US3734839A - Alkaline cyanide zinc electroplating - Google Patents
Alkaline cyanide zinc electroplating Download PDFInfo
- Publication number
- US3734839A US3734839A US00185348A US3734839DA US3734839A US 3734839 A US3734839 A US 3734839A US 00185348 A US00185348 A US 00185348A US 3734839D A US3734839D A US 3734839DA US 3734839 A US3734839 A US 3734839A
- Authority
- US
- United States
- Prior art keywords
- cyanide
- zinc
- polyethylenimine
- carbon atoms
- range
- 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 abstract description 23
- GTLDTDOJJJZVBW-UHFFFAOYSA-N zinc cyanide Chemical compound [Zn+2].N#[C-].N#[C-] GTLDTDOJJJZVBW-UHFFFAOYSA-N 0.000 title abstract description 5
- 239000011701 zinc Substances 0.000 abstract description 33
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 abstract description 32
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 32
- 229910052725 zinc Inorganic materials 0.000 abstract description 32
- 229920002873 Polyethylenimine Polymers 0.000 abstract description 27
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 abstract description 24
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 abstract description 22
- -1 PYRIDINE COMPOUND Chemical class 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 11
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 229910052736 halogen Inorganic materials 0.000 abstract description 7
- 150000002367 halogens Chemical class 0.000 abstract description 7
- 150000003839 salts Chemical class 0.000 abstract description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002659 electrodeposit Substances 0.000 abstract description 2
- SLRMQYXOBQWXCR-UHFFFAOYSA-N 2154-56-5 Chemical class [CH2]C1=CC=CC=C1 SLRMQYXOBQWXCR-UHFFFAOYSA-N 0.000 abstract 2
- CIUQDSCDWFSTQR-UHFFFAOYSA-N [C]1=CC=CC=C1 Chemical class [C]1=CC=CC=C1 CIUQDSCDWFSTQR-UHFFFAOYSA-N 0.000 abstract 1
- 125000004432 carbon atom Chemical group C* 0.000 description 20
- 238000007747 plating Methods 0.000 description 15
- 125000000217 alkyl group Chemical group 0.000 description 14
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 14
- 125000003342 alkenyl group Chemical group 0.000 description 7
- 125000003545 alkoxy group Chemical group 0.000 description 7
- 125000000304 alkynyl group Chemical group 0.000 description 7
- 125000001424 substituent group Chemical group 0.000 description 6
- 238000005282 brightening Methods 0.000 description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 3
- 229910017464 nitrogen compound Inorganic materials 0.000 description 3
- 150000002830 nitrogen compounds Chemical group 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- SSLIBLGVKYPVPA-UHFFFAOYSA-O pyridin-1-ium cyanide Chemical compound [C-]#N.[NH+]1=CC=CC=C1 SSLIBLGVKYPVPA-UHFFFAOYSA-O 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
- C25D3/24—Electroplating: Baths therefor from solutions of zinc from cyanide baths
-
- 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
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
Definitions
- R is alkyl, alkenyl or alkynyl of 1 to 4 carbon atoms, benzyl and substituted benzyl wherein the substituent is at least one of alkyl of 1 to 4 carbon atoms, halogen, cyanide, alkoxy of 1 to 4 carbon atoms, phenyl and or a hydrohalide salt thereof,
- the weight ratio of polyethylenimine to quaternary pyridine compound being within the range of :1 to 1:100.
- the electroplating bath has a weight ratio of cyanide to zinc within the range of 0.1-3.5: 1, preferably about 1:1.
- This invention relates to zinc electroplating baths and processes and more particularly to alkaline, cyamde zinc electroplating baths and processes.
- R is alkyl, alkenyl or alkynyl of 1 to 4 carbon atoms, benzyl and substituted benzyl wherein the substituent is at least one of alkyl of 1 to 4 carbon atoms, halogen, cyanide, alkoxy of 1 to 4 carbon atoms, phenyl and or a hydrohalide salt thereof,
- the weight ratio of polyethylenimine to quaternary pyridine compound being within the range of 10:1 to 1:100 and said bath having a weight ratio of cyanide to zinc within the range of 0.1-3.5: 1.
