GB2266894A - Modified tin brightener for tin-zinc alloy electroplating bath - Google Patents
Modified tin brightener for tin-zinc alloy electroplating bath Download PDFInfo
- Publication number
- GB2266894A GB2266894A GB9223163A GB9223163A GB2266894A GB 2266894 A GB2266894 A GB 2266894A GB 9223163 A GB9223163 A GB 9223163A GB 9223163 A GB9223163 A GB 9223163A GB 2266894 A GB2266894 A GB 2266894A
- Authority
- GB
- United Kingdom
- Prior art keywords
- brightener
- tin
- approximately
- alcohol
- composition
- 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.)
- Withdrawn
Links
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 17
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910001297 Zn alloy Inorganic materials 0.000 title claims abstract description 8
- 238000009713 electroplating Methods 0.000 title description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 19
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- AXLMPTNTPOWPLT-UHFFFAOYSA-N prop-2-enyl 3-oxobutanoate Chemical compound CC(=O)CC(=O)OCC=C AXLMPTNTPOWPLT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003381 stabilizer Substances 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 4
- 238000004070 electrodeposition Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 3
- 235000010234 sodium benzoate Nutrition 0.000 claims description 3
- 239000004299 sodium benzoate Substances 0.000 claims description 3
- 235000010352 sodium erythorbate Nutrition 0.000 claims description 3
- 239000004320 sodium erythorbate Substances 0.000 claims description 3
- RBWSWDPRDBEWCR-RKJRWTFHSA-N sodium;(2r)-2-[(2r)-3,4-dihydroxy-5-oxo-2h-furan-2-yl]-2-hydroxyethanolate Chemical compound [Na+].[O-]C[C@@H](O)[C@H]1OC(=O)C(O)=C1O RBWSWDPRDBEWCR-RKJRWTFHSA-N 0.000 claims description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 7
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 abstract description 4
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005282 brightening Methods 0.000 abstract description 3
- FFSAXUULYPJSKH-UHFFFAOYSA-N butyrophenone Chemical compound CCCC(=O)C1=CC=CC=C1 FFSAXUULYPJSKH-UHFFFAOYSA-N 0.000 abstract description 3
- 235000016337 monopotassium tartrate Nutrition 0.000 abstract description 3
- KYKNRZGSIGMXFH-ZVGUSBNCSA-M potassium bitartrate Chemical compound [K+].OC(=O)[C@H](O)[C@@H](O)C([O-])=O KYKNRZGSIGMXFH-ZVGUSBNCSA-M 0.000 abstract description 3
- 239000003755 preservative agent Substances 0.000 abstract description 3
- 230000002335 preservative effect Effects 0.000 abstract description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- NXPHCVPFHOVZBC-UHFFFAOYSA-N hydroxylamine;sulfuric acid Chemical compound ON.OS(O)(=O)=O NXPHCVPFHOVZBC-UHFFFAOYSA-N 0.000 abstract 1
- -1 n-propyl alcohol Chemical compound 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 239000001117 sulphuric acid Substances 0.000 abstract 1
- 235000009529 zinc sulphate Nutrition 0.000 abstract 1
- 239000011686 zinc sulphate Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 239000000470 constituent Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- ZNBNBTIDJSKEAM-UHFFFAOYSA-N 4-[7-hydroxy-2-[5-[5-[6-hydroxy-6-(hydroxymethyl)-3,5-dimethyloxan-2-yl]-3-methyloxolan-2-yl]-5-methyloxolan-2-yl]-2,8-dimethyl-1,10-dioxaspiro[4.5]decan-9-yl]-2-methyl-3-propanoyloxypentanoic acid Chemical compound C1C(O)C(C)C(C(C)C(OC(=O)CC)C(C)C(O)=O)OC11OC(C)(C2OC(C)(CC2)C2C(CC(O2)C2C(CC(C)C(O)(CO)O2)C)C)CC1 ZNBNBTIDJSKEAM-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 229910000378 hydroxylammonium sulfate Inorganic materials 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 229940123973 Oxygen scavenger Drugs 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 239000013504 Triton X-100 Substances 0.000 description 1
- 229920004890 Triton X-100 Polymers 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229920002113 octoxynol Polymers 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000080 wetting agent 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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/60—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of tin
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)
Abstract
The brightener comprises an aqueous solution containing acetaldehyde and formaldehyde as primary brightener, an alcohol such as n-propyl alcohol, a surfactant and one component of a conventional two-part tin brightener as a secondary brightener. The modified brightener is suitable for use as a brightener in the deposition of tin-zinc alloys. The function of the other component of the tin brightener is accomplished by the formaldehyde and acetaldehyde. The problem of imbalance of the two components which can adversely affect brightening is thereby avoided. The tin brightener component may be a mixture of methanol, glycolated ethylene oxide, sulphuric acid, potassium acid tartrate, butyrophenone, zinc sulphate and hydroxylamine sulphate. The composition may also include allylacetoacetate as a preservative and additional stabilizing agents.
