EP1231299B1 - Light alloy-based composite protective multifunction coating - Google Patents

Light alloy-based composite protective multifunction coating Download PDF

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Publication number
EP1231299B1
EP1231299B1 EP99958538A EP99958538A EP1231299B1 EP 1231299 B1 EP1231299 B1 EP 1231299B1 EP 99958538 A EP99958538 A EP 99958538A EP 99958538 A EP99958538 A EP 99958538A EP 1231299 B1 EP1231299 B1 EP 1231299B1
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EP
European Patent Office
Prior art keywords
coating
oxide
accordance
pores
ceramic
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Expired - Lifetime
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EP99958538A
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German (de)
English (en)
French (fr)
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EP1231299A1 (en
EP1231299A4 (en
Inventor
Alexandr Sergeevich Shatrov
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Isle Coat Ltd
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Isle Coat Ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/044—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/048—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material with layers graded in composition or physical properties
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/80—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/024—Anodisation under pulsed or modulated current or potential
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/026—Anodisation with spark discharge

Definitions

  • the invention can be used in various branches of engineering, electronics, medicine and other fields in which non-ferrous metals and their alloys are used.
  • the invention relates to a technology for applying protective coatings to such metals and alloys and also to components and articles made from them.
  • non-ferrous alloy components with a hardening ceramic coating instead of components of traditional materials (ceramic, high-alloy steels and cast irons) makes possible an considerable increase in the durability and reliability of highly-loaded and rapidly wearing components, a reduction in weight and an improvement in the dynamic characteristics of units.
  • One way of creating such coatings is the formation on the protected component of a porous ceramic coating, into the pores of which various fillers are introduced.
  • a fault common to all the above processes is the limitation of their application at high temperatures arising in operating in extreme conditions of use of the components, and low ratings for the thermal and electrical conductivity of the coatings.
  • the rotor is made of steel.
  • the gas-thermal dusting-on process can be used to apply coatings of virtually any compositions to any backings.
  • coatings applied by gas-thermal dusting-on do not bond firmly enough to the base. This fault is worse if non-ferrous alloys form the base, since they rapidly dissipate heat and intensively form thin oxide films under the effect of the plasma jet.
  • non-ferrous alloys react critically to the high temperature of the dusting-on process, since the surfaces of aluminium and magnesium alloys can be melted, and the overheating of titanium alloys leads to a reduction in their fatigue resistance.
  • the coatings produced by this process are strong, wear-resistant and resistant to corrosion at high temperatures.
  • the use of high temperatures in this technology makes it impossible to apply such coatings to components made of non-ferrous alloys.
  • the main problem with the process described is the low mechanical strength and instability of the basic anode-oxide coating.
  • Anode coatings of a thickness of more than 10 ⁇ m have a large number of pores, which are hydrated to a considerable degree (water content in the coating exceeds 10%), and their composition also includes 10-20% of electrolyte anions built into the structure of the coating.
  • electrolyte anions built into the structure of the coating.
  • the electrolyte components and water depart from the structure of the coating, which leads to breaks and crumbling in the anode-oxide layer and is detrimental to its protective properties.
  • the anode-oxide layers consist mainly of amorphous phases of oxides, and consequently their strength and micro-hardness are not high.
  • One task of the present invention is to develop a composite coating for non-ferrous alloy components, possessing good wear resistance and a low friction coefficient throughout the working life of the component, resistance to aggressive media and ability to withstand dynamic contact loads and vibrations.
  • a second task of this invention is to develop a composite coating for non-ferrous alloy components, possessing high wear resistance and scratch resistance, resistance to erosion wear and to the action of abrasive media at high temperatures, and also resistance to corrosion.
  • a third task of this invention is to develop an ecologically safe and comparatively inexpensive technology for the application of composite coatings to non-ferrous alloys, which can be used in series production.