- an aqueous addition agent for an alkaline electroplating bath consisting essentially of an aqueous solution at a pH between 4.5 and 8 of a combination of polyethylenimine having a molecular Weight between about 600 and 60,000 and a quaternary pyridine compound of the formula:
- R is alkyl, alkenyl or alkynyl of 1 to 4 carbon atoms, benzyl and substituted benzyl wherein the substituent is at least one of alkyl of 1 to 4 carbon atoms, halogen, cyanide, alkoxy of 1 to 4 carbon atoms, phenor a hydrohalide salt thereof,
- the weight ratio of polyethylenimine to quaternary pyridine compound being within the range of 10:1 to 1:100, said combination being at a concentration in solution of between 1 and 50 percent by weight.
- the polyethylenimine useful in the plating bath has a erably at about 1 to 30 percent by weight.
- weights below 600 and about 60,000 may also be empH of the aqueous solution should be between about 4.5 ployed, although those below 600 are not generally availand 8.
- pH outside this range the quaternary pyridine able commercially while those much over 60,000 are not 5 compound will tend to precipitate or the solution will be sufficiently soluble to be generally useful.
- a preferred pH range is 5.5 to 7.
- Poly- The plating bath is operated according to normal proethylenimine is added to the bath to give a concentration cedures using a sodium cyanide concentration within the of 0.005 to 2 grams per liter, preferably 0.02 to 0.2 gram range of about 5 to 45 grams per liter, preferably 5 to 20 per liter for barrel plating and 0.05 to 0.5 gram per liter grams per liter, and most preferably about 7 grams per for rack plating.
- liter and a zinc concentration about 5 to 20 grams per The quaternary pyridine compounds useful in the liter, and most preferably about 7 grams per liter.
- the higher cyanide concentrations are employed in high cyanide plating baths and the present brightening system is effective at these concentrations to enable the electroplater to convert his bath to lower cyanide levels, i.e., in the range of about 5 to grams per liter.
- the weight ratio of cyanide R to zinc should be in the range of about 0.1-3.5 :1, prefwherein R is alkyl, alkenyl, or alkynyl of 1 to 4 carbon 20 erably about 1:1 to 2:1 at the low cyanide levels.
- Plating atoms, benzyl and substituted benzyl wherein the ubbath temperatures will usually be between 20 and 40 C.
- stituent is at least one of alkyl of 1 to 4 carbon atoms, however, the brightening system can provide bright dehalogen, cyanide, alkoxy of 1 to 4 carbon atoms, phenyl posits over a wide current density range at temperatures and up 10 55 C-
- bath-soluble polymers may be added to the CHz-N plating bath in particular situations to give further improvements in operation.
- polyvinyl alcohol 00- or an oxidized polyvinyl alcohol can be used to replace or a hydrohalide salt ther of, a portion of the polyethylenimine in rack plating to give improved brightness to the zinc deposit.
- the brightening system of the present invention has the pyridinium 3-Carb0XYlat and y pyridinium advantages of good shelf life, good chemical stability in boxylate
- other compounds which may be used are 1-(4- the plating bath and a wide operating range so that the methylbenlyl) pyridinium 3-cafboxylflte, 'M- electroplater can make a running conversion from a high y pyridinium 3-carb0Xy1ate, y pyridinium cyanide bath to a low cyanide bath without affecting the carboxylate, and l-propargyl pyridinium 3-carboxylate. uality of the plating work.
- Thfise Compounds can also be Used as the hy r h l
- the invention can be further understood by referring salts such as hydrochloride or hydrobromide.
- salts such as hydrochloride or hydrobromide.
- the quatert th following examples in which parts and percentages nary pyridine compound is added to the bath to give are b weight unl other i indi t d,
- G A ratio used will depend upon the type of plating operation employed, the temperature of operation and the concen- Zn metaufmm Zno) tration of the bath. Generally, when the concentration of Sodium cyamdq the bath increases the Wei ht ratio will shift to hi her Sdmm hydmxlde 75 g g Sodium carbonate 52 concentrations of the quaternary pyridine compound.
- the combination of brightening ingredients used are Hull Cell panels were plated at 25 C. for 5 minutes at preferably used in the form of aqueous addition agents for 2 amps. using combinations of polyethylenimine and a zinc electroplating baths.
