JP2009263759A - Alloy thin film formed from alloy of metal rhodium and metal rhenium by electrolytic technology - Google Patents
Alloy thin film formed from alloy of metal rhodium and metal rhenium by electrolytic technology Download PDFInfo
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- 239000010948 rhodium Substances 0.000 title claims abstract description 32
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 19
- 239000000956 alloy Substances 0.000 title claims abstract description 19
- 229910052703 rhodium Inorganic materials 0.000 title claims abstract description 19
- 239000010409 thin film Substances 0.000 title claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 title claims description 18
- 239000002184 metal Substances 0.000 title claims description 18
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 title claims description 9
- 229910052702 rhenium Inorganic materials 0.000 title claims description 7
- 229910001092 metal group alloy Inorganic materials 0.000 title 1
- 238000007747 plating Methods 0.000 claims abstract description 25
- 239000010408 film Substances 0.000 claims abstract description 15
- 229910000691 Re alloy Inorganic materials 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229910000629 Rh alloy Inorganic materials 0.000 claims 2
- 229910001369 Brass Inorganic materials 0.000 claims 1
- 229910000881 Cu alloy Inorganic materials 0.000 claims 1
- 230000004913 activation Effects 0.000 claims 1
- 239000010951 brass Substances 0.000 claims 1
- 230000007797 corrosion Effects 0.000 claims 1
- 238000005260 corrosion Methods 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 239000002344 surface layer Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 230000006866 deterioration Effects 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 235000014676 Phragmites communis Nutrition 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- YWFDDXXMOPZFFM-UHFFFAOYSA-H rhodium(3+);trisulfate Chemical compound [Rh+3].[Rh+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O YWFDDXXMOPZFFM-UHFFFAOYSA-H 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- WMFZVLIHQVUVGO-UHFFFAOYSA-N phenyl-(4-phenylphenyl)methanol Chemical compound C=1C=C(C=2C=CC=CC=2)C=CC=1C(O)C1=CC=CC=C1 WMFZVLIHQVUVGO-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003281 rhenium Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000008719 thickening 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
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- Electroplating Methods And Accessories (AREA)
Abstract
Description
本発明は、金属ロジュウムと、同じく金属レニュウムをイオン化した溶液を用いて、電解技術により、ロジュウム・レニュウムの二元合金の、０．１ミクロン〜１０．０ミクロンの厚みを有する薄膜を、提供する。 The present invention provides a thin film having a thickness of 0.1 μm to 10.0 μm of a binary alloy of rhodium and rhenium by electrolytic technique using a metal rhodium and a solution obtained by ionizing metal rhenium. .
パソコンを初めとし、家庭用電気機器、自動車のオートマチック機器等に、多数用いられているリード・スイッチの、接点部は、現在、激しいＯＮ−ＯＦＦの反復作動に、耐える為に，膜厚２．０〜５．０μのロジュウムめっきを施工し、ＯＮ＝ＯＦＦに際して生じる、電気スパークによる高温と機械的消耗に耐えている。 The contact point of the reed switch, which is widely used in personal electric appliances such as personal computers, automatic appliances for automobiles, etc., has a film thickness of 2. A 0 to 5.0 micron rhodium plating is applied to withstand high temperatures and mechanical wear caused by electric sparks that occur when ON = OFF.
近年では，同スイッチのＯＮ−ＯＦＦの反復回数・通電電流の容量が大きくなり、ロジュウム膜の耐摩耗性・耐スパーク性の改良が望まれている。 In recent years, the number of repetitions of ON / OFF of the switch and the capacity of energization current have increased, and improvement of the wear resistance and spark resistance of the rhodium film is desired.
その為に、現在では、ロジュウム被膜の上に，ルテニュウム、又はイリジュウムの、めっきを施工する手段が用いられているが、これ等のめっきが未だ完全とはいえず、また、コスト面でも、マイナス要因となっている。 For this reason, currently, means for applying a plating of ruthenium or iridium on the rhodium film is used, but these platings are not yet complete, and the cost is negative. It is a factor.
