DE2658003C3 - Bad für die elektrolytische Abscheidung von Zinn-Gold-Legierungen - Google Patents
Bad für die elektrolytische Abscheidung von Zinn-Gold-LegierungenInfo
- Publication number
- DE2658003C3 DE2658003C3 DE2658003A DE2658003A DE2658003C3 DE 2658003 C3 DE2658003 C3 DE 2658003C3 DE 2658003 A DE2658003 A DE 2658003A DE 2658003 A DE2658003 A DE 2658003A DE 2658003 C3 DE2658003 C3 DE 2658003C3
- Authority
- DE
- Germany
- Prior art keywords
- tin
- bath
- bath according
- gold
- complex
- 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
- 230000008021 deposition Effects 0.000 title claims description 5
- JVPLOXQKFGYFMN-UHFFFAOYSA-N gold tin Chemical group [Sn].[Au] JVPLOXQKFGYFMN-UHFFFAOYSA-N 0.000 title claims description 5
- 229910001020 Au alloy Inorganic materials 0.000 title claims description 3
- 239000003353 gold alloy Substances 0.000 title claims description 3
- -1 halide ions Chemical class 0.000 claims description 21
- 239000010931 gold Substances 0.000 claims description 19
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 16
- 239000003513 alkali Substances 0.000 claims description 7
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 claims description 7
- 150000004820 halides Chemical class 0.000 claims description 6
- 229910052736 halogen Inorganic materials 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- WOFVPNPAVMKHCX-UHFFFAOYSA-N N#C[Au](C#N)C#N Chemical compound N#C[Au](C#N)C#N WOFVPNPAVMKHCX-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims 1
- 150000002191 fatty alcohols Chemical class 0.000 claims 1
- 229910052718 tin Inorganic materials 0.000 description 16
- 229910052737 gold Inorganic materials 0.000 description 12
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- SYRHIZPPCHMRIT-UHFFFAOYSA-N tin(4+) Chemical compound [Sn+4] SYRHIZPPCHMRIT-UHFFFAOYSA-N 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical class Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229940071182 stannate Drugs 0.000 description 3
- HSJKGGMUJITCBW-UHFFFAOYSA-N 3-hydroxybutanal Chemical compound CC(O)CC=O HSJKGGMUJITCBW-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 150000001447 alkali salts Chemical class 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 235000011167 hydrochloric acid Nutrition 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 2
- 229940081974 saccharin Drugs 0.000 description 2
- 235000019204 saccharin Nutrition 0.000 description 2
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 125000005402 stannate group Chemical group 0.000 description 2
- 229960003080 taurine Drugs 0.000 description 2
- 150000003606 tin compounds Chemical class 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- ZXHCSYLXFAZWOL-UHFFFAOYSA-N 6-ethyl-6-methylcyclohexa-2,4-dien-1-amine Chemical compound CCC1(C)C=CC=CC1N ZXHCSYLXFAZWOL-UHFFFAOYSA-N 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000005228 aryl sulfonate group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 description 1
- RNFNDJAIBTYOQL-UHFFFAOYSA-N chloral hydrate Chemical compound OC(O)C(Cl)(Cl)Cl RNFNDJAIBTYOQL-UHFFFAOYSA-N 0.000 description 1
- 229960002327 chloral hydrate Drugs 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- SMVRDGHCVNAOIN-UHFFFAOYSA-L disodium;1-dodecoxydodecane;sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O.CCCCCCCCCCCCOCCCCCCCCCCCC SMVRDGHCVNAOIN-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 150000002344 gold compounds Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000010952 in-situ formation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- KUDPGZONDFORKU-UHFFFAOYSA-N n-chloroaniline Chemical compound ClNC1=CC=CC=C1 KUDPGZONDFORKU-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 229910001432 tin ion Inorganic materials 0.000 description 1
