CS240582B1 - Electrolytic aqueous bath for nickel-phosphorus alloy deposition - Google Patents
Electrolytic aqueous bath for nickel-phosphorus alloy deposition Download PDFInfo
- Publication number
- CS240582B1 CS240582B1 CS84902A CS90284A CS240582B1 CS 240582 B1 CS240582 B1 CS 240582B1 CS 84902 A CS84902 A CS 84902A CS 90284 A CS90284 A CS 90284A CS 240582 B1 CS240582 B1 CS 240582B1
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- Czechoslovakia
- Prior art keywords
- nickel
- concentration
- water
- per
- phosphorus alloy
- Prior art date
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- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 title claims description 6
- 229910001096 P alloy Inorganic materials 0.000 title claims description 4
- 230000008021 deposition Effects 0.000 title description 3
- 229910001868 water Inorganic materials 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004327 boric acid Substances 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims description 5
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000004254 Ammonium phosphate Substances 0.000 claims 1
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims 1
- 235000019289 ammonium phosphates Nutrition 0.000 claims 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims 1
- 229910000159 nickel phosphate Inorganic materials 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 239000001488 sodium phosphate Substances 0.000 claims 1
- 229910000162 sodium phosphate Inorganic materials 0.000 claims 1
- GJYJYFHBOBUTBY-UHFFFAOYSA-N alpha-camphorene Chemical compound CC(C)=CCCC(=C)C1CCC(CCC=C(C)C)=CC1 GJYJYFHBOBUTBY-UHFFFAOYSA-N 0.000 abstract description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 abstract description 3
- XXSPKSHUSWQAIZ-UHFFFAOYSA-L 36026-88-7 Chemical compound [Ni+2].[O-]P=O.[O-]P=O XXSPKSHUSWQAIZ-UHFFFAOYSA-L 0.000 abstract description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 abstract description 2
- 239000000080 wetting agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 239000003792 electrolyte Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- -1 nickel fluoroborate Chemical compound 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005323 electroforming Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- RUQIYMSRQQCKIK-UHFFFAOYSA-M sodium;2,3-di(propan-2-yl)naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(C(C)C)C(C(C)C)=CC2=C1 RUQIYMSRQQCKIK-UHFFFAOYSA-M 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Chemically Coating (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
Lázeň sestává z fluoroboritanu nikelnatého v koncentraci 100 až 600 g na '1 000 ml vody, kyseliny borité v koncentraci 10 až 50 g na 1 000 ml vody a fosfornanu nikelnatého, sodného nebo amonného, případně kyseliny fosfrité v koncentraci 1 až 50 g na 1 000 mi vody. Pro odstranění vodíkového pittingu je použit přídavek smáčedla v koncentraci 0,01 až 1 g na 1000 ml vody.The bath consists of nickel borohydride at a concentration of 100 to 600 g per 1 000 ml of water, boric acid at a concentration of 10 to 50 g per 1 000 ml of water and nickel, sodium or ammonium hypophosphite or phosphite acid at a concentration of 1 to 50 g per 1 000 mi water. Addition of a wetting agent at a concentration of 0.01 to 1 g per 1000 ml of water is used to remove hydrogen pitting.
Vynález se týká složení elektrolytické vodní lázně pro· vylučování slitiny nikl — fosfor.The present invention relates to an electrolytic water bath composition for the precipitation of a nickel-phosphorus alloy.
Elektrolyticky vylučované povlaky nikl — fosfor mají podstatně vyšší mikrotvrdost než mají ostatní vylučované slitiny niklu. Používají se případech, kdy jsou na vyloučený kovový povlak kladeny velké nároky z hlediska otěru a kluzných vlastností. Elektrolyticky vyloučené povlaky slitiny nikl — fosfor mají po tepelném zpracování zvýšenou mikrotvrdost až o 50 % a jejich kvalita se vyrovná povrchům z · tvrdého chrómu.Electrolytically deposited nickel-phosphorus coatings have a significantly higher microhardness than other deposited nickel alloys. It is used when there is a high demand on abrasion and sliding properties on the deposited metal coating. Electrolytically deposited nickel-phosphorus coatings have an increased microhardness of up to 50% after heat treatment and their quality is comparable to hard chrome surfaces.
Dosud používané a v literatuře uváděné elektrolyty pro vylučování slitiny nikl-fosfor pracují při teplotách 80 až 90 °C a nízkém pH 0,5 až 1,5. Obsahují-li nikl ve formě síranů, chloridů a fosfor ve formě kyseliny fosforite.The electrolytes used for the deposition of the nickel-phosphorus alloy to date have been operating at temperatures of 80-90 ° C and low pH of 0.5-1.5. If they contain nickel in the form of sulphates, chlorides and phosphorus in the form of phosphorous acid.
