EP1205582A1 - Verfahren zur elektrolytischen Abscheidung aus einer chromhaltigen Lösung - Google Patents
Verfahren zur elektrolytischen Abscheidung aus einer chromhaltigen Lösung Download PDFInfo
- Publication number
- EP1205582A1 EP1205582A1 EP00124672A EP00124672A EP1205582A1 EP 1205582 A1 EP1205582 A1 EP 1205582A1 EP 00124672 A EP00124672 A EP 00124672A EP 00124672 A EP00124672 A EP 00124672A EP 1205582 A1 EP1205582 A1 EP 1205582A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- electrolyte
- molybdenum
- acid
- added
- organic compound
- 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.)
- Granted
Links
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
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
-
- 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
-
- 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
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
- C25D3/10—Electroplating: Baths therefor from solutions of chromium characterised by the organic bath constituents used
Definitions
- chrome for surface finishing has long been in the Industry.
- the application range from thin layers for decorative purposes up to the formation of hard chrome layers.
- hard chrome plating is high hardness and wear resistance, resistance to chemical influences, corrosion resistance as well as high temperature resistance desirable benefits.
- the present invention is therefore based on the object of providing a method for producing an alloy which overcomes the disadvantages known in the prior art and ensures the production of a layer which is characterized by a comparison with the pure one Chrome layers are characterized by higher corrosion and especially chloride resistance, as well as a high gloss overall.
- the process is also intended to ensure high current yields.
- the invention is intended to propose an electrolyte for carrying out the method.
- the invention proposes one Deposit chromium alloy from an electrolyte, which in addition to chromium and Sulfuric acid also contains an isopolyanion-forming metal, e.g. Molybdenum, vanadium, tungsten or niobium.
- Molybdenum e.g. Molybdenum, vanadium, tungsten or niobium.
- molybdenum which in the form of molybdic acid or of molybdenum salts is added to the electrolyte.
- Chromium-molybdenum layers made from a sulfuric acid electrolyte are deposited, have low cracks with wide cracks, which from the Surface to the base material, which the Corrosion resistance deteriorates.
- the method according to the invention overcomes this disadvantage by adding an organic compound, especially by adding a sulfonic acid, as this increases the crack density clearly increased.
- the cracks with the inventive method deposited layers are therefore very fine and no longer reach to Base material. This affects the extremely advantageous Corrosion resistance and brings about a clear advantage with the deposited layers compared to the inventive method known chrome-molybdenum layers.
- the electrolyte can contain molybdic acid in an amount of 10 g / l be added up to the solubility limit.
- the addition of 50-70 g / l molybdic acid has proven to be particularly advantageous.
- the Electrolyte chromic acid in an amount of 100 g / l to 400 g / l depending on the desired installation rate.
- the electrolyte has catalyzing Sulfuric acid in a quantity range from 1 g / l to 6 g / l, although it preferably contains 2 g / l.
- the organic compound comes with a concentration of over 0.1 g / l added to the electrolyte, has been found to be particularly advantageous proved an amount of 2 g / l.
- halide preferably complex halides can be added.
- the method according to the invention advantageously enables the Operating parameters electrolyte composition, electrolyte temperature and / or Current density set depending on the desired molybdenum incorporation rate can be. In this way, depending on the respective requirements inventive coating can be provided.
- electrolytically deposited chromium-molybdenum alloy layers Molybdenum incorporation rate between 0.1 wt .-% and 10 wt .-%. It turned out that optimized deposition results can be achieved when chrome and Sulfuric acid in a ratio of approx. 100: 1 and chromic and molybdic acid are contained in the electrolyte in a ratio of approx. 3: 1 to 4: 1.
- the electrolyte is connected to an external power source.
- the method according to the invention advantageously allows a wide current density working range while ensuring a very shiny layer deposition.
- Current can be supplied with a current density in the range from 5 A / dm 2 to at least 200 A / dm 2 , so that high-speed chrome plating is also possible without any problems.
- the method according to the invention advantageously enables a safe adhesive, corrosion-resistant and shiny layer with high cathodic To separate the current yield. This is preferably done with a cathodic Current efficiency of not less than 15%, preferably worked over 20%.
- a coating has proven to be particularly advantageous which is formed according to the invention at a current density working range of 20-50 A / dm 2 with a very shiny deposition and a molybdenum incorporation rate of 1%.
- an element of the VI main group can be added to the electrolyte become.
- This additive can be used as a salt or as a mixture thereof be added.
- the salt is e.g. Sulfates, halides, carbonates, chromates, Dichromates, oxides, hydroxides, acetates, sulfonates and compounds in which the element is present as an anion.
