まれる。
【効果】触媒は、誘電材料の基板を含む基板に金属を無電解的にめっきするために使用することができ、従来のスズ/パラジウム触媒と比較して容易に酸化しないため、保管に際してだけでなく無電解めっき中も安定している。フラボノイドグリコシド安定化剤は、生分解性であるという点を除いて、従来のスズ/パラジウム触媒中の塩化第一スズと同様に機能し、したがって、塩化第一スズが廃棄の際にもたらすような環境的な危険をもたらさない。安定化剤を製作するために使用される原材料は、本質的にどこにでもある植物生命体から容易に入手可能である。
【選択図】なし
Description
190mgのナリンギン二水和物を、750mlのDI水を含有するビーカーに溶解した。水を50℃に加熱して、ナリンギン二水和物の溶解を支援した。25ml DI水中の290mg Na2PdCl4を、撹拌しながらナリンギン溶液に添加して、実質的に均一なオレンジ色の溶液を形成した。10ml DI水中の93mg NaBH4を、撹拌子で激しく撹拌しながら上記の実質的に均一な溶液に添加した。上記溶液は、色がオレンジ色から黒色に変化し、コロイド状パラジウムナノ粒子の形成を示した。パラジウム金属対ナリンギンのモル比は、1:0.3だった。その後、水性コロイド状ナリンギン及びパラジウムナノ粒子を含有するビーカーを、50℃水浴に12時間配置して、ナノ粒子の貯蔵寿命安定性を試験した。pHを、ACCUMET AB15 pH計で12時間にわたってモニタした。溶液中で過剰NaBH4からH2ガス及び水酸化物が形成されるため、pHは、7から9に変動した。12時間後、ビーカーの底には、観察可能な黒色沈殿物は存在しなかった。したがって、ナノ粒子は安定していた。
190mgのナリンギン二水和物を、750mlのDI水を含有するビーカーに溶解した。水を50℃に加熱して、ナリンギン二水和物の溶解を支援した。25ml DI水中の440mg Na2PdCl4を、撹拌しながらナリンギン溶液に添加して、実質的に均一なオレンジ色の溶液を形成した。10ml DI水中の140mg NaBH4を、撹拌子で激しく撹拌しながら上記実質的に均一な溶液に添加した。上記溶液は、色がオレンジ色から黒色に変化し、コロイド状パラジウムナノ粒子の形成を示した。パラジウム金属対ナリンギンのモル比は1:0.2であり、浴のpHは、8〜9であった。その後、水性コロイド状パラジウムナノ粒子を含有するビーカーを、50℃水浴に12時間配置して、ナノ粒子の安定性を試験した。ビーカーの底には、黒色沈殿物の観察可能な形成は存在しなかった。コロイド状ナノ粒子は、12時間にわたって安定していた。
実施例2で製作したナリンギン/パラジウムコロイド状ナノ粒子触媒の等容積の2つの試料分割量を、保存溶液から取り出し、各試料中のパラジウム濃度が50ppmになるようにDIで希釈した。一方の試料には、十分な量の2,4−ジヒドロキシ安息香酸を添加して、pHを3に調整し、他方の試料は、十分な量のグリオキシル酸を添加することにより、pHを3に調整した。
1.各積層体を、1:2の体積対容積比のエチレングリコールジメチルエーテル及び水を含んでいた膨潤溶媒に80℃で7分間浸漬した;
2.その後、各積層体を膨潤溶媒から取り出し、冷水道水で4分間すすいだ;
3.その後、各積層体を、80℃にて10分間、pH10超の1%過マンガン酸カリウムを含んでいた過マンガン酸塩水溶液で処理した;
4.その後、各積層体を、冷水道水で4分間すすいだ;
5.その後、積層体を、室温で2分間、3wt%過酸化物及び3wt%硫酸の中和剤溶液で処理した;
6.その後、各積層体を、冷水道水で4分間すすいだ;
7.その後、各積層体を、3%CIRCUPOSIT CONDITIONER(商標)231水性酸性調整剤を含有する水性浴に、40℃で5分間浸漬した;
8.その後、各積層体を、冷水道水で4分間すすいだ;
9.その後、MICROETCH(商標)748溶液を、室温で2分間、各積層体に適用した;
10.その後、各積層体を、冷水道水で4分間すすいだ;
11.その後、積層体を、室温で2分間、2g/Lグリオキシル酸及び1g/Lシュウ酸を含有するプリディップ酸性水溶液に浸漬した;
12.その後、積層体を、40℃で5分間、ナリンギン/パラジウム触媒の2つの試料のうちの1つで下塗りした;
13.その後、各積層体を、冷水で4分間すすいだ;
14. その後、積層体を、40℃及びpH13のCIRCUPOSIT880無電解銅めっき浴に浸漬し、銅を15分間基板に堆積させた;
15.その後、銅めっき積層体を、冷水で2分間すすいだ;
16.その後、上記銅めっき積層体のうちの6つを、従来型対流式オーブンに入れ、105℃で20分間乾燥させ、他の6つの積層体を、下述のICD性能用に電解銅でめっきした。