  • a coating which takes the form of a porous oxide-ceramic coating formed by the oxidation of the surface layer of the material being protected by the plasma-electrolytic oxidation method, into the pores of which are introduced metals such as Ni, Cu, Co, Fe, Cr, Mo, Ti, Al, Sb, Ag, Zn, Cd, Pb, Sn, Bi, In, Ga and mixtures of them or the carbides, oxides, nitrides, borides and silicides of metals in Groups IVB-VIB of the Mendeleyev periodic system, and mixtures of them.
  • metals such as Ni, Cu, Co, Fe, Cr, Mo, Ti, Al, Sb, Ag, Zn, Cd, Pb, Sn, Bi, In, Ga and mixtures of them or the carbides, oxides, nitrides, borides and silicides of metals in Groups IVB-VIB of the Mendeleyev periodic system, and mixtures of them.
  • the adhesion of these coatings to the base is 5-10 times as strong as the adhesion of gas-thermal dusted-on coatings, and their strength and micro-hardness are 2-5 times as great, higher than for anode-oxide layers.
  • the frequency of succession of the pulses is 50-3000 Hz.
  • Current density is 2-200 A/dm 2 .
  • a fine crystalline oxide layer of micro-hardness 300-2000 Hv, depending on the composition of the alloy base, is created on the surfaces of the non-ferrous alloy components under the effect of plasmo-chemical reactions.
  • the thickness of the layer may be from 1 to 600 ⁇ m.
  • the size of the pores varies from several tens of nanometres to several microns in diameter. Pores of size larger than one micron comprise more than 90% of the volume of all the pores. It is into these pores that the main mass of the functional compounds is introduced.
  • the porous structure of the oxide-ceramic layer serves as a matrix for the creation of the multifunctional composite coating.
  • the porosity of the coating varies through the depth of the coating. It is at its maximum at the surface, but is less by a factor of 2-6 as it approaches the basic metal.
  • the concentration of functional compounds introduced into the pores conforms to these characteristics - it is at its maximum in the layer next to the surface and decreases exponentially as the depth of coating increases.
  • Oxide-ceramic coatings with open porosity of 10-20% form an ideal matrix for the creation of composite coatings by filling this matrix with compounds possessing specific properties and fulfilling specific functions (anti-friction, thermal conductivity, anti-corrosion etc.).
  • micro-hardness of an oxide-ceramic coating has maximum values close to the basic metal and steadily decreases towards the outer surface of the coating (by 20-30%).
  • the strongly developed surface of the porous structure of the matrix layer provides excellent adhesion of the functional compounds to the oxide coating. This gives the composite coating its high cohesion strength.
  • the first group of functional compounds introduced into the pores of the oxide layer consists of the soft metals Ni, Cu, Co, Fe, Cr, Mo, Ti, Al, Sb, Ag, Zn, Cd, Pb, Sn, Bi, In, Ga and mixtures of these.
  • the metal exerts a plasticising influence on the composite coating.
  • the specific nature of this coating is due to its deformation behaviour under thermo-mechanical load.
  • the two-phase ceramic-metal structure provides a fivefold increase in shock viscosity as compared with pure ceramic.
  • Such coatings can also be used as anti-friction coatings. After finishing treatment, sectors of the oxide-ceramic layer are laid bare. These stronger sectors on the friction surface take the main load and thus raise the bearing capacity of the surface.
  • the softer sectors of the surface, as they wear, form micro-recesses and grooves, which serve as reservoirs for lubricant, and the presence of which alters the friction regime in the friction contact, facilitates the removal of the products of wear and thus improves the working capabilities of the surface.
  • composite coatings can be formed which optimally correspond to the specific conditions of use with optimal porosity and optimal composition of the functional compounds in the pores of the composite coating.
  • the second group of functional compounds introduced into the pores of the oxide layer consists of refractory compounds of metals of groups IVB-VIB in Mendeleyev's periodic system of elements: carbides, oxides, nitrides, borides and silicides.
  • All the above-listed functional compounds are applied to the porous ceramic matrix layer by known methods of electrolytic or chemical precipitation from aqueous or organic solutions, including the use of ultra-disperse powders, chemical or physical precipitation from gas or vapour phases or the friction-mechanical method (rubbing on) using powders, bars, brushes etc.
  • the functional compounds are introduced into the pores of the oxide-ceramic matrix coating to a depth of 1-150 ⁇ m, depending on the depth of the oxide coating itself and the volume of the pores in it.
  • the working surface is subjected to machine finishing (polishing, lapping, fine grinding, honing, superfinish) until the components are at the required dimensions and roughness of the surfaces, or until the apexes of the oxide-ceramic coating are revealed (bared).
  • machine finishing polishshing, lapping, fine grinding, honing, superfinish
  • This machine treatment makes it possible to remove excess layers of functional compounds and to distribute the remaining part uniformly over the surface.
  • Machine treatment also means that there is no need for the friction surfaces to be run in.
  • the external cylindrical surface is subjected to plasma electrolytic oxidation over a period of 120 min in a phosphate-silicate electrolyte (pH 11) at a temperature of 30°C.
