JPWO2014188834A1 - メッキ膜の製造方法 - Google Patents
メッキ膜の製造方法 Download PDFInfo
- Publication number
- JPWO2014188834A1 JPWO2014188834A1 JP2015518163A JP2015518163A JPWO2014188834A1 JP WO2014188834 A1 JPWO2014188834 A1 JP WO2014188834A1 JP 2015518163 A JP2015518163 A JP 2015518163A JP 2015518163 A JP2015518163 A JP 2015518163A JP WO2014188834 A1 JPWO2014188834 A1 JP WO2014188834A1
- Authority
- JP
- Japan
- Prior art keywords
- plating
- acid
- plating film
- solvent
- organic solvent
- 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.)
- Granted
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
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- 239000002904 solvent Substances 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 21
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- 238000000034 method Methods 0.000 claims description 58
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- 239000011669 selenium Substances 0.000 claims description 15
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 11
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 229910052787 antimony Inorganic materials 0.000 claims description 9
- 229910052711 selenium Inorganic materials 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 7
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- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- YQUVCSBJEUQKSH-UHFFFAOYSA-N protochatechuic acid Natural products OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
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- 229910052716 thallium Inorganic materials 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- WXTMDXOMEHJXQO-UHFFFAOYSA-N 2,5-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC(O)=CC=C1O WXTMDXOMEHJXQO-UHFFFAOYSA-N 0.000 description 2
- WHBMMWSBFZVSSR-UHFFFAOYSA-N 3-hydroxybutyric acid Chemical compound CC(O)CC(O)=O WHBMMWSBFZVSSR-UHFFFAOYSA-N 0.000 description 2
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- 229910052726 zirconium Inorganic materials 0.000 description 1
- 150000003952 β-lactams Chemical class 0.000 description 1
- 150000003953 γ-lactams Chemical class 0.000 description 1
- 150000003954 δ-lactams Chemical class 0.000 description 1
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Abstract
Description
1.実施の形態
1−1.メッキ製品の構成
1−2.メッキ膜の製造方法
2.適用例
3.実施例
(1−1.メッキ製品の構成)
図1は、本開示の一実施の形態に係るメッキ製品の断面構成を模式的に表したものである。このメッキ製品10は、被メッキ物としての基体11の上にメッキ膜12が設けられたものであり、例えば熱を直接電気エネルギーに変換する熱電変換素子に用いることができる。メッキ膜12は例えば非水メッキ法により成膜される。