17.乾燥した後、第1のセットの6つの銅めっき積層体を、従来型実験室乾燥器に20分間又はそれらが室温に冷却するまで入れておいた;及び
18.その後、第1のセットの6つの銅めっき積層体を、従来のセロテープ試験法を使用して、接着性について試験した。
コロイド状ナノ粒子触媒中のパラジウム濃度を100ppmに増加させたことを除いて、上記の実施例3に記載のめっき法を繰り返した。試料は、安定していたと考えられ、沈殿物は観察可能ではなかった。めっきした銅積層体は全て、良好な形態を有する明るく輝く銅堆積を示し、セロテープ試験に合格した。銅積層体からテープを除去した後セロテープに貼り付いていた銅金属は、観察可能ではなかった。平均バックライト試験結果は、4.6以上4.9以下の範囲だった。ICDは、上記積層体のいずれでも観察されなかった。
1.2gのルチン三水和物を、800mlのDI水を含有するビーカーに添加した。1N NaOH溶液を撹拌しながら添加して、溶液pHを11.2に調整した。別のビーカーで、1.65gのp−トルエンスルホン酸銀を、40mlのDI水に溶解した。銀イオン溶液を、激しく撹拌しながらルチン三水和物溶液に添加した。上記2つの溶液を混合した1分後、数ミリリットルの溶液を取り出して、UV−vis測定用に希釈した。スペクトルは、Agilent社製UV−Vis分光光度計8453を使用して測定した。UV−Visスペクトルは、412nm付近に強い吸収ピークを示し、銀ナノ粒子の形成が示された。銀金属対ルチン三水和物のモル比は、1:0.3だった。触媒水溶液を含有するビーカーを、50℃の水浴に12時間配置して、その安定性を試験した。沈殿は観察されなかった。保存溶液から等容積の10分割量を取り出すことにより、銀ナノ粒子溶液を無電解銅めっき用触媒として試験した。その後、各分割量をDI水で320ppm銀に希釈し、アスコルビン酸又はジヒドロキシ安息香酸でpH3〜6に調整した。複数のスルーホールを有する10個の積層体を準備した:SY−1141、SY−1000−2、TUC−752、370HR(Isola社)、及びNP−175(Nanya社)。上記触媒は、積層体の全てで無電解めっきを開始させた。積層体は全て、外観が明るく輝き滑らかだった。上記積層体のうちの5つを、接着性について試験した。全てが、セロテープ試験に合格した。バックライト性能を、上記5つの積層体について試験した。平均値は、4.5〜4.8であった。これは、一般的に工業規格により受け入れられるものである。残りの5つの積層体を、実施例3に記載のようにICDについて分析した。上記5つの積層体では、ICDは検出されなかった。
ロビニン/銀コロイド状ナノ粒子触媒を、800mlのDI水を含有するビーカーに1.07gロビニンを室温にて溶解することにより調製する。1N NaOH溶液を撹拌しながら添加して、溶液pHを11に調整する。別のビーカーで、1.42gのp−トルエンスルホン酸銀を、40mlのDI水に溶解する。銀イオン溶液を、激しく撹拌しながらロビニン溶液に添加する。銀金属対ロビニンのモル比は、1:0.28である。触媒水溶液を含有するビーカーを、50℃の水浴に12時間配置して、その安定性を試験する。12時間後、上記溶液を観察する。沈殿物は予想されず、上記触媒が依然として安定していることが示される。
ヘスペリジン/銀コロイド状ナノ粒子触媒を、800mlのDI水を含有するビーカーに1.65gのヘスペリジンを室温にて溶解することにより調製する。1N NaOH溶液を撹拌しながら添加して、溶液pHを11に調整する。別のビーカーで、2.2gのp−トルエンスルホン酸銀を、60mlのDI水に溶解する。銀イオン溶液を、激しく撹拌しながらヘスペリジン溶液に添加する。銀対ヘスペリジンのモル比は、1:0.34である。触媒水溶液を含有するビーカーを、50℃の水浴に12時間配置して、その安定性を試験する。12時間後、上記溶液を観察する。沈殿物は予想されず、上記触媒が依然として安定していることが示される。
ジオスミン/パラジウムコロイド状ナノ粒子触媒を、500mlのDI水を含有するビーカーに195mgのジオスミンを室温にて溶解することにより調製する。撹拌しながら、30ml DI水中の300mg Na2PdCl4を添加し、空気撹拌を使用して、混合物を激しく撹拌する。その後、10ml DI水中の100mg NaBH4を、激しく空気撹拌しながら上記溶液に添加する。上記溶液は黒色になり、パラジウムイオンがパラジウム金属に還元され、パラジウムナノ粒子の形成が示される。パラジウム対ジオスミンのモル比は、1:0.3である。上記触媒の溶液は、ACCUMET AB15 pH計を使用して測定すると、8以上9以下のpHを有する。上記触媒水溶液を含有するビーカーを、50℃の水浴に12時間配置して、その安定性を試験する。12時間後、上記溶液を観察する。沈殿物は予想されず、上記触媒が依然として安定していることが示される。
