EP2055801A1 - Procédé destiné au durcissement de surfaces de pièces usinées en acier inoxydable et sels fondus pour l'exécution du procédé - Google Patents

Procédé destiné au durcissement de surfaces de pièces usinées en acier inoxydable et sels fondus pour l'exécution du procédé Download PDF

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Publication number
EP2055801A1
EP2055801A1 EP08018519A EP08018519A EP2055801A1 EP 2055801 A1 EP2055801 A1 EP 2055801A1 EP 08018519 A EP08018519 A EP 08018519A EP 08018519 A EP08018519 A EP 08018519A EP 2055801 A1 EP2055801 A1 EP 2055801A1
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EP
European Patent Office
Prior art keywords
molten salt
stainless steel
salt
workpieces
weight
Prior art date
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Granted
Application number
EP08018519A
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German (de)
English (en)
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EP2055801B1 (fr
Inventor
Ulrich Dr. Baudis
Michael. Dr. Merz
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Durferrit GmbH Thermotechnik
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Durferrit GmbH Thermotechnik
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Publication of EP2055801A1 publication Critical patent/EP2055801A1/fr
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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
    • 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
    • C23C8/40—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 using liquids, e.g. salt baths, liquid suspensions
    • C23C8/42—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 using liquids, e.g. salt baths, liquid suspensions only one element being applied
    • C23C8/44—Carburising
    • C23C8/46—Carburising of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/34—Methods of heating
    • C21D1/44—Methods of heating in heat-treatment baths
    • C21D1/46—Salt baths
    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/18—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions
    • C23C10/20—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions only one element being diffused
    • C23C10/24—Salt bath containing the element to be diffused
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/001—Austenite

