GB1583923A - Electrodeposition of tin/nickel alloys - Google Patents
Electrodeposition of tin/nickel alloys Download PDFInfo
- Publication number
- GB1583923A GB1583923A GB1961978A GB1961978A GB1583923A GB 1583923 A GB1583923 A GB 1583923A GB 1961978 A GB1961978 A GB 1961978A GB 1961978 A GB1961978 A GB 1961978A GB 1583923 A GB1583923 A GB 1583923A
- Authority
- GB
- United Kingdom
- Prior art keywords
- nickel
- solution according
- tin
- solution
- electrodeposition
- 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
Links
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims description 21
- 238000004070 electrodeposition Methods 0.000 title claims description 11
- 229910000990 Ni alloy Inorganic materials 0.000 title claims description 8
- 229910001128 Sn alloy Inorganic materials 0.000 title claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- 238000007747 plating Methods 0.000 claims description 11
- 229920002873 Polyethylenimine Polymers 0.000 claims description 10
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 9
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 9
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 9
- 235000011150 stannous chloride Nutrition 0.000 claims description 9
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 8
- GPUMPJNVOBTUFM-UHFFFAOYSA-N naphthalene-1,2,3-trisulfonic acid Chemical compound C1=CC=C2C(S(O)(=O)=O)=C(S(O)(=O)=O)C(S(=O)(=O)O)=CC2=C1 GPUMPJNVOBTUFM-UHFFFAOYSA-N 0.000 claims description 8
- 239000001119 stannous chloride Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- 239000011135 tin Substances 0.000 description 15
- 229910052718 tin Inorganic materials 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 238000007792 addition Methods 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- -1 ammonium fluoroborate Chemical compound 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- CLDVQCMGOSGNIW-UHFFFAOYSA-N nickel tin Chemical compound [Ni].[Sn] CLDVQCMGOSGNIW-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910017665 NH4HF2 Inorganic materials 0.000 description 1
- JQGGAELIYHNDQS-UHFFFAOYSA-N Nic 12 Natural products CC(C=CC(=O)C)c1ccc2C3C4OC4C5(O)CC=CC(=O)C5(C)C3CCc2c1 JQGGAELIYHNDQS-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 229940045713 antineoplastic alkylating drug ethylene imines Drugs 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- WDHWFGNRFMPTQS-UHFFFAOYSA-N cobalt tin Chemical compound [Co].[Sn] WDHWFGNRFMPTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 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)
Description
(54) ELECTRODEPOSITION OF TIN/NICKEL ALLOYS
(71) We, PMD CHEMICALS LIMITED, a British company, of Broad Lane, Coventry,
CV5 7AY, Warwickshire, do hereby declare the invention for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:
This invention relates to the electrodeposition of tin/nickel alloys and the like. While it is principally concerned with tin/ nickel alloys as such (particularly bright tin/ nickel alloys) and will be described with reference to such alloys, other elements such as cobalt may be co-deposited. Such a ternary system is described for example in U.S. Patent Specification 3,772,168.
Electrodeposition of tin/nickel alloys is known in the art and the above-mentioned U.S.
Specification is but one example of the several patent specifications in this field. There is also a general discussion in an article by Dillenburg entitled "Die Abscheidung von Zinn Nickel-Legieurungsniederschlägen" in Galvanotechnik D7963 Saulgau 63(1972) Nr.4 at pages 343-346. The basic Parkinson electrolyte referred to therein contains
250 g/l Nickel chloride
50 g/l Divalent Tin chloride
40 g/l NH4HF2 and is operated at a pH of 2.5 (adjusted with ammonia) and, fairly critically for a semi-bright finish, a temperature of 68-72"C. High temperatures and low pH's lead to corrosion and oxidation problems and one of the solutions to the problem is described in the above article namely a purely chloride electrolyte which can be used at a higher pH.
A further discussion of the prior art is set out in the above U.S. Patent which claims an electrolytic method for depositing corrosion resistant tin-nickel, tin-cobalt and tin-nickelcobalt coatings on a metal base comprising providing an aqueous acid bath at pH 3.8 to about 5.5 containing bivalent water soluble salts of nickel, tin and cobalt in amounts for nickel and cobalt equivalent to 125 to 450 grams per liter as bivalent nickel chloride and 25 to 110 grams per liter as stannous chloride, there being also present in said bath the combination of 20 to 100 grams per liter (1) alkali or ammonium fluoride or (2) alkali or ammonium fluoroborate with a non-volatile amine derivative reactive with said fluoride or fluoroborate to form the amine salt thereof, the amine of said amine salt being present in an amount of from 40 to 100 cubic centimetres per liter; maintaining said bath at a temperature of about 40 to 90"C; and passing current through said bath at an average current intensity between 0.1 to 5 amperes per square decimeter using a nickel anode and providing said metal base as the cathode. The amine is said to give good throwing power and a bright finish and a number of amines are described particularly ethylene diamine and triethylenetetramine. However the polyethylene imines are all of low molecular weight and are used in relatively large amounts as pH adjusters.
