EP3287546A1 - Système anticalaminage multi-couche pour aciers durcissables par pression - Google Patents
Système anticalaminage multi-couche pour aciers durcissables par pression Download PDFInfo
- Publication number
- EP3287546A1 EP3287546A1 EP17185771.7A EP17185771A EP3287546A1 EP 3287546 A1 EP3287546 A1 EP 3287546A1 EP 17185771 A EP17185771 A EP 17185771A EP 3287546 A1 EP3287546 A1 EP 3287546A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- layer
- protective layer
- layers
- protective
- steels
- 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- Withdrawn
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Classifications
-
- 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
- C23C28/042—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 including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1212—Zeolites, glasses
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
Definitions
- the present invention relates to the field of protective layers for steels, in particular press-hardenable steels.
- a problem with this process is the scaling of the components, which occurs immediately as soon as the heated component (850 ° -950 ° C.) is taken out of the protective gas-containing furnace and comes into contact with atmospheric oxygen. If the component is austenitized under an air atmosphere, the surface is heavily scaled as low as 540 ° C.
- the resulting scale layer is inhomogeneous, brittle, peels off and offers RD 42016 / A1: AH no basis for subsequent processes such as welding, cathodic dip painting, etc. Therefore, the oxide layer is removed by blasting prior to further processing of the component.
- a protective layer for steels, in particular press-hardenable steels, characterized in that it comprises at least two layers, both of which are predominantly composed of an oxide material, and wherein the next layer to the steel (hereinafter referred to as "first layer”) Glass transition temperature of ⁇ 400 ° C and ⁇ 500 ° C, and the outer layer (hereinafter referred to as “second layer”) has a glass transition temperature of ⁇ 500 ° C and ⁇ 900 ° C.
- the glass transition temperature can be measured in particular by dilatometry of the sintered layered body.
- the term "predominantly consist” within the meaning of the present invention includes and / or in particular comprises a wt .-% proportion of ⁇ 90% by weight, more preferably ⁇ 95% by weight and most preferably ⁇ 97% by weight.
- the term "predominantly consisting of an oxide material” means that the layer in question contains no or ⁇ 3% by weight, more preferably ⁇ 1% by weight organic residues of organic precursors (such as silanes, etc.).
- the present protective layer is not limited to two layers but may be composed of multiple layers.
- first layer refers to all layers that meet the above conditions, the second as well.
- the first layer has a glass transition temperature of ⁇ 450 ° C and ⁇ 480 ° C. This has proved advantageous in many applications of the present invention.
- the second layer has a glass transition temperature of ⁇ 600 ° C and ⁇ 750 ° C. This has proved advantageous in many applications of the present invention.
- the first and / or second layer is produced from a respective starting layer by a sintering process.
- starting layer is thus understood to mean a non-sintered layer from which the respective final layer, which forms part of the protective layer according to the invention, can be produced by sintering.
- the first and / or second starting layer comprises nanoparticulate oxide particles. Preference is given to the average size of the oxidic nanoparticles in a layer between ⁇ 5 nm to ⁇ 100 nm, with a regular size distribution of the particles is preferred.
- the first and / or the second layer and / or the respective starting layers of starting materials from the group comprising oxides, hydroxides, carbonates, nitrates, silicates and salts of organic acids of Al, As, B , Ba, Ca, Ce, Co, Cr, Cu, Eu, Fe, K, La, Li, Mg, Mo, Mn, Na, Ni, P, Sb, Sm, Ti, V, W, Zn, Zr and mixtures generated from it.
- starting material (s) means and / or comprises in particular that the starting layer in question is produced from this substance (s), it usually being possible to form mixed compounds / mixed oxides or similar compounds.
- the educts of the first and / or second layer also contain additives selected from the group consisting of organic inhibitors, plasticizers, modifiers of the nanoparticle surfaces.
- additives selected from the group consisting of organic inhibitors, plasticizers, modifiers of the nanoparticle surfaces
- the added proportion (in% by weight) of Al 2 O 3 , SiO 2 , TiO 2 , and ZrO 2 in the first layer is preferably ⁇ 50%. It has thus been found that the desired properties of the first layer can often be set particularly easily.