Definitions

  • the invention relates to a method for hardening surfaces of workpieces made of stainless steel and a molten salt for carrying out the method.
  • stainless steel Due to its excellent corrosion resistance, stainless steel is used in chemical apparatus engineering, in food technology, in the petrochemical industry, in the offshore sector, in shipbuilding and aircraft construction, in architecture, in building construction and equipment construction and in many other industrial sectors.
  • Corrosion-resistant stainless steel is used when at least 13% by weight chromium is alloyed to an iron material. In most cases nickel, titanium and molybdenum are additionally contained in the iron alloy, as for example in "Stahl Merkblatt 821 Stainless Steel - Properties Information Office Stainless Steel, PF 102205, 40013 Düsseldorf www.edelstahl-rostein.de” and in “ P. Gümpel et al. Stainless Steels, Expert Verlag, Volume 349, Renningen Malmsheim 1998 ", is operated.
  • the steel is generally not sufficiently resistant to corrosion to be considered "stainless steel".
  • the content of metallic chromium in the steel is thus an important criterion for corrosion resistance, as stated in particular in the cited publication by P. Gümpel.
  • a major disadvantage of most common stainless steels such as 1.4301, 1.4441, 1.4541 or 1.4575 is that they are quite soft and thus susceptible to scratching the surface by hard particles such as dust, sand and the like.
  • Most stainless steels - apart from the so-called martensitic stainless steels - are not hardenable by physical methods such as annealing and quenching. The low surface hardness often hinders the use of stainless steel.
  • Another disadvantage of most stainless steels is their strong tendency to seize, that is, to weld the surface of two mutually sliding surfaces due to adhesion.
  • a hard and at the same time corrosion-resistant layer can be thermochemically produced by the so-called Kolster any on stainless steel.
  • This process is mentioned, for example, in "Kolsterizing - Corrosion-resistant O-surface hardening of austenitic stainless steel - Information Sheet of Bodycote Hardiff bv, Parimariboweg 45, NL-7333 Apeldoorn, info@hardiff.de".
  • the conditions of the process are, however, neither described in the patent literature nor in the generally accessible scientific literature.
  • Components treated in this way have a hard, wear-resistant layer between 10 and 35 ⁇ m thick, and the corrosion resistance of the base material is maintained. Kolsterised components must not be heated above 400 ° C, otherwise they will lose their corrosion resistance.
  • the invention has for its object to provide a method by means of which a hardening of workpieces made of stainless steel is made possible, in which at the same time a high corrosion resistance of the workpieces is obtained.
  • the inventive method is used for hardening surfaces of workpieces made of stainless steel.
  • the workpieces are immersed in a molten salt and this exposed for a period of 24 hours to 240 hours.
  • the temperature of the molten salt is less than 400 ° C.
  • the molten salt has the following composition: potassium acetate 60-100% by weight sodium 0-100% by weight metal salt 0-2% by weight
  • the treatment temperature of the workpieces that is, the temperature of the molten salt used in the present invention is smaller than the formation temperature of chromium carbide which is in the range of 420 ° C to 440 ° C, the formation of carbides in the steel matrix becomes is called the lattice structure of the stainless steel, avoided.
  • molten salt according to the invention which contains constituents from which diffusible carbon can be released and suitable activators which cause the release of diffusible carbon at low temperatures.
  • the concentration of active carbon donors (acetates or intermediate carbides) in the molten salt of the invention is very high compared to the concentration of corresponding substances (ammonia, methane, carbon monoxide) in gas atmospheres or in the plasma.
  • the relative Long treatment times of the workpieces in the molten salt are based on the fact that the diffusion rate of carbon is a function of the temperature and significantly decreases at temperatures below 450 ° C. At the low temperatures required to avoid formation of chromium carbide, long diffusion times of 24 to 240 hours must be used. However, the resulting long treatment periods are not critical because stainless steels, especially austenitic stainless steels or so-called. Duplex steels (ferritic - austenitic steels) are very insensitive to such long heat treatment periods, that is, they change their other mechanical properties or the structure so good as not.
  • Stainless steel is usually in the form of an austenitic steel, that is, the iron matrix has the structure of austenite, a face-centered cubic lattice, such as in "Steel Leaflet 821 stainless steel - Properties Information Center stainless steel, PF 102204, 40013 Dusseldorf www.edelstahl-rustproof .de “and in” P. Gümpel et al. Stainless Steels, Expert Verlag, Volume 349, Renningen Malmsheim 1998 "is described.
  • the base melt is a salt mixture of potassium acetate, sodium acetate and a metal salt. Due to the holding time at a fixed temperature, which is in any case below 400 ° C., and thus below the formation temperature of chromium carbide, and which preferably lies in the range between 320 ° C. and 380 ° C., the acetate decomposes and forms free carbon.
  • the added metal salt can also cause a catalytic decomposition of the acetate to a metal carbide, which in turn decomposes at the existing temperature and releases "atomic" carbon to the stainless steel.
  • the present invention avoids high equipment and energy costs and makes use of a light, easy for less qualified personnel easily executable procedure.
  • the tendency of the stainless steel for eating, that is, for cold welding and thus also the adhesive wear is substantially reduced.
  • the hardness of the surface of the stainless steel is increased from 200 to 300 Vickers to values up to 1000 Vickers, resulting in a high scratch resistance.
  • the metal salt contained in the molten salt of the invention preferably has the cations and anions recited in claims 3 and 4.
  • the molten salt is operated under air.
  • the disadvantage here is that by air contact an accelerated decomposition of the acetates in the molten salt is carried out by oxidation processes, whereby the efficiency in the treatment of the workpieces is reduced in the molten salt.
  • N 2 , Ar, CO, CO 2 or mixtures of these gases can be used as protective gases.
  • the acetates decompose only due to heat, no longer additionally by oxidation processes, that is, the rate of decomposition of acetates is significantly reduced.
  • the decomposition of the acetates can also be reduced with little design effort by the fact that the protective gases introduced into the molten salt, that is initiated. This results in a simultaneous circulation of the molten salt, which leads to a uniform distribution of the salts in the molten salt. In general, a circulation can also take place by introducing air into the molten salt.
  • the molten salt can also be moved mechanically, for example by stirring or tumbling.
  • a mixture of 120 g of potassium acetate and 0.2 g of NiCl 2 is melted in a crucible and at 380 ° C for 53.5 h, a bolt (material: X5 Cr Ni Mo 17-12-2) immersed. After treatment, the bolt is quenched in water. Layer thicknesses of 11 ⁇ m to 13 ⁇ m are formed.
  • the GDOS analysis according to Fig. 2 shows a significant increase of carbon (up to 16%) in this layer ( Fig. 2 shows the carbon content in wt.% depending on the distance from the surface of the workpiece).
  • Fig. 1 shows a cross-section of the workpiece (bolt) in the region of this layer.
  • Fig. 4 shows the concentration of Fe, C, Cr in the workpiece in% by weight as a function of the distance from the surface of the workpiece. How out Fig.4 can be seen, in turn, a significant increase of carbon is obtained in the layer, wherein in the layer, the proportion of Cr, Fe is reduced.
  • Fig. 3 shows a cross-section of the workpiece (bolt) in the region of this layer.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Heat Treatment Of Articles (AREA)
EP08018519A 2007-10-31 2008-10-23 Procédé destiné au durcissement de surfaces de pièces usinées en acier inoxydable et sels fondus pour l'exécution du procédé Active EP2055801B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102007051949A DE102007051949B3 (de) 2007-10-31 2007-10-31 Verfahren zum Härten von Oberflächen von Werkstücken aus Edelstahl und Verwendung einer Salzschmelze zur Durchführung des Verfahrens

Publications (2)

