NL8104808A - ELECTROLYSIS BATH AND METHOD FOR QUICK DEPOSITION OF A NICKEL LAYER. - Google Patents
ELECTROLYSIS BATH AND METHOD FOR QUICK DEPOSITION OF A NICKEL LAYER. Download PDFInfo
- Publication number
- NL8104808A NL8104808A NL8104808A NL8104808A NL8104808A NL 8104808 A NL8104808 A NL 8104808A NL 8104808 A NL8104808 A NL 8104808A NL 8104808 A NL8104808 A NL 8104808A NL 8104808 A NL8104808 A NL 8104808A
- Authority
- NL
- Netherlands
- Prior art keywords
- electrolysis bath
- nickel
- electrolysis
- bath
- nickel layer
- Prior art date
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims description 30
- 238000005868 electrolysis reaction Methods 0.000 title claims description 21
- 229910052759 nickel Inorganic materials 0.000 title claims description 14
- 238000000034 method Methods 0.000 title claims description 4
- 230000008021 deposition Effects 0.000 title claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical group [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- SHHKMWMIKILKQW-UHFFFAOYSA-N 2-formylbenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1C=O SHHKMWMIKILKQW-UHFFFAOYSA-N 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- -1 potassium perfluoroalkyl sulfonates Chemical class 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 239000000080 wetting agent Substances 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims 2
- 125000005619 boric acid group Chemical group 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 3
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000003906 humectant Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- UPPLJLAHMKABPR-UHFFFAOYSA-H 2-hydroxypropane-1,2,3-tricarboxylate;nickel(2+) Chemical compound [Ni+2].[Ni+2].[Ni+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O UPPLJLAHMKABPR-UHFFFAOYSA-H 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- PXIGQZGKWPSHTM-UHFFFAOYSA-N molecular fluorine;potassium Chemical class [K].FF PXIGQZGKWPSHTM-UHFFFAOYSA-N 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- C25D3/12—Electroplating: Baths therefor from solutions of 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)
- Cosmetics (AREA)
Description
*· * -1-* · * -1-
VO 23ÖTVO 23ÖT
Elektrolysebad en werkwijze voor snelle afzetting van een nikkellaagElectrolysis bath and method for rapid deposition of a nickel layer
Het is in de bekledingstechniek bekend elektrolytische nikkellagen af te zetten onder toepassing van verbruikbare anoden.It is known in the coating art to deposit electrolytic nickel layers using consumable anodes.
De toepassing van verbruikbare anoden wordt voorgeschreven, omdat men overtuigd was, dat organische toevoegsels aan bet bad zouden 5 worden afgebroken bij aanwezigheid van niet verbruikbare anoden.The use of consumable anodes is prescribed because it was believed that organic bath additives would degrade in the presence of non-consumable anodes.
Bovendien is bekend, dat de spanningen in het afgezette nikkel ongunstig worden beïnvloed door de niet verbruikbare anoden. Om verschillende commerciële redenen zou het zeer gewenst zijn, niet oplosbare anoden te gebruiken in een elektrolys eb ad voor nikkel 10 zonder dat afbraak van toevoegsels optreedt of nikkellagen met spanning worden gevormd.Moreover, it is known that the stresses in the deposited nickel are adversely affected by the non-consumable anodes. For various commercial reasons, it would be highly desirable to use insoluble anodes in an electrolysis ad nickel 10 without degradation of additives or stressed nickel layers being formed.
Typische Amerikaanse octrooischriften betreffende elektrolytische afzettingen van nikkel zijn o.a. de Amerikaanse octrooischriften 2.228.991, 2.h09.119, 2Λ09.120, 2.U85.1U9 en 2.998.360.Typical U.S. patents related to nickel electrolytic deposits include U.S. Patents 2,228,991, 2h09,119, 2Λ09,120, 2U85.1U9, and 2,998,360.
15 Voorzover valt na te gaan hebben deze octrooien betrekking op de toepassing van gebruikelijke of gemodificeerde verbruikbare anoden.As far as can be ascertained, these patents relate to the use of conventional or modified consumable anodes.