  • the regime is anode-cathode; current density 20 A/dm 2 ; magnitude (amplitude) of final voltage; anode 600 V, cathode 190 V.
  • the depth of the oxide-ceramic coating is 120 ⁇ m, micro-hardness 1800 Hv, open porosity 20%.
  • a specimen of alloy D16 (AlCu 4 Mg 2 ) is subjected to the same treatment as that in Example 1, and possesses the following characteristics: depth of oxide coating 120 ⁇ m, micro-hardness 1800 Hv, open porosity 20%.
  • the specimen was subjected to chemical nickel-plating and then polishing.
  • the depth of penetration of the nickel after polishing is about 10 ⁇ m.
  • the concentration of nickel is at its maximum in the layer next to the surface and decreases exponentially as the depth of coating increases.
  • a specimen of alloy AK4-2 (AlCu 2 , Mg 2 Fe Ni) is subjected to plasma electrolytic oxidation for a period of 90 minutes in a phosphate-silicate electrolyte (pH 11) at a temperature of 30°C
  • the regime is anode-cathode; current density 15 A/dm 2 ; magnitude of final voltage: anode 550 V, cathode 120 V.
  • a composite layer consisting of 20% Cr and 80% Cr 3 C 2 is applied to the specimen by the chemical precipitation method from the gaseous phase. In the course of precipitation, the specimen was heated to 300°C. After this, the specimen was polished. The depth of penetration of the functional compound Cr-Cr 3 C 2 into the porous structure was about 7 ⁇ m.
  • a specimen of alloy VT6 (TiAl 6 V 4 ) was oxidised in an aluminate-sulfate electrolyte (pH 9) for 20 minutes at a temperature of 20°C.
  • Regime anode; current density 50 A/dm 2 ; magnitude of final anode voltage 300 V.
  • a layer of nickel was applied to the specimen by the method of chemical precipitation from the gaseous phase.
  • the specimen was heated to 200°C. After this, the cylindrical surface of the specimen was polished.
  • the depth of penetration of the nickel compound into the porous structure was 3 ⁇ m.
  • a specimen of alloy VMD12 (MgZn 6 MnCu) was oxidised in an aluminate-fluoride electrolyte (pH 12) for 40 minutes at a temperature of 20°C.
  • Regime anode-cathode; current density 8 A/dm 2 ; magnitude of final voltage: anode 350 V, cathode 130 V.
  • a composite layer of nickel was applied to the specimen by the method of chemical precipitation from the gaseous phase. During precipitation, the specimen was heated to 200°C. After this, the cylindrical surface of the specimen was polished. The depth of penetration of the nickel compound into the porous structure of the layer was 10 ⁇ m.
  • a specimen of alloy ABM-3 (AlBe 60 Mg 2 ) - of the "localloy" type - was oxidised in a phosphate-silicate electrolyte (pH 11) for 120 minutes at a temperature of 30°C.
  • Depth of oxide-ceramic coating 100 ⁇ m, micro-hardness 790 Hv, open porosity 18%.
  • a composite layer of nickel was applied to the specimen by the method of chemical precipitation from the gaseous phase. In the course of precipitation, the specimen was heated to 200°C. After this, the cylindrical surface of the specimen was polished. Depth of penetration of the nickel compound into the porous structure of the oxide layer: 8 ⁇ m.
  • a ring-cylinder arrangement with intersecting axes for point contact was selected.
  • a fixed specimen of steel ShKh15, hardness HRC 3 58-60 was pressed to the moving specimen (ring) to which the coating under study had been applied.
  • the tests were conducted in boundary friction regime, in which several droplets of spindle oil are applied to the coated specimen before the test.
  • the slip rate was 2 m/sec, normal load in the contact of the specimens - 75 N.
  • the test took 60 seconds.
  • Ten identical tests were conducted on each ring. The mean values for the characteristics were calculated from the results of these tests.
  • Wear resistance was assessed from wear in weight and dimensions by comparing the dimensions of spots on the steel specimen and the loss of mass of the coated specimen.
  • test results demonstrate the efficiency of using composite coatings on various backings as compared with the usual oxide-ceramic coating on aluminium alloy.
  • the friction coefficient is little more than half, counter-body wear is reduced by a factor of 2-5 and wear of the ring coating itself by a factor of up to 10.
  • the proposed composite coating has such unique properties as high strength and hardness in combination with a certain plasticity, exceptional resistance to wear and scratching, and high resistance to corrosion and vibrations, we have the opportunity to widen considerably the application of non-ferrous metal components.
  • the proposed process for producing protective coatings is distinguished by being ecologically harmless and by its low costs, and is suitable for use on an industrial scale.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Paints Or Removers (AREA)
  • Road Signs Or Road Markings (AREA)
  • Heat Treatment Of Steel (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Sliding-Contact Bearings (AREA)
EP99958538A 1999-08-17 1999-08-17 Light alloy-based composite protective multifunction coating Expired - Lifetime EP1231299B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/RU1999/000298 WO2001012883A1 (fr) 1999-08-17 1999-08-17 Revetement de protection composite multifonctions a base d'alliages legers