- the amount of additive is in a range of 0.25 mmol to 2.5 mol / l, but preferably less than or equal to 0.1 mol / l.
- the addition of selenium or tellurium has been particularly advantageous proved.
- the Amounts to be added to the individual catalysts can vary and depend depends on the bath composition and the deposition conditions.
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)
- Removal Of Specific Substances (AREA)
- Electrolytic Production Of Metals (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
Description
Claims (23)
- Verfahren zur Beschichtung von Werkstoffen, insbesondere von metallischen Werkstoffen, wobei zur Bildung einer Korrosions- und insbesondere Chloridbeständigen Schicht, die sich durch einen hohen Glanz auszeichnet, eine Chromlegierung aus einem Elektrolyten abgeschieden wird, der neben Chrom- und Schwefelsäure zumindest ein Isopolyanionen ausbildendes Metall sowie eine organische Verbindung enthält.
- Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Isopolyanionen ausbildende Metall Molybdän in Form von Molybdänsäure oder von Molybdänsalzen dem Elektrolyten zugesetzt wird.
- Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß dem Elektrolyten Molybdänsäure in einer Menge von 10 g/l bis zur Löslichkeitsgrenze hinzugegeben wird.
- Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß dem Elektrolyten Molybdänsäure in einer Menge von 50 g/l bis 70 g/l hinzugegeben wird.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 4, dadurch gekennzeichnet, daß als organische Verbindung eine kurzkettige aliphatische Sulfonsäure, deren Salze und/oder deren Halogenderivate dem Elektrolyten zugegeben werden.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die organische Verbindung in einer Konzentration von 0,1 g/l bis 10 g/l dem Elektrolyten hinzugefügt wird.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 6, dadurch gekennzeichnet, daß ca. 2 g/l der organischen Verbindung dem Elektrolyten zugesetzt wird.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 7, dadurch gekennzeichnet, daß Methansulfonsäure verwendet wird.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 8, dadurch gekennzeichnet, daß ein Zusatzstoff aus der VI Hauptgruppe als Salz oder anders geartete Mischung in einem Bereich von 0,25 mMol bis 2,5 Mol/l Elektrolyt dem Elektrolyten zugesetzt wird.
- Verfahren nach Anspruch 9, dadurch gekennzeichnet, daß Selen und/oder Tellur verwendet wird.
- Verfahren nach Anspruch 9 oder 10, dadurch gekennzeichnet, daß der Zusatzstoff in einer Menge von unter oder gleich 0,1 Mol/l Elektrolyt bezogen auf das jeweilige Element liegt.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 11, dadurch gekennzeichnet, daß die Bestromung mit einer Stromdichte in einem Bereich von 5 A/dm2 bis 200 A/dm2 durchgeführt wird.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 12, dadurch gekennzeichnet, daß die Bestromung mit einer Stromdichte von 20 A/dm2 bis 100A/dm2 erfolgt.
- Verfahren nach einem oder mehreren der obigen Ansprüche 1 bis 13, dadurch gekennzeichnet, daß die Molybdäneinbaurate einen Wert zwischen 0,1 Gew.-% und 10,0 Gew.-% aufweist.
- Verfahren nach einem oder mehreren der vorherigen Ansprüche 1 bis 14, dadurch gekennzeichnet, daß mit einer kathodischen Stromausbeute von nicht weniger als 15%, vorzugsweise von über 20%, gearbeitet wird.
- Verfahren nach einem oder mehreren der vorherigen Ansprüche 1 bis 15, dadurch gekennzeichnet, daß mit einer Badtemperatur von 20 bis 70°C gearbeitet wird.
- Verfahren nach einem oder mehreren der vorherigen Ansprüche 1 bis 16, dadurch gekennzeichnet, daß die Betriebsparameter Elektrolytzusammensetzung, Elektrolyttemperatur und/oder Stromdichte in Abhängigkeit der gewünschten Molybdäneinbaurate gewählt werden können.
- Elektrolyt zur Durchführung des Verfahrens nach einem der Ansprüche 1 bis 17 für die galvanische Abscheidung einer Chrom-Molybdän-Legierung, dadurch gekennzeichnet, daß dieser neben Chrom- und Schwefelsäure auch ein Isopolyanionen ausbildendes Metall in Form von Säure oder Salz oder einem anderen Derivat zusätzlich eine organische Verbindung aufweist.
- Elektrolyt nach Anspruch 18, dadurch gekennzeichnet, daß er Molybdän als Isopolyanionen ausbildendes Metall, sowie eine kurzkettige aliphatische Sulfonsäure, deren Salze und/oder deren Halogenderivate, als organische Verbindung enthält.