Zie blz. 2, kolom 2, regels 53~6k van het Amerikaanse.oetrόσιε chrift 2.228.991. . ·See page 2, column 2, lines 53 ~ 6k of the United States publication 2,228,991. . ·
De uitvinding heeft betrekking op een nieuw en verbeterd 20 elektrolysebad voor toepassing van niet verbruikbare anoden en het kan worden bedreven met betrekkelijk grote elektrolysesnelheid onder vorming van nikkelafzettingen die betrekkelijk vrij zijn van spanningen. De niet verbruikbare anoden die bij de werkwijze volgens deze uitvinding kunnen worden gebruikt zijn voorbeeld geplatineerd 25 titaan, geplatineerd tantaal, geplatineerd niobium of platina zelf.The invention relates to a new and improved electrolysis bath for the use of non-consumable anodes and it can be operated at a relatively high electrolysis rate to form nickel deposits which are relatively free of stress. The non-consumable anodes that can be used in the method of this invention are, for example, platinum-plated titanium, platinum-plated tantalum, platinum-plated niobium, or platinum itself.
Bovendien kan men titaananoden gebruiken die bekleed zijn met oxyde-mengsels, zoals een mengsel van rutheniumoxyde en titaanoxyde.In addition, titanium anodes can be used which are coated with oxide mixtures, such as a mixture of ruthenium oxide and titanium oxide.
Het elektrolysebad volgens de uitvinding bevat een aantal verplichte toevoegsels, welke niet worden afgebroken bij bewerkingen 30 bij aanwezigheid van niet-verbruikbare anoden. Behalve een gebruikelijke nikkelbron bij voorbeeld nikkelsulfaat, en een geleidings-elektrolyt, zoals boorzuur, bevat het elektrolysebad orthoformyl-__ benzeensulfonzuur als glansmiddel en een mengsel van kaliuuroerfluor- 810480¾ ~ - ·> -2- alkylsulfonaten, dat o.a. in de handel is onder de naam FC98, als bevochtigingsmiddel.The electrolysis bath of the invention contains a number of mandatory additives, which are not degraded in operations in the presence of non-consumable anodes. In addition to a conventional nickel source, for example, nickel sulfate, and a conductive electrolyte such as boric acid, the electrolysis bath contains orthoformyl benzene sulfonic acid as a brightener and a mixture of potassium fluorine fluorides, which are, inter alia, commercially available under the name FC98, as a humectant.
In het algemeen zullen de elektrolysebaden volgens de uitvinding als volgt zijn samengesteld: 5 Component Concentratie (g/l)In general, the electrolysis baths according to the invention will be composed as follows: 5 Component Concentration (g / l)
Nikkelzout _30 tot 105 (als Ni)Nickel salt _30 to 105 (as Ni)
Elektrolyt .20 tot 100 O-formylbenzeensulfonzuur 0,25 tot 390 FC 98 0,02 tot 0,2 10 De bij voorkeur gebruikte bronnen voor nikkel zijn nikkel- sulfaat:,. nikkelcitraat, nikkelcarbonaat en dergelijke. Deze zouten worden bij voorkeur gebruikt in een hoeveelheid van 135-^70 g/l om de gewenste concentratie aan nikkelionen te verschaffen.Electrolyte .20 to 100 O-formylbenzene sulfonic acid 0.25 to 390 FC 98 0.02 to 0.2 The preferred sources of nickel are nickel sulfate. nickel citrate, nickel carbonate and the like. These salts are preferably used in an amount of 135-70 g / l to provide the desired concentration of nickel ions.
De elektrolyten, die voor de uitvinding het meest nuttig 15 zijn, zijn boorzuur, citroenzuur, en dergelijke. De bij voorkeur .The electrolytes most useful for the invention are boric acid, citric acid, and the like. The preferred.
in de elektrolysebaden volgens de uitvinding gebruikte hoeveelheden . ' . - ’zullen liggen tussen ongeveer 22,5.en ^5 g/l. Toepassing van ‘ i · · boorzuur heeft bijzonder de voorkeur.amounts used in the electrolysis baths according to the invention. ". - "will be between about 22.5. And ^ 5 g / l. The use of "i · · boric acid is particularly preferred.
• μ De organische componenten van het bad zijn gewoonlijk de .• μ The organic components of the bath are usually the.
20 glansmiddelen en de bevochtigingsmiddelen. In het elektrolysebad' volgens de uitvinding, .wordt als glansmiddel orthoformylbenzeen- sulf onzuur gebruikt. Het gebruikte bevochtigingsmi ddel is FC9Ö, : ï.20 brighteners and the wetting agents. In the electrolysis bath according to the invention, orthoformylbenzenesulfonic acid is used as the brightener. The humectant used is FC9Ö,: ï.
een produkt, dat in de handel wordt gebracht door Minnesota Mining and Manufacturing Co. of prodükten met gelijkwaardige samenstelling.a product marketed by Minnesota Mining and Manufacturing Co. or products of equivalent composition.