本実施の形態のメッキ膜12の製造方法としては、非水メッキを用いる電解メッキ法(以下、非水メッキ法という。)が好ましい。これは、主たるメッキ溶媒として有機溶剤を用いる手法であり、溶媒として水を用いるメッキ法(以下、水性メッキ法という。)よりも広範囲の種類金属を析出させることができる。これは、非水メッキ法では水またはプロトンに由来する水素ガスが発生しにくいので、酸化還元電位の著しく卑な金属(例えばアルカリ金属およびアルカリ土類金属)でも析出させることができるからである。さらに、非水メッキ法では、水に由来する酸素や溶存酸素の存在により水性メッキ法では析出させられないアルミニウム,チタン,タリウム,ニオブ,バナジウム等の酸素と親和性が高い金属も析出させることができる。また、非水メッキ法では、メッキ溶媒としてプロトン性が低い溶媒を選択することにより、気泡の発生によるメッキ面へのピンホール発生を抑えることができる。高電圧(例えば10V以上)を印加してもカソード電極における水素の発生が起こりにくいからである。さらに、非水メッキ法では、複数の有機溶剤を混合することによりメッキ溶媒の性質を制御することができる。これにより、メッキ膜の特性を制御するあたり、その自由度が向上する。
Bi(NO3)3・5H2O + K2TeO3 → 6K+ + 6NO3 - + Bi2(TeO3)3↓
この場合、使用する有機溶媒を変える、2種類以上の有機溶媒を混合する、あるいは水を添加する、などの方法のほか、上述したように高配位性の化合物(配位子)を配合して塩を溶解させる方法を取ることもできる。配位子としては上記した有機溶媒の中でも特に極性が大きなもののほか、高配位性の液体または個体の化合物で有機溶媒に溶解するもの、などを用いることができる。好適に用いられるものとしては、含窒素有機溶剤として挙げたエタノールアミン、ジエタノールアミン、トリエタノールアミンなどのほか、ヒドロキシ酸なども挙げることができる。
表記実施の形態において説明したメッキ膜12を設けたメッキ製品10は、先に述べたように、例えば熱電変換素子に用いることができる。
以下、本開示の実施例具体的に説明するが、本技術はこれらの実施例のみに限定されるものではない。
エチレングリコール(メッキ溶媒)100mlに硝酸ビスマス・五水和物1.9g、亜テルル酸カリウム1.0gを入れ、室温で撹拌した。白色沈殿が生じたところでトリエタノールアミン2.0gを加えて撹拌し、完全に溶解してメッキ液とした。このメッキ液を、アノード電極32(白金板、64mm×64mm)およびカソード電極33(銅板、64mm×64mm)を取り付けたガラス製の容器に入れ、室温において回転子で撹拌した。ここで、基体11としてのカソード電極33の上に直接、メッキを行う方法を取った。アノード電極32には非溶解性電極である白金板を用いた。印加する電圧は、図4の交流波形において、図4に示した各パラメータを表1に示した数値に設定した。実験例1−1〜1−3の条件下、それぞれ室温で30分間に亘って電圧を印加した結果、銀光沢を有するメッキ膜12を得た。
(1)
基体と、メッキ溶媒としての有機溶剤にBiおよびTeを溶解させたメッキ溶液とを用意することと、
前記メッキ溶液に浸漬された一対の電極間に電圧を印加することにより、前記基体上にメッキ膜を形成することと
を含む
メッキ膜の製造方法。
(2)
前記メッキ溶液として、SbおよびSeのうちの少なくとも一方を前記有機溶剤に溶解させたものを用いる
上記(1)記載のメッキ膜の製造方法。
(3)
前記メッキ溶液として、前記有機溶剤にBi(NO3 )3 ・5H2 OおよびK2 TeO3 を溶解させる
上記(1)または(2)に記載のメッキ膜の製造方法。
(4)
前記メッキ溶液として、前記有機溶剤に
KSb(OH)6 ,C8 H10 K2 O15 Sb2 ,K2 SeO3 ,およびK2 SeO4のうちの1種以上をさらに溶解させる
上記(1)から(3)のいずれか1に記載のメッキ膜の製造方法。
(5)
前記メッキ溶液に、水、エタノールアミン、ジエタノールアミン、トリエタノールアミン、ヒドロキシ酸、クラウンエーテルおよびエチレンジアミン四酢酸(EDTA)のうちの1種以上をさらに添加する
上記(1)から(4)のいずれか1に記載のメッキ膜の製造方法。
(6)
前記電圧として交流電圧を印加する
上記(1)から(5)のいずれか1に記載のメッキ膜の製造方法。
(7)
Cu,AgおよびAlからなる群から選択される1以上の元素を含む基体と、
前記基体上に設けられ、BiおよびTeを含むメッキ膜と
を有するメッキ製品。
(8)
前記メッキ膜は、SbおよびSeのうちの少なくとも一方を含む
上記(7)記載のメッキ製品。
Claims (8)
- 基体と、メッキ溶媒としての有機溶剤にBi(ビスマス)およびTe(テルル)を溶解させたメッキ溶液とを用意することと、
前記メッキ溶液に浸漬された一対の電極間に電圧を印加することにより、前記基体上にメッキ膜を形成することと
を含む
メッキ膜の製造方法。 - 前記メッキ溶液として、Sb(アンチモン)およびSe(セレン)のうちの少なくとも一方を前記有機溶剤に溶解させたものを用いる
請求項1記載のメッキ膜の製造方法。 - 前記メッキ溶液として、前記有機溶剤にBi(NO3 )3 ・5H2 OおよびK2 TeO3 を溶解させる
請求項1記載のメッキ膜の製造方法。 - 前記メッキ溶液として、前記有機溶剤にKSb(OH)6 ,C8 H10 K2 O15 Sb2 ,K2 SeO3 ,およびK2 SeO4のうちの1種以上をさらに溶解させる
請求項2記載のメッキ膜の製造方法。 - 前記メッキ溶液に、水、エタノールアミン、ジエタノールアミン、トリエタノールアミン、ヒドロキシ酸、クラウンエーテルおよびエチレンジアミン四酢酸(EDTA)のうちの1種以上をさらに添加する
請求項1記載のメッキ膜の製造方法。 - 前記電圧として交流電圧を印加する
請求項1記載のメッキ膜の製造方法。 - Cu,AgおよびAlからなる群から選択される1以上の元素を含む基体と、
前記基体上に設けられ、BiおよびTeを含むメッキ膜と
を有するメッキ製品。 - 前記メッキ膜は、SbおよびSeのうちの少なくとも一方を含む
請求項7記載のメッキ製品。
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