- Elektrolyt nach Anspruch 18 oder 19, dadurch gekennzeichnet, daß der Elektrolyt Chromsäure in einer Menge von 100 g/l bis 400 g/l enthält.
- Elektrolyt nach einem der Ansprüche 18 bis 20, dadurch gekennzeichnet, daß der Elektrolyt Schwefelsäure in einer Menge von 1 g/l bis 6 g/l enthält.
- Elektrolyt nach einem der Ansprüche 18 bis 21, dadurch gekennzeichnet, daß er einen Zusatzstoff aus der VI Hauptgruppe als Salz oder anders geartete Mischung in einem Bereich von 0,25 mMol bis 2,5 Mol/l Elektrolyt enthält.
- Chrom-Molybdän-Legierungsschicht, elektrolytisch abgeschieden gemäß dem Verfahren nach einem oder mehreren der Ansprüche 1 bis 17, dadurch gekennzeichnet, daß die Molybdäneinbaurate einen Wert zwischen 0,1 Gew.-% und 10,0 Gew.-% aufweist.
Priority Applications (13)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DK00124672T DK1205582T3 (da) | 2000-11-11 | 2000-11-11 | Fremgangsmåde til elektrolytisk udskillelse fra en chromholdig oplösning |
DE50015318T DE50015318D1 (de) | 2000-11-11 | 2000-11-11 | Verfahren zur elektrolytischen Abscheidung aus einer chromhaltigen Lösung |
EP00124672A EP1205582B1 (de) | 2000-11-11 | 2000-11-11 | Verfahren zur elektrolytischen Abscheidung aus einer chromhaltigen Lösung |
AT00124672T ATE405694T1 (de) | 2000-11-11 | 2000-11-11 | Verfahren zur elektrolytischen abscheidung aus einer chromhaltigen lösung |
ES00124672T ES2310985T3 (es) | 2000-11-11 | 2000-11-11 | Procedimiento para la deposicion electrolitica a partir de una solucion que contiene cromo. |
US10/169,959 US6837981B2 (en) | 2000-11-11 | 2001-11-03 | Chromium alloy coating and a method and electrolyte for the deposition thereof |
CNB018036236A CN1306069C (zh) | 2000-11-11 | 2001-11-03 | 用于沉积铬合金的方法 |
KR10-2002-7008837A KR100503210B1 (ko) | 2000-11-11 | 2001-11-03 | 크롬 합금을 적층하는 방법 |
CA002396946A CA2396946C (en) | 2000-11-11 | 2001-11-03 | Method for the deposition of a chromium alloy |
BR0107473-3A BR0107473A (pt) | 2000-11-11 | 2001-11-03 | Processo para precipitação de uma liga de cromo |
PCT/EP2001/012747 WO2002038835A1 (de) | 2000-11-11 | 2001-11-03 | Verfahren zur abscheidung einer chromlegierung |
EP01980543A EP1250472A1 (de) | 2000-11-11 | 2001-11-03 | Verfahren zur abscheidung einer chromlegierung |
JP2002541146A JP3873025B2 (ja) | 2000-11-11 | 2001-11-03 | クロム合金を析出させる方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP00124672A EP1205582B1 (de) | 2000-11-11 | 2000-11-11 | Verfahren zur elektrolytischen Abscheidung aus einer chromhaltigen Lösung |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1205582A1 true EP1205582A1 (de) | 2002-05-15 |
EP1205582B1 EP1205582B1 (de) | 2008-08-20 |
Family
ID=8170352
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00124672A Expired - Lifetime EP1205582B1 (de) | 2000-11-11 | 2000-11-11 | Verfahren zur elektrolytischen Abscheidung aus einer chromhaltigen Lösung |
EP01980543A Withdrawn EP1250472A1 (de) | 2000-11-11 | 2001-11-03 | Verfahren zur abscheidung einer chromlegierung |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01980543A Withdrawn EP1250472A1 (de) | 2000-11-11 | 2001-11-03 | Verfahren zur abscheidung einer chromlegierung |
Country Status (12)
Country | Link |
---|---|
US (1) | US6837981B2 (de) |
EP (2) | EP1205582B1 (de) |
JP (1) | JP3873025B2 (de) |
KR (1) | KR100503210B1 (de) |
CN (1) | CN1306069C (de) |
AT (1) | ATE405694T1 (de) |
BR (1) | BR0107473A (de) |
CA (1) | CA2396946C (de) |
DE (1) | DE50015318D1 (de) |
