US3890210A - Method and electrolyte for electroplating rhodium-rhenium alloys - Google Patents
Method and electrolyte for electroplating rhodium-rhenium alloys Download PDFInfo
- Publication number
- US3890210A US3890210A US507831A US50783174A US3890210A US 3890210 A US3890210 A US 3890210A US 507831 A US507831 A US 507831A US 50783174 A US50783174 A US 50783174A US 3890210 A US3890210 A US 3890210A
- Authority
- US
- United States
- Prior art keywords
- rhodium
- rhenium
- bath
- compound
- deposit
- 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.)
- Expired - Lifetime
Links
- 238000009713 electroplating Methods 0.000 title claims abstract description 22
- -1 rhodium-rhenium Chemical compound 0.000 title claims abstract description 20
- 229910000691 Re alloy Inorganic materials 0.000 title claims abstract description 18
- 239000003792 electrolyte Substances 0.000 title description 6
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 68
- 239000010948 rhodium Substances 0.000 claims abstract description 68
- WUAPFZMCVAUBPE-UHFFFAOYSA-N Rhenium Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052702 rhenium Inorganic materials 0.000 claims abstract description 44
- 238000007747 plating Methods 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 238000000151 deposition Methods 0.000 claims abstract description 8
- 239000010953 base metal Substances 0.000 claims description 18
- IIACRCGMVDHOTQ-UHFFFAOYSA-N Sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 150000003282 rhenium compounds Chemical class 0.000 claims description 10
- 229910001369 Brass Inorganic materials 0.000 claims description 8
- 239000010951 brass Substances 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229910000906 Bronze Inorganic materials 0.000 claims description 6
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 6
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 6
- JOTGKJVGIIKFIQ-UHFFFAOYSA-N Perrhenic acid Chemical compound [OH2][Re]([OH2])(=O)(=O)(=O)O[Re](=O)(=O)=O JOTGKJVGIIKFIQ-UHFFFAOYSA-N 0.000 claims description 6
- 230000002378 acidificating Effects 0.000 claims description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 6
- 150000001340 alkali metals Chemical class 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 239000010974 bronze Substances 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 150000003284 rhodium compounds Chemical class 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- 239000002253 acid Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910052697 platinum Inorganic materials 0.000 description 8
- 229910000629 Rh alloy Inorganic materials 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 239000005092 Ruthenium Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000004070 electrodeposition Methods 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 4
- 229910052707 ruthenium Inorganic materials 0.000 description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 229910001260 Pt alloy Inorganic materials 0.000 description 2
- FLNJGSYVLQBPLF-UHFFFAOYSA-K [Rh+3].NS([O-])(=O)=O.NS([O-])(=O)=O.NS([O-])(=O)=O Chemical compound [Rh+3].NS([O-])(=O)=O.NS([O-])(=O)=O.NS([O-])(=O)=O FLNJGSYVLQBPLF-UHFFFAOYSA-K 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 230000000996 additive Effects 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical class [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 2
- 230000003139 buffering Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000536 complexating Effects 0.000 description 2
- 230000001419 dependent Effects 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 150000001455 metallic ions Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 230000000737 periodic Effects 0.000 description 2
- 239000011253 protective coating Substances 0.000 description 2
- 150000003281 rhenium Chemical class 0.000 description 2
- 150000003283 rhodium Chemical class 0.000 description 2
- CDPPVBDJYWOMMV-UHFFFAOYSA-K rhodium(3+);phosphate Chemical compound [Rh+3].[O-]P([O-])([O-])=O CDPPVBDJYWOMMV-UHFFFAOYSA-K 0.000 description 2
- 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 2
- 239000000126 substance Substances 0.000 description 2
- 229910052716 thallium Inorganic materials 0.000 description 2
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/567—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of platinum group metals
Abstract
Disclosed is an electroplating bath suitable for depositing a rhodium-rhenium alloy containing at least 70 weight % rhodium. Rhodium and rhenium are present in the plating bath in the form of soluble plateable compounds in a preferred weight ratio of at least about 4:1. The deposits obtained by this bath exhibit improved brightness over comparable baths containing no rhenium even without the addition of lead.
Description
United States Patent [1 Stevens et al.