According to the invention there is provided an aqueous solution for the simultaneous electrodeposition of tin and nickel, containing nickel and stannous ions and, in addition, a polyethylene imine having a molecular weight in the range 10,000 to 30,000 as a brightener.
The nickel and tin are preferably present as chloride but the fluorides, for example, could be used instead. Other preferred features of the basic solutions will be apparent from the above U.S. Patent.
Ethylene imines are conveniently prepared by copolymerising ethylene dichloride and ammonia and for the purposes of this invention the preferred molecular weight of the imine is about 20,000. The pH is desirably adjusted with ammonia to 4-6 preferably about 5.5.
Operating temperatures should be in the range 68-75"C.
Preferably ammonium bifluoride is present in an amount of at least 40 g/l, and the polyethylene imine in an amount from 0.01 to 0.03% by volume.
It has been found that naphthalene trisulfonic acid is particularly suitable as a stress reducer in the solutions of the invention.
The alloy may be deposited direct on copper and copper base alloys. On steel an undercoat of not less than 0.0003 in. (0.008 mm) of copper is recommended. Aluminium and zinc-base alloys should also be first plated with copper.
The plating tank is desirably of steel lined with rubber or plastic; however free sulphur and filler contents of the rubber should be low and plastics containing plasticiser are unsuitable.
The electrolyte is usually operated at 700C (158"F) and suitable heating methods are external water jacket steam coils or internal electric heaters cased in nickel. Piping, pumps and filters may be neoprene lined or of nickel. The electrolyte should be kept clear by filtration and cloth alone is unsuitable for a filter medium as it will not retain fine particle which cause pitting. Nickel anodes are preferably used with the tin content maintained by regular additions of stannous chloride (approximately 3.8 lib/1000 A hr depending on drag-out). Separate tin and nickel anodes can be used in the ratio 1:2 on the same anode circuit; the tin anodes must be bagged and withdrawn from the electrolyte when not in use, but nickel anodes should remain in the electrolyte.
The pH may be measured with narrow range indicator papers and adjusted by additions of hydrochloric acid or ammonia.
The stannous tin concentration should be maintained at the desired concentration; this concentration will tend to decrease with time due to oxidation to the stannic form. Adjustment is conveniently by addition of stannous chloride and ammonium bifluoride in equal amounts but they should be dissolved in water and brought into operating pH before adding to the main tank.
The nickel concentration may be maintained by additions of nickel chloride.
Purification of the bath can be carried out with activated carbon at 2 gpl and maintaining at 70"C for 2 hours then filtering. If contamination with metallic impurities is found, plating out overnight steel cathodes at 5 a.s.f. will purify the electolyte.
The tin nickel deposit has little self-smoothing action and its brightness will therefore depend on the quality of the surface to be plated, a bright deposit is obtained on a clean polished article.
Example
Composition of Bath
Tin chloride (SnCl2 2H20) - 50 g/l
Nickel chloride (NiC12 6H20) - 250 g/l
NH4F HF - 40 g/l
NH4 OH - 35 mls/l
Naphthalene trisulfonic acid (NTSA) - 0.2 g/l
Aripol S5 - 0.025%
(= 0.25 mls/litre)
Aripol S5 consists of a polyethylene imine based polymer as a 20% solution with a pH of approximately 7. This material is sold by Float Ore Ltd. of Uxbridge.
Procedure for making up the bath
A tank is filled with about half the required volume of demineralised water and heated to 65"C. The constituents are added in the following order:
1. Ammonium bifluoride
2. Ammonia
3. Stannous chloride
4. Nickel chloride
The solution is allowed to stand and is then carbon treated with 2 g/ l carbon at 65"C for three hours. It is then filtered. The pH of the solution is adjusted to 5.5 and the NTSA and Aripol S5 are added followed by water to make up to the required volume.
Operating Conditions
Temperature - 70"C pH - 5.5
Current density - Rack plating 10-40 A/ft2
Barrel plating 5-15 A/ft2
Plating rate - Rack plating 0.6,a/min at l8 A ft3
Barrel plating 7.5,u in 20 min at 10 A ft2
The composition of the alloy was 65 % Tin/ 35 % Nickel which corresponds to the equiatomic ratio and is achieved unless the electrolyte composition or the operating conditions are grossly out of balance.
A particular advantage obtainable using the electrodeposition method of the present invention is that a barrel plating technique can be used having conventional apparatus.
WHAT WE CLAIM IS: I. An aqueous solution for the simultaneous electrodeposition of tin and nickel. containing nickel and stannous ions and, in addition, a polyethylene imine having a molecular weight in the range 10,000 to 30,000 as a brightener.
2. A solution according to claim I wherein the polyethylene imine has a molecular weight of about 20,000.
3. A solution according to claim 1 or 2, wherein the amount of the polyethylene imine present is from 0.01 to 0.03% by volume.