- Additives for the plating baths quaternary pyridine compound as brighteners in the stock can be prepared by dissolving the polyethylenimine and 55 solution. Each panel was bright-dipped in dilute nitric quaternary pyridine compound at the desired ratio at a acid before examination. The brightener added and results solids content of about 1 to 50 percent by weight, prefare shown in Table I.
- h drNgrE.1$PO 1-benzy1pyridiniiun 3-carb0xylate
- PEI Polyethy1enimine
- qnethyl BPC l -(4,-methylbenzyl) pryidinium a-carbogylate y 0 tom 0.
- Hull Cell panels were plated for 5 minutes at 2 amps. at 25 C., 35 C. and 45 C. from a plating bath of the following composition:
- R is alkyl, alkenyl or alkynyl of 1 to 4 carbon atoms, benzyl and substituted benzyl wherein the substituent is at least one of alkyl of 1 to 4 carbon atoms, halogen, cyanide, alkoxy of 1 to 4 carbon atoms, phenyl and war I about 600 and 1800 which is at a concentration within the range of 0.005 to 2 grams per liter.
- an aqueous alkaline cyanide zinc electroplating bath comprising: having added to said bath a combination of polyethylenimine having a molecular weight within the range of about 600 and 1800 and l-benzyl pyridinium 3-carboxylate, at a weight ratio within the range of about 1:1 to 1:20 and each at a concentration within the range of about 0.02 to 0.5 gram per liter, said bath having a weight ratio of cyanide to zinc of 1:1 at a cyanide concentration as sodium cyanide of about 5 to 20 grams per liter.
- R is alkyl, alkenyl or alkynyl of 1 to 4 carbon atoms, benzyl and substituted benzyl wherein the substituent'is at least one of alkyl of 1 to 4 carbon atoms, halogen, cyanide, alkoxy of 1 to 4 carbon atoms,
- the weight ratio of polyethylenimine to quaternary pyridine compound being within the range of 10:1 to 1:100, maintaining said bath at a weight ratio of cyanide to zinc within the range of 0.1-3.5 :1, and said polyethylenirnine being at a concentration within the range of 0.005 to 2 grams per liter.
- An aqueous addition agent for an alkaline electroplating bath consisting essentially of an aqueous solution at a pH between 4.5 and 8 of a combination of polyethylenimine having a molecular weight between about 600 and 60,000 and a quaternary pyridine compound of the formula:
- R is alkyl, alkenyl or alkynyl of 1 to 4 carbon atoms, benzyl and substituted benzyl wherein the substituent is at least one of alkyl of 1 to 4 carbon atoms, halogen, cyanide, alkoxy of 1 to 4 carbon atoms, phenyl and COO- 15.
- the aqueous addition agent of claim 15 wherein the polyethylenimine molecular weight is within the range of about 600 and 1800.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US18534871A | 1971-09-30 | 1971-09-30 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3734839A true US3734839A (en) | 1973-05-22 |
Family
ID=22680624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00185348A Expired - Lifetime US3734839A (en) | 1971-09-30 | 1971-09-30 | Alkaline cyanide zinc electroplating |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US3734839A (enrdf_load_stackoverflow) |
| JP (1) | JPS549578B2 (enrdf_load_stackoverflow) |
| CA (1) | CA995620A (enrdf_load_stackoverflow) |
| FR (1) | FR2154685B1 (enrdf_load_stackoverflow) |
| GB (1) | GB1358371A (enrdf_load_stackoverflow) |
| IT (1) | IT968456B (enrdf_load_stackoverflow) |
| SE (1) | SE7600163L (enrdf_load_stackoverflow) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4229267A (en) * | 1979-06-01 | 1980-10-21 | Richardson Chemical Company | Alkaline bright zinc plating and additive therefor |