Nevýhodou těchto · elektrolytů je vysoká provozní teplota a tím i značná energetická náročnost. Přitom při dlouhodobém provozu je technicky velmi náročné udržet nízkou hodnotu pH v rozmezí 0,5 až 1,5.The disadvantage of these electrolytes is the high operating temperature and thus the considerable energy consumption. However, it is technically very difficult to maintain a low pH value in the range of 0.5 to 1.5 during long-term operation.
Další známé, · avšak méně používané typy elektrolytů obsahují karbonové kyseliny, jako například ' kyselinu citrónovou. Tyto látky sice umožňují pracovat s provozní teplotou lázně podstatně nižší, v rozmezí 40 až 60 stupňů · Celsia, , při ,dlouhodobém provozu však dochází k rozkladu karbonových kyselin. Rozkladné produkty · pak zvyšují vnitřní pnutí vyloučených povlaků a tím dochází ke vzniku trhlin a destrukci vyloučených povlaků.Other known, but less used types of electrolytes include carbon acids, such as citric acid. Although these materials allow to operate at a substantially lower bath temperature, in the range of 40 to 60 degrees Celsius, carbon dioxide decomposes in long-term operation. The decomposition products then increase the internal stress of the deposited coatings, causing cracks and destruction of the deposited coatings.
Vynález odstraňuje nedostatky dosud známých elektrolytických lázní pro vylučování slitiny nikl —. fosfor a jeho podstata spočívá ve složení elektrolytu, který sestává z fluoroboritanu nikelnatého v koncentraci 100 až 600 g na 1 000 ml vody, kyseliny borité v koncentraci 10 až 50 g na 1000 ml vody a fosfornanu nikelnatého, sodného, nebo amonného, případně kyseliny fosforite v koncentraci 1 až 50 g na 1 000 ml vody.The present invention overcomes the drawbacks of the prior art electrolytic baths for the nickel-alloy deposition. phosphorus and its essence consists of an electrolyte consisting of nickel borohydride at a concentration of 100 to 600 g per 1 000 ml of water, boric acid at a concentration of 10 to 50 g per 1000 ml of water and nickel, sodium or ammonium hypophosphite in a concentration of 1 to 50 g per 1000 ml of water.
Pro další zlepšení kvality a odstranění · vodíkového pittingu je · výhodný přídavek ethylenoxidových smáčedel, případně alkylsulfonanových smáčedel v koncentraci 0,1 až 1 g na 1 000 ml vody.The addition of ethylene oxide surfactants or alkylsulfonate surfactants in a concentration of 0.1 to 1 g per 1000 ml of water is preferred to further improve the quality and remove hydrogen pitting.
Elektrolyt pracuje při provozních teplotách 30 až 50 °C v oblasti 2 až 3,5 pH. Katodová proudová hustota se pohybuje v rozmezí 1 až 16 A/dm2. Hlavní výhodou elektrolytu podle vynálezu je velmi nízká hodnota vnitřního pnutí a jeho dobrá životnost. Mikrotvrdost povlaků je vysoká, 900 až 1200 HM a není nutné další tepelné zpracování. Mikrotvrdost se v · rozmezí teplot 20 až 40 °C nemění. Vyloučené, povlaky obsahují 1 . až 20 % hmotnostních fosforu v závislosti , na koncentraci fosforu v elektrolytické lázni. Vzhledem k nízkému vnitřnímu pnutí jsou · vyloučené povlaky vhodné v oblasti galvanoplastiky.The electrolyte operates at operating temperatures of 30 to 50 ° C in the range of 2 to 3.5 pH. The cathode current density is in the range of 1 to 16 A / dm2. The main advantage of the electrolyte according to the invention is the very low value of the internal stress and its good service life. The microhardness of the coatings is high, 900 to 1200 HM, and no further heat treatment is required. The microhardness does not change in the temperature range of 20 to 40 ° C. Excluded coatings contain 1. up to 20% by weight of phosphorus depending on the concentration of phosphorus in the electrolytic bath. Due to the low internal stress, the deposited coatings are suitable in the field of electroforming.