[ METHOD AND ELECTROLYTE FOR ELECTROPLATING RHODlUM-RHENIUM ALLOYS [75] Inventors: Peter Stevens, Parsippany; George R. Lurie, South Bound Brook, both of NJ.
[73] Assignee: Oxy Metal Industries Corporation,
Detroit, Mich.
[22] Filed: Sept. 20, 1974 [21] Appl. No.: 507,831
Related U.S. Application Data [63] Continuation-impart of Ser. No. 372376, June 21 1973, abandoned.
[52] U.S. Cl 204/43 N [51] Int. Cl C23b 5/32 [58] Field of Search 204/43 N, 45 R, 45.5, 47,
[ June 17, 1975 [56] References Cited OTHER PUBLICATIONS Abner Brenner, Electrodeposition of Alloys," Vol. ll, pp. 598-606, (1963).
Primary E.\'aminer-G. L. Kaplan Attorney, Agent, or Firm-Arthur E. Kluegel; Richard P. Mueller; Betram F. Claeboe 5 7 ABSTRACT I Disclosed is an electroplating bath suitable for deposabout 4:1. The deposits obtained by this bath exhibit improved brightness over comparable baths containing no rhenium even without the addition of lead.
7 Claims, No Drawings .1 METHOD AND ELECTROLYTE FOR ELECTROPLATING RHODlUM-RHENIUM ALLOYS,
CROSS-REFERENCE TO RELATED APPLICATION This application is a continuation-in-part of U.S. Ser. No. 372,376 filed June 21, 1973, now abandoned.
BACKGROUND OF THE INVENTION This invention relates to improvements in and relating to the electrodeposition of rhodium alloys.
Electrodeposited rhodium has found considerable favor in recent years as a decorative coating material and as a contact face material owing to its extreme hardness and its resistance to corrosion and tarnish. Under normal conditions, rhodium is substantially un affected by contact with common acids and chemicals.
Deposits of rhodium typically exhibit desirable characteristics with regard to resistance to corrosion and wear, and superior hardness coupled with exceptionally high resistance to heat and good electrical conductivity. These properties render the rhodium deposit useful not only as protective coatings for silverware and jewelry but also as protecting parts for electronic applications. The primary disadvantage of rhodium deposits is that they are somewhat lacking in desired brightness for certain applications.
U.S. Pat. No. 3,671,408 discloses a bath suitable for depositing a rhodium-platinum alloy. Both rhodium and platinum are classified as precious metals and the price of such metals is on the order of $55/oz. and upward. The present invention permits the plater to obtain brightened deposits of a predominately rhodium alloy without incorporating a Group VIII (b) precious metal.
U.S. Pat. No. 3,692,641 teaches a deposit containing ruthenium, rhodium and platinum. The deposit is predominately ruthenium and contains minor portions of rhodium or platinum. Additionally, the bath disclosed in that patent contains indium thallium or gallium elements of Group III (a) of the Periodic Table of Elements. Since the deposit of that patent contains only minor portions of rhodium, it does not exhibit the well known advantageous characteristics of a rhodium deposit. US. Pat. No. 3,31 1,547 likewise discloses a rhodium alloy deposit containing the Group III (a) element indium as the alloying metal. None of the foregoing patents disclose the use of rhenium as a brightener for rhodium deposits.
SUMMARY OF THE INVENTION It has now been discovered that a rhodium deposit of improved brightness can be obtained by including in the electroplating bath a minor quantity of a soluble rhenium compound. The bath is aqueous and acidic and contains a soluble rhodium compound and a compatible soluble rhenium compound in a weight ratio of rhodium to rhenium sufficient to deposit an alloy containing at least 70 weight rhodium.
DETAILED DESCRIPTION OF THE INVENTION The scope of the invention includes an electroplating bath, a method of electroplating comprising electrolyzing the bath, and the resulting plated article.
Since it is desired that the deposit exhibit to the extent possible the advantageous characteristics of a pure rhodium deposit, the deposit should be predominately rhodium. By predominately, we mean the deposit should contain at least weight rhodium. Preferably, the deposit will contain at least about weight rhenium and most preferably weight The rhenium content of the electroplating bath is dependent upon the rhodium concentration. The rhodium concentration may be between 0.1 and 15 grams per liter and preferably between 0.5 and 5 grams per liter. The desired rhenium content may vary somewhat depending on the presence and concentration of additive components and operating conditions such as current density but should be selected to provide a deposit of at least 70 weight rhodium. Under normal operating conditions specified below, the weight ratio of rhodium to rhenium is at least 4:1 and is preferably at least 10:1. Typically, the rhenium content will vary between and 200 mg/l.