Publications (3)

Publication Number Publication Date
EP1231299A1 EP1231299A1 (en) 2002-08-14
EP1231299A4 EP1231299A4 (en) 2006-08-02
EP1231299B1 true EP1231299B1 (en) 2012-01-18

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EP99958538A Expired - Lifetime EP1231299B1 (en) 1999-08-17 1999-08-17 Light alloy-based composite protective multifunction coating

Country Status (12)

Country Link
EP (1) EP1231299B1 (enExample)
JP (1) JP2003507574A (enExample)
KR (1) KR20020042642A (enExample)
CN (1) CN1367849A (enExample)
AT (1) ATE541962T1 (enExample)
AU (1) AU1588600A (enExample)
BR (1) BR9917460A (enExample)
CA (1) CA2382164A1 (enExample)
CZ (1) CZ2002572A3 (enExample)
MX (1) MXPA02001672A (enExample)
NO (1) NO20020748L (enExample)
WO (1) WO2001012883A1 (enExample)

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DE102007052575A1 (de) * 2007-11-03 2009-05-07 Märzhäuser Wetzlar GmbH & Co. KG Schutzschicht
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FR2966533B1 (fr) * 2010-10-21 2014-02-21 Astrium Sas Organe de frottement pour l'assemblage de deux pieces.
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US20160153112A1 (en) 2013-07-19 2016-06-02 Fundación Cidaut Metallic substrate with ceramic coating and method for obtaining it
RU2543659C1 (ru) * 2013-09-02 2015-03-10 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский государственный университет" Способ получения композиционного металлокерамического покрытия на вентильных металлах и их сплавах
FR3014912B1 (fr) 2013-12-16 2016-01-01 Snecma Procede de fabrication d'une piece revetue d'un revetement protecteur
CN104975292B (zh) * 2014-04-08 2018-08-17 通用汽车环球科技运作有限责任公司 制造用于轻金属工件的抗腐蚀且有光泽的外观涂层的方法
CN105887159B (zh) * 2016-05-12 2018-04-10 广东省材料与加工研究所 一种兼具装饰性和功能性的镁合金复合涂层制备方法
CN105887084B (zh) * 2016-05-12 2018-10-30 广东省材料与加工研究所 一种具有自修复功能的镁合金复合涂层制备方法
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AU2010255982B2 (en) * 2009-06-02 2014-04-03 Aap Implantate Ag Osteosynthesis with nano-silver
US12226550B2 (en) 2012-02-03 2025-02-18 Saga University Method of manufacturing a bioimplant

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JP2003507574A (ja) 2003-02-25
EP1231299A1 (en) 2002-08-14
AU1588600A (en) 2001-03-13
WO2001012883A1 (fr) 2001-02-22
NO20020748D0 (no) 2002-02-15
EP1231299A4 (en) 2006-08-02
NO20020748L (no) 2002-04-12
BR9917460A (pt) 2002-04-02
KR20020042642A (ko) 2002-06-05
ATE541962T1 (de) 2012-02-15
CN1367849A (zh) 2002-09-04
CA2382164A1 (en) 2001-02-22
MXPA02001672A (es) 2002-12-13

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