Description
TIN-ZINC ALLOY BRIGETENER BACKGROUND OF THE INVENTION AFIELD OF THE INVENTION
This invention relates generally to the field of electroplating alloys of tin and zinc, and specifically to a brightener for use in a tin-zinc plating bath.
BACKGROUND ART
Brighteners are widely used in electroplating processes to provide a pleasing decorative finish to the electrodeposited metal. In particular, there are numerous commercially available brighteners for use in conventional tin plating processes.
However, such brighteners do not affect the brightness of zinc, and thus their use with a tin-zinc alloy will result in a deposit having a mottled granular appearance.
The present invention provides an aqueous brightener for the electrodeposition of tin-zinc alloys and one that is particularly useful in a sulfuric acid-based plating solution.
S'-1JDSARY OF THE INVENTION
The brightener of the present invention comprises an aqueous sclution of acetaldehyde, formaldehyde, an alcohol such an npropyl alcohol, a surfactant and one component of a conventional tin brightener. The composition may also include allylacetoacetate as a preservative and additional stabilizing agents.
DETAILED DESCRIPTION OF THE INVENTION
In the following description, for purposes of explanation and not limitation, specific substances, concentrations, etc. are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well known processes are omitted so as to not obscure the description of the present invention with unnecessary detail.
The preferred brightener composition contains (1) acetaldehyde, (2) formaldehyde, (3) alcohol, (4) a surfactant and (5) a tin brightener. Although not essential, the brightener preferably further includes allylacetoacetate and a stabilizing agent.
The relative concentrations of the constituent chemicals are set forth in Table 1 below, the balance of the composition comprising distilled or deionized water. Minimum, nominal and maximum values are given for the concentrations of each constituent. The nominal values are consistent with experimental results, and are known to provide satisfactory performance. It is believed that comparable performance may be achieved with concentrations anywhere within the indicated ranges or even beyond. Thus, this invention is not strictly limited to the values given.
TABLE 1
CONCENTRATION (Per liter) CONSTITUENT MINIMUM NOMINAL MAXIMUM acetaldehyde 2 ml 30 ml 150 ml formaldehyde 5 ml 80 ml 250 ml alcohol 2 ml 30 ml 150 ml surfactant 1 ml 30 ml 150 ml tin brightener 50 ml 350 ml 700 ml allylaceto acetate 5g 50 g 200 stabilizer Per suDPlier's specifications n-propyl alcohol is suitable for use as the alcohol in the composition, however, any other common alcohol may be substituted therefor.
The surfactant of the preferred composition is Triton X 1 Triton X-100" is a trademark of Rohm & Haas Company designating a surfactant based on alkylaryl polyether alcohols, sulfonates and sulfates.
The acetaldehyde and formaldehyde act as a primary brightener for the tin-zinc deposit, breaking the granular structure throughout a current density range of approximately 1-100 ASF.
Any conventional tin brightener may be used as a secondary brightener component, giving a lustrous plated appearance to the tin-zinc deposit. Only one component of a conventional two part tin brightener is used in the subject composition, the function of the other component being accomplished by the addition of formaldehyde and acetaldehyde. This avoids a problem frequently encountered with the use of conventional two-part tin brighteners, whereby an imbalance of the two components may adversely affect te brightening of the deposit or may stop the plating process altogether.