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical class [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/60—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of tin
-
- 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
- C25D3/62—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of gold
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)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US05/644,236 US4013523A (en) | 1975-12-24 | 1975-12-24 | Tin-gold electroplating bath and process |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DE2658003A1 DE2658003A1 (de) | 1977-07-07 |
| DE2658003B2 DE2658003B2 (de) | 1980-11-27 |
| DE2658003C3 true DE2658003C3 (de) | 1982-01-21 |
Family
ID=24584032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE2658003A Expired DE2658003C3 (de) | 1975-12-24 | 1976-12-21 | Bad für die elektrolytische Abscheidung von Zinn-Gold-Legierungen |
Country Status (12)
| Country | Link |
|---|---|
| US (1) | US4013523A (enExample) |
| JP (1) | JPS608315B2 (enExample) |
| BE (1) | BE849410A (enExample) |
| CA (1) | CA1075191A (enExample) |
| CH (1) | CH603826A5 (enExample) |
| DE (1) | DE2658003C3 (enExample) |
| ES (1) | ES454476A1 (enExample) |
| FR (1) | FR2336496A1 (enExample) |
| GB (1) | GB1567200A (enExample) |
| IT (1) | IT1066698B (enExample) |
| NL (1) | NL164331C (enExample) |
| SE (1) | SE417728B (enExample) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4406419C1 (de) * | 1994-02-28 | 1995-04-13 | Heraeus Gmbh W C | Bad zum galvanischen Abscheiden von Silber-Gold-Legierungen |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3012999C2 (de) * | 1980-04-03 | 1984-02-16 | Degussa Ag, 6000 Frankfurt | Bad und Verfahren zur galvanischen Abscheidung von hochglänzenden und duktiler Goldlegierungsüberzügen |
| DE3347594A1 (de) * | 1983-01-04 | 1984-07-12 | Omi International Corp., Warren, Mich. | Bad zur galvanischen abscheidung einer verschleissfesten goldlegierung und verfahren zur abscheidung einer verschleissfesten goldlegierung unter verwendung dieses bades |
| US4470886A (en) * | 1983-01-04 | 1984-09-11 | Omi International Corporation | Gold alloy electroplating bath and process |
| DE3509367C1 (de) * | 1985-03-15 | 1986-08-14 | Degussa Ag, 6000 Frankfurt | Bad und Verfahren zur galvanischen Abscheidung von Gold/Zinn-Legierungsueberzuegen |
| DE3881520D1 (de) * | 1988-09-05 | 1993-07-08 | Cockerill Sambre Sa | Verfahren zur elektroplattierung zon zinn. |
| CH680370A5 (enExample) * | 1989-12-19 | 1992-08-14 | H E Finishing Sa | |
| DE4406434C1 (de) * | 1994-02-28 | 1995-08-10 | Heraeus Gmbh W C | Bad zum galvanischen Abscheiden von Gold-Zinn-Legierungen |
| US6544397B2 (en) * | 1996-03-22 | 2003-04-08 | Ronald Redline | Method for enhancing the solderability of a surface |
| USRE45842E1 (en) * | 1999-02-17 | 2016-01-12 | Ronald Redline | Method for enhancing the solderability of a surface |
| US6248228B1 (en) | 1999-03-19 | 2001-06-19 | Technic, Inc. And Specialty Chemical System, Inc. | Metal alloy halide electroplating baths |
| JP4392640B2 (ja) * | 2000-10-11 | 2010-01-06 | 石原薬品株式会社 | 非シアン系の金−スズ合金メッキ浴 |
| US20060237324A1 (en) * | 2003-05-21 | 2006-10-26 | Fred Hayward | Pulse plating process for deposition of gold-tin alloy |
| WO2005110287A2 (en) * | 2004-05-11 | 2005-11-24 | Technic, Inc. | Electroplating solution for gold-tin eutectic alloy |