- the added proportion (in% by weight) of Al 2 O 3 , SiO 2 , TiO 2 , and ZrO 2 in the second layer is preferably ⁇ 75%. It has been found in this way that the desired properties of the second layer can be adjusted very often so often.
- the total thickness of the protective layer is from ⁇ 2 ⁇ m to ⁇ 10 ⁇ m, preferably ⁇ 4 ⁇ m to ⁇ 6 ⁇ m It turned out that the protective layer usually has excellent protection properties, but at the same time allows good deformability and handling.
- the ratio between the thickness of the first and the second layer is preferably from ⁇ 0.8 to ⁇ 1.2. This has proven to be advantageous for many applications within the present invention.
- the present invention also relates to the use of a protective layer according to the invention as a scale protection system for steels.
- scale protection system means or includes the protection of the steel from the formation of thick layers of oxidation products (scale layers) at temperatures up to 950 ° C. for periods of up to 5 minutes, more preferably up to 10 minutes.
- the present invention also relates to a process for producing one or more starting layers of the protective layer according to the invention, which process comprises a sol-gel process.
- sol-gel process means or includes in particular a process using polymeric and / or particulate sols and colloidal dispersions, whereby combinations of sols and dispersions are also possible.
- the initial protective layer is preferably applied by (possibly repeated) dip coating.
- this comprises a thermal sintering step which is carried out after the layer application and by which the final protective layer is thus produced.
- FIG. 1 shows a diagram indicating the increase in mass over time for two steel samples which have been coated with a protective layer according to the invention, as well as two comparative samples.
- Bindzil 50 / 80® (SiO 2 nanoparticles) is slowly added at 40 ° C. with rapid stirring. These nanoparticles have a corona of a surfactant (1,2-benzisothiazol-3- (2H) -one) that protects the particles from coagulation. 5 ml of water with dissolved Al (NO 3 ) 3 and Ca (NO 3 ) 2 are slowly added to this mixture with vigorous stirring. Later, Levasil 300/30 ® (SiO 2 nanoparticles) is added. At the end, the pH is controlled again, this time within 9-13. The lower it is, the longer the dispersion can be stored. The result is a milky-white, slightly viscous solution. On prolonged standing, however, it tends to form a phase separation, which can be easily eliminated by shaking.
- a surfactant (1,2-benzisothiazol-3- (2H) -one
- Levasil 300/30 ® is added .
- the pH is controlled, which should be within 9-13.
- protective layers A and B are applied to two steel samples (22MnB5, 35 x 15 x 1.5mm 3 ).
- the steel samples are blasted with SiO 2 microparticles (70-110 ⁇ m) and they are cleaned in an ethanol bath in an ultrasonic bath (100 W) for 3 minutes of residues of the sand particles.
- the activation of the samples by immersion in a Nital solution (2 wt .-% HNO 3 in ethanol) for at least 5 seconds.
- the samples are rinsed with ethanol and dried quickly with hot air (up to 350 ° C).
- the coating of the substrate is carried out by immersion at room temperature.
- the pull-out speed is up to 50 mm / s.
- the dispersion for the steel-proximate first layer is applied by dipping, followed by rapid drying with hot air (up to 350 ° C). A crack-free, slightly white-cloudy and dry layer is obtained.
- the dispersion for the outer, second layer is applied by immersion, followed by rapid drying with hot air (up to 350 ° C). A crack-free, slightly white-cloudy and dry layer is obtained.
- Layers A and B are resistant to abrasion and stable under normal conditions against air oxidation.
- the steel samples on which the protective layers A and B are applied are sintered in a preheated oven (900-950 ° C) in air-atmosphere.
- Table 2 shows the chemical compositions as well as the glass transition temperatures and the expansion coefficients of the protective layers A and B after sintering.
- Fig. 1 is the mass increase (as a measure of the oxidation) compared to an uncoated 22MnB5 steel sheet and a AlSi-coated 22MnB5 steel sheet (Usibor 1500 ® ) shown.
- the protective layers of the invention layer thickness 6.0 ⁇ 0.5 microns
- the Usibor 1500 has a significantly greater thickness (AlSi layer about 25-30 microns).