A typical tin brightener suitable for use with the present invention is a composition of methanol, glycolated ethylene oxide, sulfuric acid, potassium acid tartrate, butyrophenone, zinc sulfate, and hydroxylamine sulfate. The potassium acid tartrate acts as a primary brightener and the methanol improves wetability.
Glycolated ethylene oxide, a non-ionic surfactant and wetting agent, also assists as a secondary component of the brightener system. The zinc sulfate is used as a catalyst and the butyrophenone as an anti-oxidant to the chelating agents. The sulfuric acid is a pH adjuster, and the hydroxylamine sulfate is the oxygen scavenger for the brightener system preventing age discoloration.
Allylacetoacetate is preferably added to the composition as indicated in Table 1. Although not essential, this chemical acts as a preservative to extend the shelf-life of the brightener composition. Furthermore, most conventional tin brighteners contain benzolodene acetone, and allylacetoacetate assists in keeping this chemical in solution. In addition, allylacetoacetate is, by nature, a cleaning agent and assists in improving adhesion of the deposited alloy.
A stabilizing agent or antioxidant is preferably added to the composition to prevent the brightener from aging and/or discoloring. Any one of the following or similar chemicals may be added as the stabilizing agent: butyl hydroxytoluene (BHT), sodium benzoate, sodium erythorbate, hydroquinone and p hi-droxybenzonic acid ester. Of these, hydroquinone is also a reducing agent and will act as an additional brightening component.
The brightener of the present invention is preferably prepared by combining the acetaldehyde, formaldehyde and alcohol with an appropriate amount of distilled or deionized water while stirring continuously. The surfactant and allylacetoacetate are then added to the solution, followed by the selected tin brightener and stabilizing agent, while continuing to stir the mixture. The brightener as thus prepared has a shelf-life in the range of approximately 6 months to 1 year.
The brightener of the present invention is useful for a wide range of tin-zinc alloys ranging from approximately 98% tin-2% zinc which is widely used for electrical applications to aproximately 75% tin-25% zinc which offers a high degree of corrosion resistance.
It will be recognized that the above described invention may be embodied in other specific forms without departing from the spirit or essential characteristics of the disclosure. Thus it is understood that the invention is not to be limited by the foregoing illustrative examples except as set forth in the claims.
Claims (9)
1. An aqueous brightener for the electrodeposition of tinzinc alloy comprising:
(a) approximately 2-150 ml/l acetaldehyde;
(b) approximately 5-250 ml/l formaldehyde;
(c) approximately 2-150 ml/l alcohol;
(d) approximately 1-150 ml/l surfactant;
(e) approximately 50-700 ml/l tin brightener.
2. The composition of claim 1 further comprising approximately 5-200 g/l allylacetoacetate.
3. The composition of claim 2 further comprising a stabilizing agent selected from the group consisting of butyl hydroxytoluene, sodium benzoate, sodium erythorbate, hydroquinone and p-hydroxybenzonic acid ester.
4. The composition of claim 1 wherein the alcohol is npropyl alcohol.
5. An aqueous brightener for the electrodeposition of tin znc alloy comprising:
(a) approximately 30 ml/l acetaldehyde;
(b) approximately 80 ml/l formaldehyde;
(c) approximately 30 ml/l alcohol;
(d) approximately 30 ml/l surfactant;
(e) approximately 350 ml/l tin brightener.
6. The composition of claim 5 further comprising approximately 50 g/l allylacetoacetate.
7. The composition of claim 6 further comprising a stabilizing agent selected from the group consisting of butyl hydroxytoluene, sodium benzoate, sodium erythorbate, hydroquinone & d p-hydroxybenzonic acid ester.