DK (1) | DK1205582T3 (de) |
ES (1) | ES2310985T3 (de) |
WO (1) | WO2002038835A1 (de) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004050960A1 (de) * | 2002-11-29 | 2004-06-17 | Federal-Mogul Burscheid Gmbh | Herstellung strukturierter hartchromschichten |
US8110087B2 (en) | 2004-04-21 | 2012-02-07 | Federal-Mogul Burscheid Gmbh | Production of a structured hard chromium layer and production of a coating |
US8337687B2 (en) | 2008-04-04 | 2012-12-25 | Federal-Mogul Burscheid Gmbh | Structured chrome solid particle layer and method for the production thereof |
DE102012010315A1 (de) | 2012-05-24 | 2013-11-28 | Eurosun Solartechnik UG (haftungsbeschränkt) | Substrat einer Chalkopyrit-Dünnschichtzelle und Verfahren zu seiner Herstellung |
Families Citing this family (13)
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---|---|---|---|---|
EP1507026A1 (de) * | 2003-08-14 | 2005-02-16 | Enthone Inc. | Verfahren zur selektiven oder vollständigen Inertisierung von Werkstücken und Anlagenteilen mittels nicht reaktiver Beschichtungen |
US20050081937A1 (en) * | 2003-10-17 | 2005-04-21 | Wilmeth Steven L. | Piping for abrasive slurry transport systems |
US20050081936A1 (en) * | 2003-10-17 | 2005-04-21 | Wilmeth Steven L. | Piping for concrete pump systems |
DE102004036588A1 (de) * | 2004-07-28 | 2006-03-23 | Robert Bosch Gmbh | Bateriepack sowie Elektrohandwerkzeugmaschine |
JP4650157B2 (ja) * | 2005-01-12 | 2011-03-16 | マツダ株式会社 | 摺動部用メッキ皮膜及び同皮膜の形成方法 |
JP2007291423A (ja) * | 2006-04-21 | 2007-11-08 | Mazda Motor Corp | 摺動部材 |
CN101892502B (zh) * | 2010-07-27 | 2012-02-01 | 华南理工大学 | 一种铜-铬-钼三元合金镀层及其制备方法 |
CN103046093B (zh) * | 2012-12-21 | 2015-08-26 | 江苏大学 | 一种提高高速钢轧辊表层耐磨性的脉冲电沉积方法 |
PL2845928T3 (pl) * | 2013-09-05 | 2020-05-18 | Macdermid Enthone Inc. | Wodna kompozycja elektrolitu o obniżonej emisji do atmosfery |
JP2016029430A (ja) | 2014-07-25 | 2016-03-03 | セイコーエプソン株式会社 | 電気光学装置、電気光学装置の製造方法、及び電子機器 |
DE102015105761A1 (de) * | 2015-04-15 | 2016-10-20 | HDO Druckguss- und Oberflächentechnik GmbH | Bauteil mit aufgebrachter Chromschicht mit Wolframanteil und Molybdänanteil und Verfahren zur Herstellung eines solchen Bauteils mittels ternärer Abscheidung |
US10794452B2 (en) * | 2018-04-06 | 2020-10-06 | Shimano Inc. | Bicycle chain |
CN109537002B (zh) * | 2018-12-07 | 2020-10-27 | 重庆立道新材料科技有限公司 | 一种超高硬度镀铬添加剂及其应用 |
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SU834264A1 (ru) * | 1979-11-21 | 1981-05-30 | Московский Вечерний Металлургическийинститут | Электролит дл осаждени покрытийиз СплАВА HA OCHOBE XPOMA |
US5196108A (en) * | 1991-04-24 | 1993-03-23 | Scot Industries, Inc. | Sucker rod oil well pump |
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US3745097A (en) | 1969-05-26 | 1973-07-10 | M & T Chemicals Inc | Electrodeposition of an iridescent chromium coating |
GB1455580A (en) * | 1973-12-13 | 1976-11-17 | Albright & Wilson | Electrodeposition of chromium |
CS214553B1 (cs) * | 1979-11-30 | 1984-02-28 | Ladislav Herbansky | Sposob galvan iekého nanášania funkčněj vrstvy odolnéj Hlavně proti otěru |
US4392922A (en) * | 1980-11-10 | 1983-07-12 | Occidental Chemical Corporation | Trivalent chromium electrolyte and process employing vanadium reducing agent |
US4588481A (en) | 1985-03-26 | 1986-05-13 | M&T Chemicals Inc. | Chromium plating bath for producing non-iridescent, adherent, bright chromium deposits at high efficiencies and substantially free of cathodic low current density etching |