Publication Number Publication Date
EP2055801A1 true EP2055801A1 (fr) 2009-05-06
EP2055801B1 EP2055801B1 (fr) 2012-12-05

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EP08018519A Active EP2055801B1 (fr) 2007-10-31 2008-10-23 Procédé destiné au durcissement de surfaces de pièces usinées en acier inoxydable et sels fondus pour l'exécution du procédé

Country Status (6)

Country Link
US (1) US8083866B2 (fr)
EP (1) EP2055801B1 (fr)
JP (1) JP5371376B2 (fr)
CA (1) CA2642322A1 (fr)
DE (1) DE102007051949B3 (fr)
DK (1) DK2055801T3 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2757423B1 (fr) * 2013-01-17 2018-07-11 Omega SA Pièce pour mouvement d'horlogerie
CN103233215B (zh) * 2013-05-10 2015-08-12 江苏永昊高强度螺栓有限公司 螺栓表面发黑工艺
DE102016215709A1 (de) * 2015-08-28 2017-03-02 Tsubakimoto Chain Co. Kettenkomponente und Kette

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2249581A (en) * 1938-11-30 1941-07-15 Holden Artemas F Nonpoisonous carburizing liquid bath
US3840450A (en) 1963-10-21 1974-10-08 K Inoue Method of diffusing substances into surface zones of conductive bodies
EP0054962A1 (fr) * 1980-12-23 1982-06-30 Degussa Aktiengesellschaft Procédé non polluant de carburation de l'acier en bain de sel fondu
US4461655A (en) * 1982-02-23 1984-07-24 National Research Development Corporation Fused salt bath composition
DE102006026883B3 (de) 2006-06-09 2007-08-16 Durferrit Gmbh Verfahren zum Härten von Edelstahl und Salzschmelze zur Durchführung des Verfahrens

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2537830A (en) * 1944-09-14 1951-01-09 Artemas F Holden Self-agitating metallurgical salt bath
US2948644A (en) * 1948-05-29 1960-08-09 Gerhard W Ahrens Pack carburizing with furane derivatives
EP0072789A1 (fr) * 1981-02-18 1983-03-02 National Research Development Corporation Composition de bain de sel fondu

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2249581A (en) * 1938-11-30 1941-07-15 Holden Artemas F Nonpoisonous carburizing liquid bath
US3840450A (en) 1963-10-21 1974-10-08 K Inoue Method of diffusing substances into surface zones of conductive bodies
EP0054962A1 (fr) * 1980-12-23 1982-06-30 Degussa Aktiengesellschaft Procédé non polluant de carburation de l'acier en bain de sel fondu
US4461655A (en) * 1982-02-23 1984-07-24 National Research Development Corporation Fused salt bath composition
DE102006026883B3 (de) 2006-06-09 2007-08-16 Durferrit Gmbh Verfahren zum Härten von Edelstahl und Salzschmelze zur Durchführung des Verfahrens

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
ALWART S ET AL: "LOW-TEMPERATURE NITROCARBURIZING", ADVANCED MATERIALS & PROCESSES, AMERICA SOCIETY FOR METALS. METALS PARK, OHIO, US, vol. 154, no. 3, 1 September 1998 (1998-09-01), pages 41 - 43, XP000778078, ISSN: 0882-7958 *
BAUDIS U ET AL: "UNTERSUCHUNGEN ZUM VERSTAENDNIS DER CHEMISCHEN REAKTIONEN BEIM NITROCARBURIEREN IN SALZSCHMELZEN", HTM HAERTEREI TECHNISCHE MITTEILUNGEN, CARL HANSER VERLAG, MUNCHEN, DE, vol. 58, no. 5, 1 January 2003 (2003-01-01), pages 251 - 256, XP001186002, ISSN: 0341-101X *
D. GÜNTHER ET AL., OBERFLÄCHENHÄRTUNG VON AUSTENITISCHEN STÄHLEN UNTER BEIBEHALTUNG DER KORROSIONSBESTÄNDIGKEIT HÄRTEREI-TECHN. MITT., vol. 56, 2001, pages 74 - 83
H.-J. SPIES ET AL., MAT.-WISS. U. WERKSTOFFTECHNIK, vol. 30, 1999, pages 457 - 464
Y. SUN; T. BELL ET AL., THE RESPONSE OF AUSTENITIC STAINLESS STEEL TO LOW TEMP. PLASMA NITRIDING

Also Published As

Publication number Publication date
DK2055801T3 (da) 2013-01-28
US8083866B2 (en) 2011-12-27
JP2009108411A (ja) 2009-05-21
JP5371376B2 (ja) 2013-12-18
CA2642322A1 (fr) 2009-04-30
DE102007051949B3 (de) 2009-03-12
EP2055801B1 (fr) 2012-12-05
US20100108198A1 (en) 2010-05-06

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