| WO2006078549A1 (en) * | 2005-01-21 | 2006-07-27 | Technic, Inc. | Pulse plating process for deposition of gold-tin alloy |
| DE102005006982A1 (de) * | 2005-02-15 | 2006-08-17 | Basf Ag | Verwendung nichtionischer Tenside bei der Metallgewinnung durch Elektrolyse |
| US10260159B2 (en) * | 2013-07-05 | 2019-04-16 | The Boeing Company | Methods and apparatuses for mitigating tin whisker growth on tin and tin-plated surfaces by doping tin with gold |
| WO2019125951A1 (en) * | 2017-12-18 | 2019-06-27 | New Mexico Tech University Research Park Corporation | Tin-indium alloy electroplating solution |
| JP7349427B2 (ja) * | 2018-07-03 | 2023-09-22 | 株式会社Jcu | ３価クロムメッキ液およびこれを用いたクロムメッキ方法 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1905105A (en) * | 1930-02-20 | 1933-04-25 | Directors Of The University Of | Electrodeposition of tin-gold alloys |
| US3598706A (en) * | 1967-12-11 | 1971-08-10 | Trifari Krussman And Fishel In | Acid gold plating baths |
| CH494284A (fr) * | 1968-11-28 | 1970-07-31 | Sel Rex Corp | Procédé pour le dépôt électrolytique d'un alliage d'or avec au moins un autre métal commun et bain aqueux de placage pour la mise en oeuvre de ce procédé |
-
1975
- 1975-12-24 US US05/644,236 patent/US4013523A/en not_active Expired - Lifetime
-
1976
- 1976-12-14 BE BE173266A patent/BE849410A/xx not_active IP Right Cessation
- 1976-12-14 CA CA267,802A patent/CA1075191A/en not_active Expired
- 1976-12-15 FR FR7637803A patent/FR2336496A1/fr active Granted
- 1976-12-16 NL NL7613972.A patent/NL164331C/xx not_active IP Right Cessation
- 1976-12-16 CH CH1583076A patent/CH603826A5/xx not_active IP Right Cessation
- 1976-12-17 SE SE7614214A patent/SE417728B/xx unknown
- 1976-12-21 DE DE2658003A patent/DE2658003C3/de not_active Expired
- 1976-12-22 GB GB53549/76A patent/GB1567200A/en not_active Expired
- 1976-12-22 IT IT52736/76A patent/IT1066698B/it active
- 1976-12-22 ES ES454476A patent/ES454476A1/es not_active Expired
- 1976-12-24 JP JP51156097A patent/JPS608315B2/ja not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4406419C1 (de) * | 1994-02-28 | 1995-04-13 | Heraeus Gmbh W C | Bad zum galvanischen Abscheiden von Silber-Gold-Legierungen |
Also Published As
| Publication number | Publication date |
|---|---|
| ES454476A1 (es) | 1977-12-01 |
| NL164331C (nl) | 1980-12-15 |
| IT1066698B (it) | 1985-03-12 |
| GB1567200A (en) | 1980-05-14 |
| SE7614214L (sv) | 1977-06-25 |
| JPS5281032A (en) | 1977-07-07 |
| SE417728B (sv) | 1981-04-06 |
| NL164331B (nl) | 1980-07-15 |
| CA1075191A (en) | 1980-04-08 |
| NL7613972A (nl) | 1977-06-28 |
| FR2336496A1 (fr) | 1977-07-22 |
| US4013523A (en) | 1977-03-22 |
| BE849410A (fr) | 1977-06-14 |
| DE2658003A1 (de) | 1977-07-07 |
| CH603826A5 (enExample) | 1978-08-31 |
| FR2336496B1 (enExample) | 1981-07-24 |
| JPS608315B2 (ja) | 1985-03-01 |
| DE2658003B2 (de) | 1980-11-27 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| OD | Request for examination | ||
| C3 | Grant after two publication steps (3rd publication) | ||
| 8327 | Change in the person/name/address of the patent owner |
Owner name: OMI INTERNATIONAL CORP. (EINE GESELLSCHAFT N.D.GES |
|
| 8328 | Change in the person/name/address of the agent |
Free format text: HAUCK, H., DIPL.-ING. DIPL.-WIRTSCH.-ING., 8000 MUENCHEN SCHMITZ, W., DIPL.-PHYS. GRAALFS, E., DIPL.-ING., 2000 HAMBURG WEHNERT, W., DIPL.-ING., 8000 MUENCHEN DOERING, W., DIPL.-WIRTSCH.-ING. DR.-ING., PAT.-ANW., 4000 DUESSELDORF |
|
| 8339 | Ceased/non-payment of the annual fee |