" · - .· 25 . Voor de meeste doeleinden wordt de pH van het elektrolysebad ' ' i . : . . . · ' , ’··.’. ' -; · ingesteld op 2-5 en bij. voorkeur op 2,5-4,5. De verbindingen, die ^ ·! ' -- ‘ - · ' · ï worden gebruikt om de pH' in te stellen omvatten nikkelcarbonaat’, zwavelzuur, kaliumnitraat of citroenzuur. . 'For most purposes, the pH of the electrolysis bath '' i.:... · ',' ··. '.' -; 5-4.5 The compounds which are used to adjust the pH include nickel carbonate, sulfuric acid, potassium nitrate or citric acid.
De elektrolysebaden volgens de uitvinding worden bedreven , - o .. ..The electrolysis baths according to the invention are operated, - o .. ..
30 bij een temperatuur van ongeveer 46-57 C-en bij betrekkelijk grote 2 2 stroomdichtheid, tot aan 108 Amp/dm en bij voorkeur van 10,8-65 Amp/dm .30 at a temperature of about 46-57 ° C and at a relatively large 2 2 current density, up to 108 Amp / dm and preferably from 10.8-65 Amp / dm.
. De mogelijkheid dergelijke grote stroomdichtheden toe te passen is een ander belangrijk voordeel van de elektrolysebaden volgens de uitvinding. ' / 35 De nikkellagen, welke onder toepassing van de baden volgens ".’8 1 0 4 8 0 8 ~~~ : “ ; - «ί’ * -3- de uitvinding worden af gezet op verschillende substraten onderscheiden zich doordat ze half glanzend en ductiel zijn en weinig spanning vertonen. lot dusver was het nodig, verbruikbare anoden te getruiken om dergelijke eigenschappen te verkrijgen.. The ability to use such high current densities is another important advantage of the electrolysis baths of the invention. The nickel layers deposited on the various substrates are distinguished by using the baths according to the invention. be glossy and ductile and exhibit little stress, it has previously been necessary to use consumable anodes to obtain such properties.
5 De uitvinding wordt toegelicht door het volgende voorbeeld.The invention is illustrated by the following example.
VoorbeeldExample
Een elektrolysebad werd bereid met de volgende samenstelling:An electrolysis bath was prepared with the following composition:
Componenten Concentratie g/lComponents Concentration g / l
Nikkelsulfaat 75 (als Ni) 10 Boor zuur ' 1*0 O-formylbenzeensulfonzuur 1,5 FC 98* *FC98 is een mengsel van kaliumperfluoralkjclsulfonaten.Nickel sulfate 75 (as Ni) 10 Boric acid 1 * 0 O-formylbenzene sulfonic acid 1.5 FC 98 * * FC98 is a mixture of potassium perfluoroalkyl sulfonates.
V66r gebruik van het bad werd voldoende nikkelcarbonaat 15 toegevoegd om de pE te brengen op ongeveer 2,5. Daarna werd ' het bad gebruikt om koper te bekleden bij 55°C en bij ' / 2 f 5,1* arnp/dm in een gebruikelijke elektrolyse-inrichting met geplati- neerde titaananoden. De gevormde nikkellaag was halfglanzend en ductiel. Verdere analyse toonde aan, dat weinig spanningen aanwezig 20 waren. Bij de toepassing van dit bad werd praktisch geen afbraak van de organische bestanddelen van het bad waargenomen.Before using the bath, sufficient nickel carbonate 15 was added to bring the pE to about 2.5. Thereafter, the bath was used to coat copper at 55 ° C and at about 5.1% arnp / dm in a conventional electrolyser with plated titanium anodes. The nickel layer formed was semi-gloss and ductile. Further analysis showed that few voltages were present. When using this bath, practically no degradation of the organic constituents of the bath was observed.