本発明は、上記の欠点を解除する為に、金属表面技術を用いて、ロジュウムＲｈ・レニュウムＲｅの合金めっき被膜を形成し、この分野の電気接点に対応する性能の改善を試みた。 In order to eliminate the above-mentioned drawbacks, the present invention attempted to improve the performance corresponding to the electric contacts in this field by forming an alloy plating film of rhodium Rh / Renium Re by using a metal surface technique.
また、本発明によるＲｈ−Ｒｅ合金被膜は、独特の青味を持った銀白色の色調を呈するので、その合金比率を、変動する事により、青銀白色から，青灰色と、色調の変動が出来、時計など装飾品の表面処理にも応用される。 In addition, the Rh—Re alloy coating according to the present invention exhibits a silver-white color tone with a unique bluish color. Therefore, by changing the alloy ratio, the color tone changes from blue-silver white to blue-gray. Can be applied to surface treatment of decorative items such as watches.
りーど・スイッチの接点部は、電流のＯＮ−ＯＦＦの作動時に、スパークを発生する為に、ピン・ポイントで、高温度になり、此れが連続反復を繰り返す為に、接点部表面の温度が上昇し、通常の接点部のように、銅又は、その合金に、金めっきを施工した程度では、忽ち、接点の表面が、スパークにより、飛散したり、溶解又は、酸化し、本来の機能の働きを、損ねてしまう。 The contact point of the relay switch becomes a high temperature at the pin point to generate a spark when the current is turned on and off, and the temperature of the surface of the contact part repeats repeatedly. As the normal contact part rises, the surface of the contact is scattered, melted or oxidized by sparks to the extent that gold or copper is applied to copper or its alloy, and the original function The work of will be impaired.
その為に、リード・スイッチの場合は、接点部を、ガラス管の中に封入して、ガラス管の中を、真空又は、不活性ガスを充満し、酸化防止を行っている。 Therefore, in the case of a reed switch, the contact portion is enclosed in a glass tube, and the glass tube is filled with a vacuum or an inert gas to prevent oxidation.
更に、ＯＮ−ＯＦＦによる、発熱による消耗を、防止する為に、融点の高い、金属を、接点部に被服する必要がある。 Furthermore, in order to prevent wear due to heat generation due to ON-OFF, it is necessary to coat the contact portion with a metal having a high melting point.
現在、リード・スイッチの接点部には、一般には、２〜５ミクロンのロジュウムめっきを施工している。用途によっては、その被膜の上に、更に、ルテニュウム或いは、イリジュウムのめっきを重ねて、その耐熱特性の向上を図っている。併し、この方法では、製作工程の、複雑さと、製品のコスト高が回避できない。 Currently, 2 to 5 micron rhodium plating is generally applied to the contact portion of the reed switch. Depending on the application, ruthenium or iridium plating is further stacked on the coating to improve its heat resistance. At the same time, this method cannot avoid the complexity of the manufacturing process and the high cost of the product.
課題を解決する手段として、本発明は、ロジュウムに対し、更に高融点で且つ、硬度を有し、更に、コスト・ダウンの期待が持てる金属を選択し、此れを、金属ロジュウムと、同一溶液中で、合金として、電解析出させ、所定の性能を保持した金属薄膜を提供する事を、開発した。 As a means for solving the problems, the present invention selects a metal having a higher melting point and hardness than rhodium, and that can be expected to reduce costs, and this is the same solution as metal rhodium. In particular, it has been developed to provide a metal thin film that is electrolytically deposited and maintains a predetermined performance as an alloy.
本発明では、金属ロジュウムと共析して、金属ロジュウムの特性を更に向上させる事に期待できる金属として、原子番号７５のレニュウムＲｅを採用した。 In the present invention, rhenium Re having an atomic number of 75 is employed as a metal that can be expected to eutect with the metal rhodium and further improve the properties of the metal rhodium.
金属レニュウムは、融点３１８０℃であり、この数値は、タングステン（Ｗ）に次ぐ、現在地球上で、発見されている金属で、２番目である。 Metallic rhenium has a melting point of 3180 ° C., which is the second metal that is currently found on earth after tungsten (W).