CN1004711B (zh) * | 1987-01-26 | 1989-07-05 | 北京市理化分析测试中心 | 微裂纹铬电镀液及电镀方法 |
CN1016875B (zh) * | 1989-04-03 | 1992-06-03 | 陈惠国 | 含多种纯稀土的镀铬添加剂及其应用 |
US5176813A (en) | 1989-11-06 | 1993-01-05 | Elf Atochem North America, Inc. | Protection of lead-containing anodes during chromium electroplating |
-
2000
- 2000-11-11 DE DE50015318T patent/DE50015318D1/de not_active Expired - Lifetime
- 2000-11-11 AT AT00124672T patent/ATE405694T1/de active
- 2000-11-11 ES ES00124672T patent/ES2310985T3/es not_active Expired - Lifetime
- 2000-11-11 EP EP00124672A patent/EP1205582B1/de not_active Expired - Lifetime
- 2000-11-11 DK DK00124672T patent/DK1205582T3/da active
-
2001
- 2001-11-03 BR BR0107473-3A patent/BR0107473A/pt not_active Application Discontinuation
- 2001-11-03 JP JP2002541146A patent/JP3873025B2/ja not_active Expired - Fee Related
- 2001-11-03 CN CNB018036236A patent/CN1306069C/zh not_active Expired - Fee Related
- 2001-11-03 WO PCT/EP2001/012747 patent/WO2002038835A1/de active IP Right Grant
- 2001-11-03 US US10/169,959 patent/US6837981B2/en not_active Expired - Lifetime
- 2001-11-03 CA CA002396946A patent/CA2396946C/en not_active Expired - Fee Related
- 2001-11-03 KR KR10-2002-7008837A patent/KR100503210B1/ko active IP Right Grant
- 2001-11-03 EP EP01980543A patent/EP1250472A1/de not_active Withdrawn
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SU834264A1 (ru) * | 1979-11-21 | 1981-05-30 | Московский Вечерний Металлургическийинститут | Электролит дл осаждени покрытийиз СплАВА HA OCHOBE XPOMA |
US5196108A (en) * | 1991-04-24 | 1993-03-23 | Scot Industries, Inc. | Sucker rod oil well pump |
Non-Patent Citations (1)
Title |
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DATABASE WPI Section Ch Week 198215, Derwent World Patents Index; Class M11, AN 1982-30415E, XP002166021 * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004050960A1 (de) * | 2002-11-29 | 2004-06-17 | Federal-Mogul Burscheid Gmbh | Herstellung strukturierter hartchromschichten |
US7699970B2 (en) | 2002-11-29 | 2010-04-20 | Federal-Mogul Burscheid Gmbh | Production of structured hard chrome layers |
US8277953B2 (en) | 2002-11-29 | 2012-10-02 | Federal-Mogul Burscheid Gmbh | Production of structured hard chrome layers |
US8110087B2 (en) | 2004-04-21 | 2012-02-07 | Federal-Mogul Burscheid Gmbh | Production of a structured hard chromium layer and production of a coating |
US8337687B2 (en) | 2008-04-04 | 2012-12-25 | Federal-Mogul Burscheid Gmbh | Structured chrome solid particle layer and method for the production thereof |
DE102012010315A1 (de) | 2012-05-24 | 2013-11-28 | Eurosun Solartechnik UG (haftungsbeschränkt) | Substrat einer Chalkopyrit-Dünnschichtzelle und Verfahren zu seiner Herstellung |
Also Published As
Publication number | Publication date |
---|---|
JP3873025B2 (ja) | 2007-01-24 |
DE50015318D1 (de) | 2008-10-02 |
WO2002038835A1 (de) | 2002-05-16 |
BR0107473A (pt) | 2002-11-19 |
DK1205582T3 (da) | 2008-11-24 |
EP1205582B1 (de) | 2008-08-20 |
ES2310985T3 (es) | 2009-02-01 |
CA2396946C (en) | 2008-02-19 |
ATE405694T1 (de) | 2008-09-15 |
KR100503210B1 (ko) | 2005-07-21 |
EP1250472A1 (de) | 2002-10-23 |
US20030121794A1 (en) | 2003-07-03 |
CN1395629A (zh) | 2003-02-05 |
CN1306069C (zh) | 2007-03-21 |
JP2004513242A (ja) | 2004-04-30 |
CA2396946A1 (en) | 2002-05-16 |
US6837981B2 (en) | 2005-01-04 |
KR20020074194A (ko) | 2002-09-28 |
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