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Nanotechnology (AREA)
- Dispersion Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102016115746.5A DE102016115746A1 (de) | 2016-08-24 | 2016-08-24 | Mehrschichtiges Zunderschutzsystem für presshärtbare Stähle |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3287546A1 true EP3287546A1 (fr) | 2018-02-28 |
Family
ID=59713781
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP17185771.7A Withdrawn EP3287546A1 (fr) | 2016-08-24 | 2017-08-10 | Système anticalaminage multi-couche pour aciers durcissables par pression |
Country Status (2)
Country | Link |
---|---|
EP (1) | EP3287546A1 (fr) |
DE (1) | DE102016115746A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3974180A1 (fr) | 2020-09-28 | 2022-03-30 | Volkswagen Aktiengesellschaft | Procédé de fabrication d'un élément en tôle d'acier moulé à chaud et trempé à la presse |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102020107749A1 (de) | 2020-03-20 | 2021-09-23 | Peter Amborn | Verfahren zur Vermeidung der Oxidation der Oberfläche eines metallischen Substrats sowie metallisches Substrat hergestellt nach dem Verfahren |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007015635A1 (de) * | 2007-03-31 | 2008-10-02 | Schaeffler Kg | Beschichtung eines Bauteils aus gehärtetem Stahl und Verfahren zum Aufbringen der Beschichtung |
DE102007038215A1 (de) * | 2007-08-13 | 2009-02-19 | Nano-X Gmbh | Verfahren zur Herstellung einer aktiven Korrosionsschutzbeschichtung auf Bauteilen aus Stahl |
WO2011144603A1 (fr) * | 2010-05-20 | 2011-11-24 | Rheinisch-Westfälische Technische Hochschule Aachen | Couche à base de nanoparticules servant à protéger des aciers contre le calaminage |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102006056427B4 (de) | 2006-11-28 | 2016-01-21 | Nano-X Gmbh | Verfahren zum Aufbringen eines Beschichtungsmaterials auf ein Substrat und Verwendung des Verfahrens |
DE102008019785A1 (de) | 2008-04-18 | 2009-10-22 | Itn Nanovation Ag | Verfahren zum Herstellen einer korrosionsstabilen, gasdichten Beschichtung und Verwendung der Beschichtung |
RS54157B1 (en) | 2012-12-17 | 2015-12-31 | Henkel Ag & Co. Kgaa | MULTI-PHASE METHOD OF COATING STEEL BEFORE THERMO |
DE102015204802A1 (de) | 2015-03-17 | 2016-09-22 | Magna International Inc. | Beschichtetes Stahlbauteil, Verfahren zur Herstellung des Stahlbauteils und Herstellungsanlage |
-
2016
- 2016-08-24 DE DE102016115746.5A patent/DE102016115746A1/de not_active Withdrawn
-
2017
- 2017-08-10 EP EP17185771.7A patent/EP3287546A1/fr not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007015635A1 (de) * | 2007-03-31 | 2008-10-02 | Schaeffler Kg | Beschichtung eines Bauteils aus gehärtetem Stahl und Verfahren zum Aufbringen der Beschichtung |
DE102007038215A1 (de) * | 2007-08-13 | 2009-02-19 | Nano-X Gmbh | Verfahren zur Herstellung einer aktiven Korrosionsschutzbeschichtung auf Bauteilen aus Stahl |
WO2011144603A1 (fr) * | 2010-05-20 | 2011-11-24 | Rheinisch-Westfälische Technische Hochschule Aachen | Couche à base de nanoparticules servant à protéger des aciers contre le calaminage |
Non-Patent Citations (1)
Title |
---|
YEKEHTAZ M ET AL: "Effect of nano-particulate sol-gel coatings on the oxidation resistance of high-strength steel alloys during the press-hardening process", MATERIALS AND CORROSION, WILEY, vol. 63, no. 10, 1 October 2012 (2012-10-01), pages 940 - 947, XP001579026, ISSN: 0947-5117, [retrieved on 20120807], DOI: 10.1002/MACO.201206729 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3974180A1 (fr) | 2020-09-28 | 2022-03-30 | Volkswagen Aktiengesellschaft | Procédé de fabrication d'un élément en tôle d'acier moulé à chaud et trempé à la presse |
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Publication number | Publication date |
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DE102016115746A1 (de) | 2018-03-01 |
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