又、電解を行う時の、分解電位が、ロジュウムと近い値なので、合金めっきとして適合していると判断した。 Moreover, since the decomposition potential at the time of electrolysis was a value close to that of rhodium, it was judged to be suitable for alloy plating.
以下、本発明の、電解析出による、合金薄膜の製法について、実姉例により、具体的に説明する。 Hereafter, the manufacturing method of the alloy thin film by electrolytic deposition of this invention is demonstrated concretely by an actual sister example.
ロジュウムめっきの母体となるめっき液として、硫酸ロジュウム浴を採用る。
硫酸ロジュウムよくは、金属分２ｇ／Ｌに相当するりゅうさんロジュウム伝導補助として硫酸を加え、トータル酸量として硫酸５０ｇ／Ｌを含有する電解液を調整した。A rhodium sulfate bath is used as the plating solution that is the base of rhodium plating.
Rhodium sulphate. Sulfuric acid was often added as an auxiliary for rhodium conduction, corresponding to a metal content of 2 g / L, and an electrolyte containing 50 g / L of sulfuric acid as the total acid amount was prepared.
レニュウムは、比較的容易に入手できる、過レニュウム酸アンモンを用いた。
同塩は、金属レニュウム分６９．４％を含有する。
（Ｒｅ／ＮＨ４ＲｅＯ４）＝（１８６．２／２６８．２４）＝０．６９４５＝６９．４５％Renium used was ammonium perrenumate, which is relatively easily available.
The salt contains 69.4% metal renium.
(Re / NH 4 ReO 4 ) = (186.2 / 268.24) = 0.6945 = 69.45%
純度９９．９％の過レニュウム酸アンモンを、２．８８２ｇ精秤し、純水１００ｍｌに投入する。純水中には、予め０．５ｍｌの硫酸を加えておき、レニュウム塩の溶解を容易にした。
この溶液は、金属レニュウム２．０ｇ／１００ｍｌの溶液となる。2.882 g of ammonium perrhenate having a purity of 99.9% is precisely weighed and put into 100 ml of pure water. In pure water, 0.5 ml of sulfuric acid was added in advance to facilitate dissolution of the rhenium salt.
This solution becomes a metal rhenium 2.0 g / 100 ml solution.
００１６項で表示した硫酸ロジュウムめっき浴に、００１８項のレニュウム溶液加え、Ｒｈ：Ｒｅ＝２．０：０．１〜２．０まで、段階的に添加し，各比率に於ける電解析出を、観察した。 Add the rhenium solution of item 0018 to the rhodium sulfate plating bath indicated in item 0016, and add stepwise from Rh: Re = 2.0: 0.1 to 2.0 to perform electrolytic deposition at each ratio. Observed.
電解条件としては、通常のロジュウム単体のめっき浴の条件に準じて行った。通常のロジュウムめっきの場合の電流密度を印加した場合にはＲｈ−Ｒｅの含有比率を、Ｒｈ１０：Ｒｅ１にした場合に、析出被膜は、Ｒｈ単体の析出より、黒味を帯びた灰白色を呈し、明らかに、Ｒｈ−Ｒｅの共析被膜である事が確認された。 The electrolysis was carried out in accordance with the conditions of a normal rhodium plating bath. When the current density in the case of normal rhodium plating is applied, when the content ratio of Rh-Re is set to Rh10: Re1, the deposited film exhibits a blackish grayish white from the precipitation of Rh alone, Clearly, it was confirmed to be a Rh—Re eutectoid film.
電解条件を一定にし、浴中のＲｈ：ＲＥの含有比率を１０：１から１０：５まで、少しずつ変動した結果、Ｒｅの増加にしたがって、析出被膜の色調は、灰黒色が濃くなって来る事が確認された。 As a result of making the electrolysis conditions constant and changing the Rh: RE content ratio in the bath from 10: 1 to 10: 5 little by little, as the Re increases, the color tone of the deposited film becomes dark black. Things were confirmed.
Ｒｈ：Ｒｅの合金比率は、（１０：１）〜（１０：２）の範囲で、光沢のある青味を帯びた灰黒色の被膜が形成され、耐摩耗性も、Ｒｈ単体の被膜と同等の物が得られた。 The alloy ratio of Rh: Re is in the range of (10: 1) to (10: 2), and a glossy bluish gray-black coating is formed, and the wear resistance is equivalent to the coating of Rh alone. Was obtained.