The rhodium salts generally used for plating are rhodium sulfate, rhodium sulfamate or rhodium phosphate. However, any rhodium slat may be used which provides the rhodiumin a condition such that rhodium can be plated from an acid bath and which is stable under the acid conditions required.
The preferred rhenium compounds are the alkali metal and ammonium perrhenates and perrhenic acid. However, any rhenium salt suitable for plating rhenium may be substituted.
The bath should be maintained on the acid side by the presence of at least 10 g/l of a compatible strong inorganic acid. Preferably, the bath contains sulfamic acid in a concentration of from 10 g/l up to the solubility limit of the solution. Preferably, the sulfamic acid is present in a concentration between 20 and 150 grams per liter and most preferably between 50 and grams per liter.
The bath may additionally contain other additives well known in the art. Suitable additives include those for improving conductivity, providing buffering power, and complexing metallic ions. It has been found that concentrated sulfuric acid may be advantageously added to the present bath to improve the conductivity Normally quantities of up to 100 milliliters per liter of solution and preferably between 1 and 50 milliliters per liter of solution are satisfactory.
The rhodium-rhenium bath may be used to plate any base metal surface on which rhodium itself can be plated. Suitable base metals include brass, bronze, copper, silver, mild steel, nickel and nickel alloys. In some instances, it may be desirable to flash plate a layer of silver over the base metal prior to plating in order to avoid reaction between the base metal and the plating bath. Flash platings of palladium, palladium-gold or gold are also suitable for this purpose.
The rhodium-rhenium alloy may be deposited from the bath at a temperature of between about 60 and 180F. by passing the current at a current density of about 5 to 40 amps per square foot through the bath to a cathode immersed therein. Preferably, the current density is about 10 to 30 amps per square foot and the temperature about 80 to F.
The deposits obtained by the process of this invention range from flash coatings of approximately 2 micro inch thickness up to coatings of 200 micro inches or more. The advantage of the deposit of this invention lies in the fact that the brightness is superior to that of pure rhodium deposits known in the art.
EXAMPLE A bath was prepared containing the following ingredients per liter:
Rhodium as rhodium sulfate Sulfamic acid Concentrated sulfuric acid oom comm
The bath temperature was maintained between 110 and 120F. A current density of 20 amps/square foot was applied using a platinum anode and a brass panel. While the above concentrations were substantially maintained, plating was performed under agitation after adding rhenium in concentrations varying between approximately 0.01 and 0.15 g/l. The rhenium was added in the form of KReO In every case, the deposits obtained were bright. A titanium panel was plated and the deposit analyzed and found to contain between 10 and rhenium. Similar baths prepared without the rhenium or sulfamic acid produced no mirror bright deposits and most exhibited pitting in the deposits.
What is claimed is:
1. An aqueous acidic electroplating bath, suitable for depositing a bright rhodium-rhenium alloy consisting essentially of rhodium and rhenium comprising at least 10 g/l of sulfamic acid, from 0.1 to 15 g/l of rhodium as a plateable compound, and at least 0.01 g/l rhenium as a plateable compound in a weight ratio of rhodium to rhenium of at least 411.
2. The bath of claim 1 wherein said weight ratio is at least 10:1.
3. The bath of claim 1 wherein said rhenium concentration is from 0.1 to 0.2 g/l.
4. The bath of claim 1 comprising at least 10 ml/l of concentrated sulfuric acid and between about 50 and 100 g/l of sulfamic acid.
5. The bath of claim 1 wherein said rhodium compound is a salt selected from the group consisting of sulfate, sulfamate and phosphate and said rhenium compound is selected from the group consisting of the alkali metal and ammonium perrhenates and perrhenic acid.
6. A method of plating a rhodium-rhenium alloy deposit on a base metal surface comprising electrolyzing the surface in the presence of the bath of claim 1 with the base metal as a cathode.
7. The method of claim 6 wherein saidvbase metal is selected from the group consisting of brass, bronze,
copper, silver, mild steel, nickel and nickel alloys.