P říklldlP said
200 g/1 000 ml HžO .200 g / 1000 ml H2O.
fluoroboritanu nikelnatého, g/1 000 ml H2O kyseliny borité, · g/1 000 ml H2O fosfornanu nikelnatého,nickel fluoroborate, g / 1 000 ml H2O boric acid, · g / 1 000 ml H2O nickel hypophosphite,
0,2 g/1 000 ml H2O ethylen-oxidového smáčedla, katodová proudová hustota 1 až 5 A/dm2, provozní teplota 50 °C,0.2 g / 1000 ml H2O ethylene oxide surfactant, cathode current density 1 to 5 A / dm 2 , operating temperature 50 ° C,
PH 2,5, mikrotvrdost 1150 HM, obsah fosforu v povlaku 7,5 % hmotnostních.PH 2.5, microhardness 1150 HM, phosphorus content in coating 7.5% by weight.
Příklad 2 ,Example 2,
400 g/1 000 ml H2O fluoroboritanu nikelnatého, · g/1 000 ml H2O kyseliny borité, g/1 000 ml H2O fosfornanu sodného,400 g / 1 000 ml H2O nickel borohydride, · g / 1 000 ml H2O boric acid, g / 1 000 ml H2O sodium hypophosphite,
0,1 g/1 000 ml H2O lauryl-síranu sodného, katodová proudová hustota 1 až 8A/dm2, provozní teplota 50 °C, pH 2,4, ...........0.1 g / 1000 ml H2O sodium lauryl sulfate, cathode current density 1 to 8A / dm 2 , operating temperature 50 ° C, pH 2.4, ...........
mikrotvrdost 950 HM, obsah fosforu v povlaku 5,4 % hmotnostních.microhardness 950 HM, phosphorus content in coating 5.4% by weight.
Příkladě. 3Example. 3
400 g/1 000 ml H2O .;400 g / 1000 ml H2O.
fluoroboritanu nikelnatého · g/1 000 · ml H2O·.'· kyseliny borité ?20 g/1 000 ml H2O kyseliny fosforitůnickel fluoroborate · g / 1000 · ml H2O · · · boric acid 20 g / 1000 ml H2O phosphorous acid
0,1 g/1 000 ml H2O diisopropyl-naftalen-sulfonanu sodného katodová proudová hustota 1 až 10A'dm2 provozní teplota ' 50 °C pH 2,1 mikrotvrdost 1010 HM obsah fosforu v · povlaku 9,5 °/o hmotnostních0.1 g / 1000 ml H2O sodium diisopropyl-naphthalene sulfonate cathode current density 1 to 10A'dm 2 operating temperature '50 ° C pH 2.1 microhardness 1010 HM phosphorus content · coating 9.5% / w / w
Claims (2)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS84902A CS240582B1 (en) | 1984-02-08 | 1984-02-08 | Electrolytic aqueous bath for nickel-phosphorus alloy deposition |
| DE19853504186 DE3504186A1 (en) | 1984-02-08 | 1985-02-07 | Electrolytic water bath and process for depositing a nickel-phosphorus alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS84902A CS240582B1 (en) | 1984-02-08 | 1984-02-08 | Electrolytic aqueous bath for nickel-phosphorus alloy deposition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS90284A1 CS90284A1 (en) | 1985-07-16 |
| CS240582B1 true CS240582B1 (en) | 1986-02-13 |
Family
ID=5342071
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS84902A CS240582B1 (en) | 1984-02-08 | 1984-02-08 | Electrolytic aqueous bath for nickel-phosphorus alloy deposition |
Country Status (2)
| Country | Link |
|---|---|
| CS (1) | CS240582B1 (en) |
| DE (1) | DE3504186A1 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5032464A (en) * | 1986-10-27 | 1991-07-16 | Burlington Industries, Inc. | Electrodeposited amorphous ductile alloys of nickel and phosphorus |
| US4801947A (en) * | 1987-06-25 | 1989-01-31 | Burlington Industries, Inc. | Electrodeposition-produced orifice plate of amorphous metal |
| WO1994027302A1 (en) * | 1993-05-14 | 1994-11-24 | Kiyokawa Mekki Kougyo Co., Ltd | Metallic film resistor having fusing function and method for its manufacture |
| US6099624A (en) * | 1997-07-09 | 2000-08-08 | Elf Atochem North America, Inc. | Nickel-phosphorus alloy coatings |
-
1984
- 1984-02-08 CS CS84902A patent/CS240582B1/en unknown
-
1985
- 1985-02-07 DE DE19853504186 patent/DE3504186A1/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| CS90284A1 (en) | 1985-07-16 |
| DE3504186A1 (en) | 1985-08-08 |
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