| US5650060A (en) * | 1994-01-28 | 1997-07-22 | Minnesota Mining And Manufacturing Company | Ionically conductive agent, system for cathodic protection of galvanically active metals, and method and apparatus for using same |
| US6468411B1 (en) | 2001-07-11 | 2002-10-22 | Taskem Inc. | Brightener for zinc-nickel plating bath and method of electroplating |
| CN116695204A (zh) * | 2023-08-08 | 2023-09-05 | 宁波德洲精密电子有限公司 | 一种ic框架镀锡加工方法 |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2288798A1 (fr) * | 1974-10-24 | 1976-05-21 | Popescu Francine | Bain et procede de zingage electrolytique brillant |
| JPS5173505A (en) * | 1974-12-23 | 1976-06-25 | Kao Corp | Tomeisetsukenno seizoho |
| US4851147A (en) * | 1987-02-26 | 1989-07-25 | Finetex, Inc. | Transparent combination soap-synthetic detergent bar |
| JP5005849B2 (ja) * | 2000-01-31 | 2012-08-22 | ディップソール株式会社 | アルカリ性亜鉛及び亜鉛合金めっき浴 |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3318787A (en) * | 1964-02-07 | 1967-05-09 | Udylite Corp | Electrodeposition of zinc |
| US3296105A (en) * | 1964-04-03 | 1967-01-03 | Du Pont | Zinc cyanide electroplating bath and process |
| NL6611248A (enrdf_load_stackoverflow) * | 1965-12-02 | 1966-10-25 | ||
| US3411996A (en) * | 1965-12-02 | 1968-11-19 | Du Pont | Process for brightening zinc and cadmium electroplate using an inner salt of a quaternized pyridine carboxylic acid and compositions containing the same |
| US3472743A (en) * | 1966-12-19 | 1969-10-14 | Du Pont | Zinc plating baths and additives therefor |
| US3386898A (en) * | 1967-07-17 | 1968-06-04 | Du Pont | Alkaline, cyanide zinc electroplating bath process, and additive therefor |
-
1971
- 1971-09-30 US US00185348A patent/US3734839A/en not_active Expired - Lifetime
-
1972
- 1972-09-25 CA CA152,483A patent/CA995620A/en not_active Expired
- 1972-09-28 FR FR7234350A patent/FR2154685B1/fr not_active Expired
- 1972-09-29 GB GB4513272A patent/GB1358371A/en not_active Expired
- 1972-09-29 IT IT29888/72A patent/IT968456B/it active
- 1972-09-30 JP JP9857172A patent/JPS549578B2/ja not_active Expired
-
1976
- 1976-01-09 SE SE7600163A patent/SE7600163L/xx unknown
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4229267A (en) * | 1979-06-01 | 1980-10-21 | Richardson Chemical Company | Alkaline bright zinc plating and additive therefor |
| US5650060A (en) * | 1994-01-28 | 1997-07-22 | Minnesota Mining And Manufacturing Company | Ionically conductive agent, system for cathodic protection of galvanically active metals, and method and apparatus for using same |
| US6468411B1 (en) | 2001-07-11 | 2002-10-22 | Taskem Inc. | Brightener for zinc-nickel plating bath and method of electroplating |
| CN116695204A (zh) * | 2023-08-08 | 2023-09-05 | 宁波德洲精密电子有限公司 | 一种ic框架镀锡加工方法 |
| CN116695204B (zh) * | 2023-08-08 | 2023-11-03 | 宁波德洲精密电子有限公司 | 一种ic框架镀锡加工方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| DE2247875B2 (de) | 1976-12-30 |
| SE7600163L (sv) | 1976-01-09 |
| JPS549578B2 (enrdf_load_stackoverflow) | 1979-04-25 |
| DE2247875A1 (de) | 1973-04-05 |
| GB1358371A (en) | 1974-07-03 |
| CA995620A (en) | 1976-08-24 |
| JPS4842935A (enrdf_load_stackoverflow) | 1973-06-21 |
| FR2154685A1 (enrdf_load_stackoverflow) | 1973-05-11 |
| IT968456B (it) | 1974-03-20 |
| FR2154685B1 (enrdf_load_stackoverflow) | 1976-08-13 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| AS | Assignment |
Owner name: MCGEAN-ROHCO, INC. 1250 TERMINAL TOWER, CLEVELAND, Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:E.I. DU PONT DE NEMOURS AND COMPANY;REEL/FRAME:004015/0065 Effective date: 19820520 |