US20080023110A1 - Metal article with high interstitial content - Google Patents

Metal article with high interstitial content Download PDF

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Publication number
US20080023110A1
US20080023110A1 US11/880,597 US88059707A US2008023110A1 US 20080023110 A1 US20080023110 A1 US 20080023110A1 US 88059707 A US88059707 A US 88059707A US 2008023110 A1 US2008023110 A1 US 2008023110A1
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United States
Prior art keywords
thin metal
low temperature
product
workpiece
property
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Abandoned
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US11/880,597
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English (en)
Inventor
Peter Williams
Sunniva Collins
Steven Marx
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Swagelok Co
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Swagelok Co
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Priority to US11/880,597 priority Critical patent/US20080023110A1/en
Assigned to SWAGELOK COMPANY reassignment SWAGELOK COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: COLLINS, SUNNIVA R., MARX, STEVEN V., WILLIAMS, PETER C.
Publication of US20080023110A1 publication Critical patent/US20080023110A1/en
Abandoned legal-status Critical Current

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    • 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
    • C23C8/06—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 gases
    • C23C8/08—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 gases only one element being applied
    • C23C8/20—Carburising
    • C23C8/22—Carburising of ferrous surfaces
    • 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
    • C23C8/06—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 gases
    • C23C8/08—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 gases only one element being applied
    • C23C8/20—Carburising
    • 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
    • C21D1/06—Surface hardening
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C22/00—Alloys based on manganese
    • 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
    • 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
    • C23C8/06—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 gases
    • C23C8/08—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 gases only one element being applied
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces

Definitions

  • Case hardening is a widely used industrial process for enhancing the surface hardness of shaped metal articles.
  • the workpiece is contacted with natural gas or propane at elevated temperature whereby carbon atoms liberated by decomposition of the carbon compound diffuse into the workpiece's surface.
  • Hardening occurs through the reaction of these diffused carbon atoms with one or more metals in the workpiece thereby forming distinct chemical compounds, i.e. carbides, followed by precipitation of these carbides as discrete, extremely hard, crystalline particles in the metal forming the workpiece's surface.
  • Stickels “Gas Carburizing”, pp 312 to 324, Volume 4, ASM Handbook, ⁇ 1991, ASM International.
  • very thin workpieces are low temperature carburized so that diffused carbon reaches a substantial portion of the product's core.
  • the result is that new products are obtained which, as a whole, contain higher levels of interstitial (diffused) carbon and exhibit better combinations of properties than seen in the past.
  • this invention provides a process for producing a thin metal product in which at least one property of the thin metal product, as a whole, is enhanced by at least 10% as compared with an otherwise identical untreated product, the process comprising subjecting a thin metal workpiece to a low temperature diffusion-based surface treatment, preferably low temperature carburization. Most commonly, yield strength is substantially increased while ductility is substantially retained.
  • this invention also provides a thin metal product produced by subjecting a thin metal workpiece to a low temperature diffusion-based surface treatment, the thin metal product as a whole exhibiting at least one property which is enhanced by at least 10% as compared with an otherwise identical product not subjected to such surface treatment, preferably low temperature carburization.
  • this invention also provides a shaped article which is produced by forming a mass of the thin metal product described above into a desired shape and sintering.
  • FIGS. 1 and 2 show the effect on the yield strength and ductility of AISI 316 stainless steel foil low temperature carburized in accordance with this invention, FIG. 1 illustrating the raw load vs. displacement data and FIG. 2 showing the data normalized to a standard stress/strain curve.
  • the primary focus of this invention is on the low temperature carburization of iron-, nickel-, cobalt-, and/or chromium-based alloys, especially stainless steel.
  • elemental carbon diffuses into the metal matrix forming the workpiece without formation of carbide precipitates.
  • reference to carburizing stainless steel “without formation of carbide precipitates” will be understood to mean “without formation of the types and amounts of carbide precipitates which adversely affect the corrosion resistance of the stainless steel.”
  • low temperature carburization is carried out in the same way as done in the past so as to produced carburized workpieces whose treated surfaces or “case” contain elevated amounts of elemental carbon, normally about 2-15 atomic %, more typically about 5-10 atomic % or even 9-12 atomic %. Because low temperature carburization is a diffusion-based process, the concentration of carbon in the workpiece's surface decreases from a maximum at or very near the outermost surface of the workpiece down to an equilibrium value (which is the carbon concentration in the “native” or untreated metal from which the workpiece is made) in accordance with Fick's law.
  • reference to a carbon concentration of about 2-15 atomic % means that this is the carbon concentration at or near the workpieces surface, with this concentration falling off to the equilibrium value at depth which can be as little as 5 ⁇ from the workpiece's outer surface, but is more typically on the order of 20-50 ⁇ from the workpiece's outer surface. Greater depths of diffused carbon, e.g., as deep as 75 ⁇ or even 100 ⁇ are possible, however.
  • atomic carbon diffuses interstitially into the workpiece surfaces, i.e., carbon atoms travel through the spaces between the metal atoms without significant substitutional diffusion of the metal atoms. Because the processing temperature is low, these carbon atoms form a solid solution with the metal atoms of the workpiece surfaces. They do not react with these metal atoms to form other compounds.
  • Low temperature carburization is therefore different from normal carburization carried out at higher temperatures in which the carbon atoms react to form corrosion-promoting carbide precipitates, i.e., specific metal compounds such as M 23 C 6 (e.g., Cr 23 C 6 or chromium carbide), M 5 C 2 and the like, arranged in the form of discrete phases separate and apart from the metal matrix in which they are contained.
  • specific metal compounds such as M 23 C 6 (e.g., Cr 23 C 6 or chromium carbide), M 5 C 2 and the like, arranged in the form of discrete phases separate and apart from the metal matrix in which they are contained.
  • each of these low temperature interstitial diffusion-based surface treatments can be applied to thin metal workpieces using the technology of this invention to make new products with greater concentrations of the diffused atoms and better properties than available in the past.
  • the present invention will normally be carried on workpieces made from iron or nickel-based alloys. Such materials are well known and described for example in the above-noted U.S. Pat. No. 5,792,282, U.S. Pat. No. 6,093,303, U.S. Pat. No. 6,547,888, EPO 0787817 and Japanese Patent Document 9-14019 (Kokai 9-268364).
  • Particular alloys of interest are steels, especially steels containing 5 to 50, preferably 10 to 40, wt. % Ni. Preferred alloys contain 10 to 40 wt. % Ni and 10 to 35 wt. % Cr. More preferred are the stainless steels, especially the AISI 300 series steels. Of special interest are AISI 301, 303, 304, 309, 310, 316, 316L, 317, 317L, 321, 347, CF8M, CF3M, 254SMO, A286 and AL6XN stainless steels.
  • low temperature carburization in accordance with the present invention can also be practiced on cobalt-based alloys as well as manganese-based alloys.
  • cobalt-based alloys include MP35N and Biodur CMM, while examples of such manganese-based alloys include AISI 201, AISI 203EZ and Biodur 108.
  • phase of the metal being processed in accordance with the present invention is unimportant, as the invention can be practiced on metals of any phase structure including, but not limited to, austenite, ferrite, martensite, duplex metals (e.g., austenite/ferrite), etc.
  • a low temperature interstitial diffusion-based surface treatment is carried out on a “thin” workpiece to produce a “thin” surface-treated product.
  • a workpiece that has been subjected to a low temperature interstitial diffusion-based surface treatment can be considered as having an internal core surrounded by a diffusion-enriched surface or “case”.
  • this carburized surface will normally extend down to a depth of about 20 ⁇ to about 40 ⁇ or even 50 ⁇ from the outermost surface, although greater depths are possible. Because this case depth is extremely thin compared with the overall thickness of the workpiece, the vast majority and indeed essentially all of the article is composed of native metal i.e., metal not infused with additional amounts of interstitial carbon. As a result, the case exerts no noticeable effect on the mechanical properties of the workpiece as a whole.
  • the workpiece being processed is very thin, normally on the order of 0.0004 to 0.01 inch thick ( ⁇ 0.01 to ⁇ 0.25 mm; ⁇ 10 to ⁇ 250 ⁇ ), more typically about 0.001 to 0.003 inch thick ( ⁇ 0.025 to ⁇ 0.08 mm; ⁇ 25 to ⁇ 75 ⁇ ).
  • case thickness becomes significant relative to core thickness, the result of which is that the properties of the workpiece as a whole are indeed influenced by the case.
  • FIGS. 1 and 2 shows the stress/strain relationships exhibit by a number of different AISI 316 stainless steel foils 0.002 in ( ⁇ 0.048 mm; ⁇ 50 ⁇ ) thick which have been low temperature carburized to produce a “thin” surface-treated foil product in accordance with the present invention.
  • the untreated foil represented by Curve A reached its elastic limit at a stress of about 300 MPa (megaPascals).
  • the foils treated in accordance with the present invention, which are represented by Curve B did not reach their elastic limits until the applied stress was about 1200 MPa. This represents a four-fold increase in yield strength with ductility being substantially retained, thereby showing that these treated foils are considerably different materials from the untreated foils from which they were made.
  • the workpieces processed by the present invention are thin, normally on the order of 0.0004 to 0.01 inch thick ( ⁇ 0.01 to ⁇ 0.25 mm; ⁇ 10 to ⁇ 250 ⁇ ), more typically about 0.001 to 0.003 inch thick ( ⁇ 0.024 to ⁇ 0.08 mm; ⁇ 25 to ⁇ 75 ⁇ ).
  • workpieces of greater or lesser thickness can also be processed if desired. What is important is that these workpieces are thin enough, and the low temperature diffusion-based surface treatment carried out long enough, so that the case produced by this surface treatment imparts a not-insignificant change (i.e. ⁇ 10%) to at least one property of the product as a whole as compared with an otherwise identical workpiece from which it is made.
  • thin in relation to a workpiece which is subjected to a low temperature interstitial diffusion surface treatment will be understood to mean a thickness which is small enough so that at least one property of the product produced by the treatment is enhanced by at least 10% as compared with an otherwise identical product made without the surface treatment.
  • foil workpieces and products for the purposes of this invention include foils, wires, powder, platelets and other particulates, for example. Other shapes are also possible.
  • Various different mechanical, electrical and magnetic properties of thin metal workpieces can be enhanced by this invention. Examples include, but are not limited to hardness, yield strength, ultimate tensile strength, elastic limit, electrical resistance and magnetic susceptibility. Moreover, while the above disclosure refers to enhancing at least one of these properties by at least 10%, it should be appreciated that far greater enhancements are possible. For example, electrical resistance can be increased by as much as 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90% or even 100%, typically 15% to 60%. Similarly, yield strength increases by as much as 100%, 200%, 300%, 400% and even 500% are possible. Most significantly, these remarkable enhancement can be achieved without significant reduction in other properties such ductility, etc., as a practical matter.
  • FIGS. 1 and 2 which shows that the foils low temperature carburized in accordance with this invention, Curve B, remained ductile until they ruptured at an elongation of about 20% or more.
  • this elongation at rupture is not as great as that exhibited by the untreated foils of Curve A (about 35% elongation at rupture), it is far greater than that of the conventionally carburized foils (about 5% elongation at rupture), represented by Curve C.
  • the present invention not only achieves a substantial increase in yield strength, electrical resistance and corrosion resistance, but also does so without substantial sacrifice in ductility.
  • shaped metal articles are made by sintering processes using masses of the diffusion-treated thin metal products of this invention as their raw materials.
  • Powder metallurgy techniques for forming shaped metal articles are well known, and any such technique can be used to form shaped metal articles from the diffusion-treated powders, platelets and other particulate thin products of this invention.
  • Analogous sintering processes can also be used to form the thin metal foil products of this invention into shaped articles.
  • Such sintering processes typically involve forming a mass of metallic particles into a desired shape, optionally compacting the mass to desired density (with respect to theoretical) and heating the mass to cause the particles to melt and fuse to one another at their surfaces.
  • Analogous sintering processes can be used to form shaped metal articles from foils. These same processes can be used to form shaped articles of any desired shape from the diffusion-treated thin metal products of this invention regardless of shape, i.e., whether in the form of powder, platelet, other particulate, wire or foil. Such products are unique because they are made from new materials not previously known.
  • Magnetic susceptibility is the degree of magnetization of a material in response to an applied magnetic field.
  • Ferritic and martensitic stainless steels exhibit good, inherent magnetic susceptibility. In contrast, austenitic stainless steels exhibit essentially no magnetic susceptibility.
  • the carbon hardened surfaces produced when austenitic stainless steels and other metals having face centered cubic lattice structures are low temperature carburized do. Accordingly, when a “thin” workpiece made from an austenitic stainless steel or other metal having a face centered cubic lattice structure is low temperature carburized, the “thin” product obtained exhibits significant magnetic susceptibility since its carbon hardened surfaces represent a significant portion of its entire mass.
  • a shaped metal article made from a sintered mass of such a product, as described above also exhibits significant magnetic susceptibility as a whole since the portion of its mass which has been low temperature carburized is significant with respect to its entire mass.

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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)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Powder Metallurgy (AREA)
US11/880,597 2006-07-24 2007-07-23 Metal article with high interstitial content Abandoned US20080023110A1 (en)

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US (1) US20080023110A1 (fr)
EP (1) EP2044236A1 (fr)
JP (1) JP2009544852A (fr)
KR (1) KR20090034390A (fr)
CN (1) CN101490302A (fr)
WO (1) WO2008013765A1 (fr)

Cited By (1)

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CN102676979A (zh) * 2011-03-15 2012-09-19 台耀科技股份有限公司 提升粉末冶金不锈钢强度及硬度的方法

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WO2008124243A1 (fr) * 2007-04-05 2008-10-16 Swagelok Company Articles formés à partir de poudre métallique cémentée à basse température
CN112522661B (zh) * 2020-07-27 2021-06-25 滨中元川金属制品（昆山）有限公司 一种薄型精密紧固件微渗碳工艺

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