Het zal duidelijk zijn, dat dit voorbeeld kan worden gevarieerd en gemodificeerd zonder af te wijken van de uitvindings-gedachte. ^ ’ ΤΠΠΤίΓδ- - ~ 'It will be clear that this example can be varied and modified without departing from the inventive idea. ^ ’ΤΠΠΤίΓδ- - ~”
Claims (4)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US19989480A | 1980-10-23 | 1980-10-23 | |
| US19989480 | 1980-10-23 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| NL8104808A true NL8104808A (en) | 1982-05-17 |
Family
ID=22739453
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NL8104808A NL8104808A (en) | 1980-10-23 | 1981-10-23 | ELECTROLYSIS BATH AND METHOD FOR QUICK DEPOSITION OF A NICKEL LAYER. |
Country Status (15)
| Country | Link |
|---|---|
| JP (1) | JPS6020475B2 (en) |
| AU (1) | AU527954B2 (en) |
| BE (1) | BE890836A (en) |
| BR (1) | BR8106819A (en) |
| CA (1) | CA1180677A (en) |
| CH (1) | CH649579A5 (en) |
| DE (1) | DE3139641C2 (en) |
| DK (1) | DK422181A (en) |
| ES (1) | ES8302802A1 (en) |
| FR (1) | FR2492849A1 (en) |
| GB (1) | GB2085924B (en) |
| HK (1) | HK66786A (en) |
| IT (1) | IT1171598B (en) |
| NL (1) | NL8104808A (en) |
| SE (1) | SE8106250L (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1162505A (en) * | 1980-10-31 | 1984-02-21 | Donald R. Rosegren | Process for high speed nickel and gold electroplate system |
| US4543166A (en) * | 1984-10-01 | 1985-09-24 | Omi International Corporation | Zinc-alloy electrolyte and process |
| JP4904933B2 (en) * | 2005-09-27 | 2012-03-28 | 日立電線株式会社 | Nickel plating solution and manufacturing method thereof, nickel plating method and copper foil for printed wiring board |
| KR102281132B1 (en) * | 2019-10-24 | 2021-07-26 | 일진머티리얼즈 주식회사 | Electrolytic Nickel Foil for Thin Film-type Capacitor and Production Method of the Same |
| CN112323096A (en) * | 2020-09-23 | 2021-02-05 | 河北东恩企业管理咨询有限公司 | Preparation method of sulfur-nickel-containing round cake |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3334032A (en) * | 1964-05-08 | 1967-08-01 | Hanson Van Winkle Munning Co | Electrodeposition of nickel |
| US3697391A (en) * | 1970-07-17 | 1972-10-10 | M & T Chemicals Inc | Electroplating processes and compositions |
| ZA721964B (en) * | 1971-04-01 | 1972-12-27 | M & T Chemicals Inc | Nickel plating |
-
1981
- 1981-09-24 DK DK422181A patent/DK422181A/en not_active Application Discontinuation
- 1981-09-25 AU AU75676/81A patent/AU527954B2/en not_active Ceased
- 1981-09-25 CA CA000386693A patent/CA1180677A/en not_active Expired
- 1981-10-06 DE DE3139641A patent/DE3139641C2/en not_active Expired
- 1981-10-09 ES ES506173A patent/ES8302802A1/en not_active Expired
- 1981-10-13 JP JP56163363A patent/JPS6020475B2/en not_active Expired
- 1981-10-21 IT IT49529/81A patent/IT1171598B/en active
- 1981-10-22 BR BR8106819A patent/BR8106819A/en not_active IP Right Cessation
- 1981-10-22 FR FR8119853A patent/FR2492849A1/en active Granted
- 1981-10-22 BE BE0/206326A patent/BE890836A/en not_active IP Right Cessation
- 1981-10-22 SE SE8106250A patent/SE8106250L/en unknown
- 1981-10-22 CH CH6755/81A patent/CH649579A5/en not_active IP Right Cessation
- 1981-10-23 NL NL8104808A patent/NL8104808A/en not_active Application Discontinuation
- 1981-10-23 GB GB8132066A patent/GB2085924B/en not_active Expired
-
1986
- 1986-09-11 HK HK667/86A patent/HK66786A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| IT1171598B (en) | 1987-06-10 |
| CH649579A5 (en) | 1985-05-31 |
| DK422181A (en) | 1982-04-24 |
| DE3139641C2 (en) | 1986-07-31 |
| JPS5794589A (en) | 1982-06-12 |
| IT8149529A0 (en) | 1981-10-21 |
| BE890836A (en) | 1982-04-22 |
| FR2492849A1 (en) | 1982-04-30 |
| ES506173A0 (en) | 1983-01-16 |
| DE3139641A1 (en) | 1982-09-30 |
| HK66786A (en) | 1986-09-18 |
| AU527954B2 (en) | 1983-03-31 |
| CA1180677A (en) | 1985-01-08 |
| ES8302802A1 (en) | 1983-01-16 |
| BR8106819A (en) | 1982-07-06 |
| SE8106250L (en) | 1982-04-24 |
| GB2085924A (en) | 1982-05-06 |
| AU7567681A (en) | 1982-04-29 |
| GB2085924B (en) | 1983-06-02 |
| FR2492849B1 (en) | 1984-11-23 |
| JPS6020475B2 (en) | 1985-05-22 |
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