りーど・スイッチ等、工業的に、利用される場合は、通常は２〜５ミクロンの膜厚が要求されているので、厚付け用として、燐酸浴のめっき液を用いた。
金属分３ｇ／Ｌ；遊離燐酸７０〜１２０ｇの基本液に、過レニュウム酸アンモンを溶解し、添加して、燐酸錯塩型のＲｈ−Ｒｅの合金めっき浴を造り、電解析出のテストを行った。When industrially used such as a switch or a switch, a film thickness of 2 to 5 microns is usually required, so a phosphoric acid bath plating solution was used for thickening.
3g / L of metal content; ammonium perrhenate was dissolved in a basic solution of 70 to 120 g of free phosphoric acid and added to form a phosphoric acid complex type Rh-Re alloy plating bath, and an electrolytic deposition test was conducted. .
同めっき浴でも、硫酸浴と、同様の光沢のある青灰黒色の被膜が得られた。
電解条件は、Ｒｈ単体の厚付け燐酸ロジュウム浴と同様の条件で、目的の膜厚（２〜５ミクロン）の被膜が得られた。In the same plating bath, the same glossy blue-gray-black coating as in the sulfuric acid bath was obtained.
The electrolytic conditions were the same as those for the Rh simple substance thickened rhodium phosphate bath, and a film having a target film thickness (2 to 5 microns) was obtained.
同被膜は、５ミクロンの膜厚でも、マイクロクラックを生ぜず、良好な合金組成の被膜として、電気接点、及び、その他の耐熱性、耐摩耗性を必要とする部品の表面被服に対応できる事が、確認された。 The coating does not produce microcracks even at a thickness of 5 microns, and as a coating with a good alloy composition, it can be used for surface contact of electrical contacts and other parts that require heat resistance and wear resistance. However, it was confirmed.
析出被膜のＲｈ：Ｒｅの合金の含有比率は、Ｉ．Ｃ．Ｐ．で測定した結果、モル比で、Ｒｈ（７０％）Ｒｅ（３０％）の値が、確認された。
Ｉ．Ｃ．Ｐ．に依る測定グラフを参考に、提示する。The content ratio of the Rh: Re alloy in the deposited film is as follows. C. P. As a result, the value of Rh (70%) Re (30%) was confirmed in terms of molar ratio.
I. C. P. It is presented with reference to the measurement graph.
リードスイッチ用端子に応用する為に、５２アロイ（５２％ニッケル含有スチール）素材に，然るべき、脱脂、表面活性の工程を経て、その表面に純金めっきを、１ミクロンめっき施工を行い、次いで、本発明の、Ｒｈ−Ｒｅ合金のめっきを、燐酸浴を用いて、２ミクロン、及び５ミクロンの二段階のめっきを行い、実用試験に供し、好結果をえた。 For application to reed switch terminals, 52 alloy (52% nickel-containing steel) material is subjected to appropriate degreasing and surface activation processes. The Rh-Re alloy plating of the invention was subjected to a practical test by performing two-step plating of 2 microns and 5 microns using a phosphoric acid bath, and good results were obtained.
装飾品に対しては、本発明の硫酸酸性浴の同Ｒｈ−Ｒｅ合金めっきを０．１〜０．５ミクロン厚さに、ネックレス、指輪、ペンダントに被服して、実用に供した。 これ等は、いずれも、耐摩耗性に優れた、明るい光沢を持った、青灰色の美麗な装飾品として、評価された。
いずれも、従来の、ロジュウムめっき品と、遜色ない耐久性を持った被膜として、提供される。For the decorative article, the sulfuric acid acid bath of the present invention was coated with the same Rh-Re alloy plating in a thickness of 0.1 to 0.5 microns on a necklace, a ring and a pendant for practical use. All of these were evaluated as beautiful blue-gray ornaments with excellent abrasion resistance and bright luster.
Both are provided as a conventional coating film having durability comparable to that of a rhodium-plated product.
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