Claims (7)
1. AN AQUEOUS ACIDIC ELECTROPLATING BATH, SUITABLE FOR DEPOSITING A BRIGHT RHODIUM-RHENIUM ALLOY CONSISTING ESSENTIALLY OF RHODIUM AND THEMIUM COMPRISING AT LEAST 10 G/L OR SULFAMIC ACID, FROM 0.1 TO 15 G/L RHODIUM AS A PLATEABLE COMPOUND, AND AT LEAST 0.01 G/L RHENIUM AS A PLATEABLE COMPOUND IN A WEIGHT RATIO OF RHODIUM TO RHENIUM OF AT LEAST 4:2.
2. The bath of claim 1 wherein said weight ratio is at least 10:
3. The bath of claim 1 wherein said rhenium concentration is from 0.1 to 0.2 g/l.
4. The bath of claim 1 comprising at least 10 ml/l of concentrated sulfuric acid and between about 50 and 100 g/l of sulfamic acid.
5. The bath of claim 1 wherein said rhodium compound is a salt selected from the group consisting of sulfate, sulfamate and phosphate and said rhenium compound is selected from the group consisting of the alkali metal and ammonium perrhenates and perrhenic acid.
6. A method of plating a rhodium-rhenium alloy deposit on a base metal surface comprising electrolyzing the surface in the presence of the bath of claim 1 with the base metal as a cathode.
7. The method of claim 6 wherein said base metal is selected from the group consisting of brass, bronze, copper, silver, mild steel, nickel and nickel alloys.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US507831A US3890210A (en) | 1973-06-21 | 1974-09-20 | Method and electrolyte for electroplating rhodium-rhenium alloys |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US37237673A | 1973-06-21 | 1973-06-21 | |
| US507831A US3890210A (en) | 1973-06-21 | 1974-09-20 | Method and electrolyte for electroplating rhodium-rhenium alloys |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3890210A true US3890210A (en) | 1975-06-17 |
Family
ID=27005742
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US507831A Expired - Lifetime US3890210A (en) | 1973-06-21 | 1974-09-20 | Method and electrolyte for electroplating rhodium-rhenium alloys |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US3890210A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899693A (en) * | 2010-07-30 | 2010-12-01 | 安徽华东光电技术研究所 | Method for locally plating rhenium on oxygen-free copper matrix |
| US11421335B2 (en) | 2019-04-08 | 2022-08-23 | Umicore Galvanotechnik Gmbh | Electrolyte for the deposition of anthracite/black rhodium/ruthenium alloy layers |
-
1974
- 1974-09-20 US US507831A patent/US3890210A/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| Abner Brenner, "Electrodeposition of Alloys," Vol. II, pp. 598-606, (1963). * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899693A (en) * | 2010-07-30 | 2010-12-01 | 安徽华东光电技术研究所 | Method for locally plating rhenium on oxygen-free copper matrix |
| US11421335B2 (en) | 2019-04-08 | 2022-08-23 | Umicore Galvanotechnik Gmbh | Electrolyte for the deposition of anthracite/black rhodium/ruthenium alloy layers |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| AS | Assignment |
Owner name: HOOKER CHEMICALS & PLASTICS CORP. Free format text: MERGER;ASSIGNOR:OXY METAL INDUSTRIES CORPORATION;REEL/FRAME:004075/0885 Effective date: 19801222 |
|
| AS | Assignment |
Owner name: OCCIDENTAL CHEMICAL CORPORATION Free format text: CHANGE OF NAME;ASSIGNOR:HOOKER CHEMICAS & PLASTICS CORP.;REEL/FRAME:004126/0054 Effective date: 19820330 |
|
| AS | Assignment |
Owner name: OMI INTERNATIONAL CORPORATION, 21441 HOOVER ROAD, Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:OCCIDENTAL CHEMICAL CORPORATION;REEL/FRAME:004190/0827 Effective date: 19830915 |
|
| AS | Assignment |
Owner name: MANUFACTURERS HANOVER TRUST COMPANY, A CORP OF NY Free format text: SECURITY INTEREST;ASSIGNOR:INTERNATIONAL CORPORATION, A CORP OF DE;REEL/FRAME:004201/0733 Effective date: 19830930 |