750mlのDI水を含有するビーカーに195mgのクエルシトリン(qiercitrin)を室温にて溶解することにより、クエルシトリン/パラジウムコロイド状ナノ粒子触媒を調製する。撹拌しながら、30ml DI水中の300mg Na2PdCl4を添加し、空気撹拌を使用して、混合物を激しく撹拌する。その後、15ml DI水中の100mg NaBH4を、激しく空気撹拌しながら上記溶液に添加する。上記溶液は黒色になり、パラジウムイオンがパラジウム金属に還元され、パラジウムナノ粒子の形成が示される。上記触媒の溶液は、ACCUMET AB15 pH計を使用して測定すると、7〜8のpHを有する。パラジウム対クエルシトリンのモル比は、1:0.4である。触媒水溶液を含有するビーカーを、50℃の水浴に12時間配置して、その安定性を試験する。12時間後、上記溶液を観察する。沈殿物は予想されず、上記触媒が依然として安定していることが示される。
750mlのDI水を含有するビーカーに1.04gのミリセチン3−ラムノシドを室温にて溶解することにより、ミリセチン3−ラムノシド/銀コロイド状ナノ粒子触媒を調製する。撹拌しながら、1N NaOH溶液を添加して、溶液pHを11に調整する。別のビーカーで、1.4gのp−トルエンスルホン酸銀を、40mlのDI水に溶解する。銀イオン溶液を、激しく撹拌しながらミリセチン3−ラムノシド溶液に添加する。銀対ミリセチン3−ラムノシドのモル比は、1:0.4である。触媒水溶液を含有するビーカーを、50℃の水浴に12時間配置して、その安定性を試験する。12時間後、上記溶液を観察する。沈殿物は予想されず、上記触媒が依然として安定していることが示される。
Claims (7)
- 1つ又は複数の還元剤、並びに1つ又は複数の貴金属及び1つ又は複数のフラボノイドグリコシド及びその水和物を含むナノ粒子を含む触媒水溶液。
- 前記1つ又は複数のフラボノイドグリコシドが、一般式(I)を有する、請求項1に記載の触媒水溶液。
- 前記ナノ粒子が、1nm〜1000nmである、請求項1に記載の触媒水溶液。
- 前記1つ又は複数の貴金属対前記1つ又は複数のフラボノイドグリコシド及び水和物のモル比が、1:0.1以上1:5以下の範囲である、請求項1に記載の方法。
- a.基板を準備するステップ、
b.1つ又は複数の還元剤、並びに1つ又は複数の貴金属及び1つ又は複数のフラボノイドグリコシド及び水和物を含むナノ粒子を含む触媒水溶液を、前記基板に適用するステップ、
c.無電解金属めっき浴を使用して前記基板に金属を無電解的に堆積させるステップを含む方法。 - 前記基板が、複数のスルーホールを含む、請求項5に記載の方法。
- 前記無電解金属めっき浴が、銅、銅合金、ニッケル、及びニッケル合金浴から選択される、請求項5に記載の方法。
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KR20200128202A (ko) * | 2016-07-08 | 2020-11-11 | 이시하라 케미칼 가부시키가이샤 | 무전해 니켈 또는 니켈 합금 도금용 니켈 콜로이드 촉매액 및 무전해 니켈 또는 니켈 합금 도금방법 |
KR102341914B1 (ko) | 2016-07-08 | 2021-12-22 | 이시하라 케미칼 가부시키가이샤 | 무전해 니켈 또는 니켈 합금 도금용 니켈 콜로이드 촉매액 및 무전해 니켈 또는 니켈 합금 도금방법 |
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CN104043450A (zh) | 2014-09-17 |
CN109609932A (zh) | 2019-04-12 |
US9441300B2 (en) | 2016-09-13 |
US9597676B2 (en) | 2017-03-21 |
US20160332153A1 (en) | 2016-11-17 |
EP2777810A1 (en) | 2014-09-17 |
KR20140113550A (ko) | 2014-09-24 |
US20140272144A1 (en) | 2014-09-18 |
JP6370570B2 (ja) | 2018-08-08 |
TWI544108B (zh) | 2016-08-01 |
TW201441420A (zh) | 2014-11-01 |
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