4. A solution according to any preceding claim wherein the pH is in the range 4 - 6.
5. A solution according to claim 4 wherein the pH is about 5.5.
6. A solution according to claim 4 or 5 which contains ammonia as pH adjuster.
7. A solution according to any preceding claim which contains nickel chloride and stannous chloride.
8. A solution according to claim 7 which contains 125 - 450 g/l nickel chloride and 25 110 g/l stannous chloride.
9. A solution according to any preceding claim which contains at least 40 g/l ammonium bifluoride.
10. A solution according to any preceding claim, which also contains naphthalene trisulfonic acid.
11. A solution according to claim 10, wherein the amount of naphthalene trisulfonic acid is about 0.2 g/l.
12. A method for the simultaneous electrodeposition of tin and nickel in which there is employed a solution according to any preceding claim.
13. A method according to claim 12, wherein the solution is maintained at a temperature in the range 68-75"C.
14. A method according to claim 12 or 13 which employs a barrel plating process.
15. A method according to claim 12 substantially as hereinbefore described.
16. A tin/ nickel alloy electrodeposited by a method according to any one of claims 12 to 15.
**WARNING** end of DESC field may overlap start of CLMS **.
Claims (16)
- **WARNING** start of CLMS field may overlap end of DESC **.The composition of the alloy was 65 % Tin/ 35 % Nickel which corresponds to the equiatomic ratio and is achieved unless the electrolyte composition or the operating conditions are grossly out of balance.A particular advantage obtainable using the electrodeposition method of the present invention is that a barrel plating technique can be used having conventional apparatus.WHAT WE CLAIM IS: I. An aqueous solution for the simultaneous electrodeposition of tin and nickel. containing nickel and stannous ions and, in addition, a polyethylene imine having a molecular weight in the range 10,000 to 30,000 as a brightener.
- 2. A solution according to claim I wherein the polyethylene imine has a molecular weight of about 20,000.
- 3. A solution according to claim 1 or 2, wherein the amount of the polyethylene imine present is from 0.01 to 0.03% by volume.
- 4. A solution according to any preceding claim wherein the pH is in the range 4 - 6.
- 5. A solution according to claim 4 wherein the pH is about 5.5.
- 6. A solution according to claim 4 or 5 which contains ammonia as pH adjuster.
- 7. A solution according to any preceding claim which contains nickel chloride and stannous chloride.
- 8. A solution according to claim 7 which contains 125 - 450 g/l nickel chloride and 25 110 g/l stannous chloride.
- 9. A solution according to any preceding claim which contains at least 40 g/l ammonium bifluoride.
- 10. A solution according to any preceding claim, which also contains naphthalene trisulfonic acid.
- 11. A solution according to claim 10, wherein the amount of naphthalene trisulfonic acid is about 0.2 g/l.
- 12. A method for the simultaneous electrodeposition of tin and nickel in which there is employed a solution according to any preceding claim.
- 13. A method according to claim 12, wherein the solution is maintained at a temperature in the range 68-75"C.
- 14. A method according to claim 12 or 13 which employs a barrel plating process.
- 15. A method according to claim 12 substantially as hereinbefore described.
- 16. A tin/ nickel alloy electrodeposited by a method according to any one of claims 12 to 15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB1961978A GB1583923A (en) | 1978-05-15 | 1978-05-15 | Electrodeposition of tin/nickel alloys |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB1961978A GB1583923A (en) | 1978-05-15 | 1978-05-15 | Electrodeposition of tin/nickel alloys |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1583923A true GB1583923A (en) | 1981-02-04 |
Family
ID=10132393
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB1961978A Expired GB1583923A (en) | 1978-05-15 | 1978-05-15 | Electrodeposition of tin/nickel alloys |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB1583923A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4749626A (en) * | 1985-08-05 | 1988-06-07 | Olin Corporation | Whisker resistant tin coatings and baths and methods for making such coatings |
| EP1260614A1 (en) * | 2001-05-24 | 2002-11-27 | Shipley Co. L.L.C. | Tin plating |
-
1978
- 1978-05-15 GB GB1961978A patent/GB1583923A/en not_active Expired
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4749626A (en) * | 1985-08-05 | 1988-06-07 | Olin Corporation | Whisker resistant tin coatings and baths and methods for making such coatings |
| EP1260614A1 (en) * | 2001-05-24 | 2002-11-27 | Shipley Co. L.L.C. | Tin plating |
| US6797142B2 (en) | 2001-05-24 | 2004-09-28 | Shipley Company, L.L.C. | Tin plating |
| US7160629B2 (en) | 2001-05-24 | 2007-01-09 | Shipley Company, L.L.C. | Tin plating |
| CN1296521C (en) * | 2001-05-24 | 2007-01-24 | 希普列公司 | Composition and method for tinplating |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed | ||
| PCNP | Patent ceased through non-payment of renewal fee |