8. The composition of claim 5 wherein the alcohol is npropyl alcohol.
9. An aqueous brightener for the electrodeposition of tin-zinc alloy substantially as hereinbefore described.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US88309792A | 1992-05-15 | 1992-05-15 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB9223163D0 GB9223163D0 (en) | 1992-12-16 |
| GB2266894A true GB2266894A (en) | 1993-11-17 |
Family
ID=25381978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB9223163A Withdrawn GB2266894A (en) | 1992-05-15 | 1992-11-04 | Modified tin brightener for tin-zinc alloy electroplating bath |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2266894A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000029645A3 (en) * | 1998-11-12 | 2000-09-14 | Schloetter Fa Dr Ing Max | Aqueous solution for electrodepositing tin-zinc alloys |
| WO2001016403A1 (en) * | 1999-09-01 | 2001-03-08 | Merck Patent Gmbh | Galvanizing solution for the galvanic deposition of copper |
| EP1308541A1 (en) * | 2001-10-04 | 2003-05-07 | Shipley Company LLC | Plating bath and method for depositing a metal layer on a substrate |
| US6582582B2 (en) | 2001-03-09 | 2003-06-24 | Donald Becking | Electroplating composition and process |
| CN104357884A (en) * | 2014-11-14 | 2015-02-18 | 无锡伊佩克科技有限公司 | Method for plating zinc-tin alloy on ferrous material |
| CN105420764A (en) * | 2015-11-24 | 2016-03-23 | 安徽天思朴超精密模具股份有限公司 | Plating solution brightener material composition and preparation method of plating solution brightener |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5179643A (en) * | 1975-01-07 | 1976-07-12 | Tokyo Shibaura Electric Co | KOTAKUSUZUMETSUKYOKU |
| GB2064585A (en) * | 1979-11-19 | 1981-06-17 | Enthone | Acid Zinc Electroplating Solutions and Method Utilizing Ethoxylated/Propoxylated Polyhydric Alcohols |
| US4428803A (en) * | 1981-02-25 | 1984-01-31 | Omi International Corporation | Baths and processes for electrodepositing alloys of colbalt, tin and/or zinc |
| JPH0219490A (en) * | 1988-07-07 | 1990-01-23 | Showa Alum Corp | Surface treatment of aluminum material |
-
1992
- 1992-11-04 GB GB9223163A patent/GB2266894A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5179643A (en) * | 1975-01-07 | 1976-07-12 | Tokyo Shibaura Electric Co | KOTAKUSUZUMETSUKYOKU |
| GB2064585A (en) * | 1979-11-19 | 1981-06-17 | Enthone | Acid Zinc Electroplating Solutions and Method Utilizing Ethoxylated/Propoxylated Polyhydric Alcohols |
| US4428803A (en) * | 1981-02-25 | 1984-01-31 | Omi International Corporation | Baths and processes for electrodepositing alloys of colbalt, tin and/or zinc |
| JPH0219490A (en) * | 1988-07-07 | 1990-01-23 | Showa Alum Corp | Surface treatment of aluminum material |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000029645A3 (en) * | 1998-11-12 | 2000-09-14 | Schloetter Fa Dr Ing Max | Aqueous solution for electrodepositing tin-zinc alloys |
| US6770185B2 (en) | 1998-11-12 | 2004-08-03 | Dr.-Ing. Max Schlotter Gmbh & Co. Kg | Aqueous solution for electrodepositing tin-zinc alloys |
| WO2001016403A1 (en) * | 1999-09-01 | 2001-03-08 | Merck Patent Gmbh | Galvanizing solution for the galvanic deposition of copper |
| US6858123B1 (en) | 1999-09-01 | 2005-02-22 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Galvanizing solution for the galvanic deposition of copper |
| US6582582B2 (en) | 2001-03-09 | 2003-06-24 | Donald Becking | Electroplating composition and process |
| EP1308541A1 (en) * | 2001-10-04 | 2003-05-07 | Shipley Company LLC | Plating bath and method for depositing a metal layer on a substrate |
| CN104357884A (en) * | 2014-11-14 | 2015-02-18 | 无锡伊佩克科技有限公司 | Method for plating zinc-tin alloy on ferrous material |
| CN105420764A (en) * | 2015-11-24 | 2016-03-23 | 安徽天思朴超精密模具股份有限公司 | Plating solution brightener material composition and preparation method of plating solution brightener |
Also Published As
| Publication number | Publication date |
|---|---|
| GB9223163D0 (en) | 1992-12-16 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |