US3719518A - Process of forming a carbide layer of vanadium, niobium or tantalum upon a steel surface - Google Patents

Process of forming a carbide layer of vanadium, niobium or tantalum upon a steel surface Download PDF

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US3719518A
US3719518A US00085043A US3719518DA US3719518A US 3719518 A US3719518 A US 3719518A US 00085043 A US00085043 A US 00085043A US 3719518D A US3719518D A US 3719518DA US 3719518 A US3719518 A US 3719518A
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stock
process according
mixture
carbon
group
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N Komatsu
T Arai
M Mizutani
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Toyota Central R&D Labs Inc
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Toyota Central R&D Labs Inc
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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
    • C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
    • C23C12/02—Diffusion in one step
    • 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

Definitions

  • ABSTRACT A process for the surface treatment of an iron or iron alloy stock comprising heating a mixture of boric acid or borate.
  • the present invention can be performed without adding carbon to a mixture in the case when either said stock or said vessel includes carbon.
  • This invention relates to a process for the surface treatment of an iron or ferrous alloy material so as to form thereon a carbide layer of a metal belonging to V- a group of the periodic table.
  • halides are employed asthe coating material source, which necessitates the use of a specifically selected atmosphere furnace of rather complicated design. This kind of furnace, however, suffers appreciable corrosion caused by the attack of the gaseous halogen.
  • the surface of the stock to be coated is liable to become rather rough, and the coated layer consists of a mixed structure of the carbide and the stock material, representing thus a lower grade of surface hardness and anti-wearing performance than a layer exclusively composed of carbide.
  • the coating material is very high in price and the bonding of the coated layer with the mother stock is frequently and appreciable inferior.
  • the object of the present invention is to provide a substantially improved process for the surface treatment of iron and ferrous alloy stocks of the kind above referred to, capable of substantially obviating the aforementioned conventional drawbacks.
  • an iron or ferrous alloy stock is immersed in a fused salt bath containing one or more V-a group elements of the periodic table in the presence of carbon.
  • the carbon may be admixed with the fused salt bath material.
  • the carbon may exist in the stock to be treated. It has been found upon carrying out a large number of practical experiments that in this way, a carbide layer of V-a group element or elements can be definitely formed on the surface of the stock. The thus formed carbide layer represents a high value of hardness and a superior resistance performance against wear.
  • the process according to this invention is thus highly suitable for the surface treatment of dies, jigs and the like. It is highly productive, and it has been ascertained that the carbide layer thus obtained is strongly and tightly bonded to the surface of the mother stock and has, in addition, a dense and continuous structure, thus obviating substantially the above mentioned various conventional drawbacks.
  • boric acid B 0 and/or borate such as borax (Na B,0-,)
  • V-a group element or elements As the bath material, a mixture of boric acid (B 0 and/or borate such as borax (Na B,0-,), with V-a group element or elements is used.
  • the borate can fuse at a relatively low temperature, and acts as a kind of flux capable of keeping the stock surface in its clean and fresh state and suppressing the formation of oxide thereon.
  • V-a group element or elements can be fused in the molten state of borate.
  • V-a group elements one or more elements of vanadium (V), niobium (Nb) and tantalum (Ta), or in the form of its compound such as its ferro-alloy can be used, 5 percent by weight of V-a group element in the fused bath being sufficient.
  • the V-a group element may be added to the fused salt bath in a quantity between about lwt. percent. With use of a lesser quantity of the V-a group element than 1 wt. percent, the speed of the formation of the carbide layer would be too slow to be accepted for the practical purpose. Too much addition of V-a group element (higher than 70 wt.
  • the carbon per se or its compound may be intentionally admixed with the molten salt bath material. Under circumstances, a graphite crucible or a bath vessel made of a predominantly carbon-containing substance may be used as the carbon source.
  • the stock to be treated upon consists of a carboncontaining ferrous material, such as tool steel, structual alloy steel, cast iron or the like, the stock per se can be utilized as the carbon source.
  • low carbon stock such as of stainless steel, low carbon steel of a very low carbon content
  • a thick layer of carbide it is highly preferable to case-harden in advance of the bath treatment, the stock so as to increase the carbon content in the surface thereof, in place of otherwise increasing of the treating temperature and/or prolongation of the treating period.
  • the carbon necessary for the formation of carbide layer is introduced intentionally into the molten salt bath, it may preferably amount to about 0.03 wt. percent or higher.
  • the carbon supply quantity should exceed its dissolving extremity in the molten salt bath, a carbonaceous layer will form on the free surface of the molten bath, thus taking no part in the formation of the desirous carbide layer, but it serves to interrupt positively communication of the ambient atmosphere with the bath material.
  • an invasion of oxygen into the bath is positively prevented by the presence of the bath-covering carbonaceous layer, thereby a favorable effect being provided in the progress of the carbide formation on the stock under treatment.
  • the treating temperature may theoretically extend from the fusing point of the bath material to the melting point of the stock to be treated upon. In practice, however, it may preferably selected to about 800-1,l00C, taking the forming velocity of the carbide layer and embrittlement caused by grain growth and the like into account.
  • borax When borax is used as the molten bath material, it may preferably be admixed with one or more compounds selected from the group comprising halides such as sodium-chloride (NaCl), potassium chloride (KCl), sodium fluoride (NaF); oxides such as phosphorus oxide (P or the like; hydroxides such as sodium hydroxide ('NaOI-I), potassium hydroxide (KOI-l); sulfates; carbonates; and nitrates, so as to lower the fusing temperature of the bath material, in consideration of the melting point of borax being about 740C which lies above the transformation point of steeLIn most steel stocks when treated at a bath temperature above the transformation point of steel for quicker formation of the carbide layer, distortion may be liable to occur by virtue of the transformation of steel and the distortion mustbe naturally be avoided by lowering the adopted higher bath temperature.
  • halides such as sodium-chloride (NaCl), potassium chloride (KCl), sodium fluoride (Na
  • the treating time period depends upon the thickness of the carbide layer to be formed.
  • the treatment shorter than an hour will, however, provide no practically acceptable formation of carbide layer, although the final determination of the treating period depends upon the treating temperature.
  • the thickness of carbide layer With increase of the treating period, the thickness of carbide layer will be increased correspondingly. In practice, an acceptable thickness of carbide layer can be realized within 30 hours or shorter time period.
  • the process according to this invention can be carried into effect either under air atmosphere or inert gas atmosphere.
  • FIGS. 1-6 are several micrographic representations reproduced, however, manually, for a more clearer showing of several samples of the carbide layer formed in accordance with the novel teaching of this invention.
  • FIG. 7 is a chart illustrative of experimental wear-resisting tests performed on preferred samples of the car- EXAMPLE 1 a 50 wt. percent; 50 wt. percent mixture, 150 grs., of borax and ferro-niobium (Fe-Nb) powder containing niobium 59 wt. percent and tantalum 3.6 wt. percent, was introduced into a graphite crucible and heated up to 900C, and then a specimen, 5 mm thick, 12mm wide and 70 mm long, made of a metal, JIS SKDl (a1- loy tool steel, C 1.80-2.40 wt. percent; Si less than 0.40 wt.
  • JIS SKDl a1- loy tool steel, C 1.80-2.40 wt. percent; Si less than 0.40 wt.
  • EXAMPLE 2 A powder mixture, 150 grs., consisting of 50 wt. percent of borax and 50 wt. percent of ferro-vanadium (including 52 wt. percent of vanadium) was introduced in a graphite crucible and a specimen consisting of a steel, JIS SKDl, was treated under the same treating conditions as in the foregoing Example 1.
  • the formed layer on the specimen amounted in its thickness to about 18 microns. It was smooth and pinhole-free. 7
  • the layer consisted of vanadium carbide (VC). From an electron probe microanalysis, vanadium and carbon were detected.
  • curve 1 concerns with the first test specimen of Example 1.
  • Curve 2 relates to the second test specimen of Example 2.
  • Curve 3 relates to the specimen as a difference.
  • test specimens of SKDl-material are immersed in a molten salt bath containing borax and a V-a group element such as vanadium, niobium and tantalum placed within a bath vessel made of a material substantially including carbon, a layer of carbide of the V-a group element is formed.
  • a V-a group element such as vanadium, niobium and tantalum
  • EXAMPLE 3 A graphite crucible was used as in the foregoing Examples, and a fused salt bath mixture of borax or boric acid and V-a group element such as vanadium or a ferro-alloy such as ferro-niobium and ferro-vanadium was prepared in the crucible, and then ferrous specimens (each being 14 mm in diameter and 20 mm long) were treated as before.
  • test specimens The several test specimens, bath compositions, treating temperatures are shown in the following table:
  • EXAMPLE 5 A powder mixture, 100 grs., consisting of 50 wt. percent borax, 30 wt. percent metallic vanadium (92 wt. percent vanadium) and 20 wt. percent sodium cyanate (NaCN), was charged in a stainless steel crucible and a same test specimen was used for the similar treatment.
  • EXAMPLE 6 A powder mixture, grs., consisting of 70 wt. percent borax and 30 wt. percent of ferro-vanadium (52 wt. percent vanadium) was charged in a graphite crucible and heated up to 1,000C. A pure iron specimen having the same dimensions as in the Example 4 was immersed in the fused salt bath and kept therein for 8 hours. Then, it was taken out of the bath and aircooled. Salts deposited on the surface of the specimen were removed in a boiling water bath.
  • vanadium carbide layer can be formed effectively on the specimen surface.
  • EXAMPLE 7 A powder mixture grs., consisting of 70 wt. percent borax and 30 wt. percent ferro-niobium powder (59 wt. percent niobium and 3.6 wt. percent tantalum) was charged in a stainless steel crucible and heated up to 1,000C. A test specimen of HS 8K2 (carbon tool steel, C:l.l0-l.30 wt. Sizless than 0.35 wt. Mn: less than 0.50 wt. Pzless than 0.03 wt. S: less than 0.03 wt. was introduced in the molten bath and kept therein for 8 hours, taken out therefrom and then aircooled. Deposited salts were removed in a boiling water bath.
  • EXAMPLE 8 A powder mixture of 70 wt. percent borax and 30 wt. percent of ferro-vanadium (52 wt. percent vanadium) was used. Further treating conditions were same as in the foregoing Example 7. Test specimen was of 11S 8K2. In this way, a carbide layer, about 35 microns thick, was formed on the specimen in an effective manner. VC-diffraction was observed.
  • the process for the formation of a carbide of an element selected from the V-a group on an iron stock can be brought into effect, when necessary, without use of a specific inert gas atmosphere.
  • the present invention provides a perfectly unique process for the formation of carbide layer of V-a group element on an iron or iron alloy stock only immersing the latter in a molten salt bath containing the Va-series element, wherein the supply of the necessary carbon constituent can be performed by an intentional introduction thereof from outside of the bath into the latter or reliance made upon the bath vessel per se for this purpose when the latter has been made of carbon or carbon-containing substance.
  • the stock per se can be utilized as such carbon source, when it contains a reasonable amount of carbon.
  • a process for the surface treatment of an iron or iron alloy stock comprising the steps of heating a mixture consisting essentially of boric acid or a borate, at least one element of group V-a of the Periodic table consisting of vanadium, niobium and tantalum or a substance containing the same, and carbon or a carboncontaining substance to its fusing state in a bath vessel, and immersing the stock'in the molten bath of said mixture, thereby forming a carbide layer of said element on the stock thus treated.
  • a process for the surface treatment of an iron or iron alloy stock comprising the steps of heating a mixture consisting essentially of boric acid or a borate and at least one element of Group V-a of the Periodic table consisting of vanadium, niobium and tantalum or a substance containing the same, to its fusing state in a vessel containing carbon as its main ingredient, and immersing the stock in the molten bath of said mixture, thereby forming a carbide layer of said element on the stock thus treated.
  • a process for the surface treatment of an iron or iron alloy stock comprising the steps of heating a mixture consisting essentially of boric acid or a borate, at least one element of Group V-a of the Periodic table consisting of vanadium, niobium and tantalum or a substance containing the same to its fusing state in the vessel, and immersing an iron or iron alloy stock containing carbon in the molten bath of said mixture, thereby forming a carbide layer of said element on the stock thus treated.
  • a process according to claim 12, wherein said stock is selected from the group consisting of high-carbon steel, high-carbon alloy steel and cast iron.

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
US00085043A 1969-11-01 1970-10-29 Process of forming a carbide layer of vanadium, niobium or tantalum upon a steel surface Expired - Lifetime US3719518A (en)

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3912827A (en) * 1973-11-13 1975-10-14 Toyota Chuo Kenkyusko Kk Method for forming a chromium carbide layer on the surface of an iron, ferrous alloy or cemented carbide article
US3922405A (en) * 1973-04-12 1975-11-25 Toyoda Chuo Kenkyusho Kk Method for forming of a carbide layer of a V-a group element of the periodic table on the surface of an iron, ferrous alloy or cemented carbide article
US3930060A (en) * 1972-05-04 1975-12-30 Toyoda Chuo Kenkyusho Kk Method for forming a carbide layer of a V-a group element of the periodic table on the surface of an iron, ferrous alloy or cemented carbide article
US4158578A (en) * 1977-05-09 1979-06-19 Kabushiki Kaisha Toyota Chuo Kenkyusho Method for forming a carbide layer of a Va-Group element of the periodic table or chromium on the surface of a ferrous alloy article
US4202705A (en) * 1977-06-30 1980-05-13 Kabushiki Kaisha Toyoto Chuo Kenkyusho Treating bath, forming a mixed carbide layer of Va-Group elements on a ferrous alloy surface and resulting product
US4400222A (en) * 1980-06-17 1983-08-23 Hitachi Metals, Ltd. Method for treating surfaces
US4400224A (en) * 1981-04-20 1983-08-23 Kabushiki Kaisha Toyota Chuo Kenkyusho Method for forming a carbide layer on the surface of a ferrous alloy article or a cemented carbide article
US4440581A (en) * 1980-07-02 1984-04-03 Degussa Aktiengesellschaft Process for the production of vanadium carbide coatings on iron
US4804445A (en) * 1986-12-17 1989-02-14 Kabushiki Kaisha Toyota Chuo Kenkyusho Method for the surface treatment of an iron or iron alloy article
US5234721A (en) * 1989-05-26 1993-08-10 Rostoker, Inc. Method for forming carbide coating on various metals and their alloys
US20040018905A1 (en) * 2002-07-23 2004-01-29 Isamu Okabe Roller chain
US20110132769A1 (en) * 2008-09-29 2011-06-09 Hurst William D Alloy Coating Apparatus and Metalliding Method
EP2829635A1 (en) 2013-07-23 2015-01-28 Semih Oncel Method for controlled production of diffusion based coatings by vacuum cathodic arc systems
CN116332678A (zh) * 2023-05-30 2023-06-27 中南大学 一种在碳材料表面制备碳化钽涂层的方法
CN116397228A (zh) * 2023-06-06 2023-07-07 中南大学 一种在石墨表面制备合金/碳化钽复合涂层的方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5210935B1 (enrdf_load_stackoverflow) * 1971-03-09 1977-03-28

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US1796248A (en) * 1929-01-12 1931-03-10 Roessler & Hasslacher Chemical Process for the cementation of iron and steel
GB625192A (en) * 1946-03-23 1949-06-23 Du Pont Improvements in or relating to the carburisation of steel
US2492805A (en) * 1946-12-26 1949-12-27 Du Pont Casehardening composition
GB637635A (en) * 1948-04-22 1950-05-24 John Wilfred Britton Improvements in or relating to the case hardening of steel
GB646645A (en) * 1947-01-13 1950-11-29 Diffusion Alloys Ltd A process for simultaneously diffusing metals and carbon into iron and steel
US2568860A (en) * 1948-01-22 1951-09-25 Du Pont Process for the carburization of ferrous metals
US2694647A (en) * 1952-02-07 1954-11-16 Norman W Cole Process for applying fused metal coating onto metal base and adhesive used therein
GB722915A (en) * 1951-01-17 1955-02-02 Metro Cutanit Ltd Process for producing a hard and wear-resistant surface on ferrous bodies
US2846345A (en) * 1955-03-25 1958-08-05 Ici Ltd Method of carburizing steel and steel alloys, and fused salt bath thereof
US2885301A (en) * 1956-08-02 1959-05-05 Metal Diffusions Inc Chromizing coating
US2926111A (en) * 1958-04-03 1960-02-23 Donald G Schweitzer Method of forming a protective coating on ferrous metal surfaces
US2929741A (en) * 1957-11-04 1960-03-22 Morris A Steinberg Method for coating graphite with metallic carbides
US3203811A (en) * 1960-10-20 1965-08-31 Boller Dev Corp Molten transition metal plating baths containing zinc ammine chlorides

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1796248A (en) * 1929-01-12 1931-03-10 Roessler & Hasslacher Chemical Process for the cementation of iron and steel
GB625192A (en) * 1946-03-23 1949-06-23 Du Pont Improvements in or relating to the carburisation of steel
US2492805A (en) * 1946-12-26 1949-12-27 Du Pont Casehardening composition
GB646645A (en) * 1947-01-13 1950-11-29 Diffusion Alloys Ltd A process for simultaneously diffusing metals and carbon into iron and steel
US2568860A (en) * 1948-01-22 1951-09-25 Du Pont Process for the carburization of ferrous metals
GB637635A (en) * 1948-04-22 1950-05-24 John Wilfred Britton Improvements in or relating to the case hardening of steel
GB722915A (en) * 1951-01-17 1955-02-02 Metro Cutanit Ltd Process for producing a hard and wear-resistant surface on ferrous bodies
US2694647A (en) * 1952-02-07 1954-11-16 Norman W Cole Process for applying fused metal coating onto metal base and adhesive used therein
US2846345A (en) * 1955-03-25 1958-08-05 Ici Ltd Method of carburizing steel and steel alloys, and fused salt bath thereof
US2885301A (en) * 1956-08-02 1959-05-05 Metal Diffusions Inc Chromizing coating
US2929741A (en) * 1957-11-04 1960-03-22 Morris A Steinberg Method for coating graphite with metallic carbides
US2926111A (en) * 1958-04-03 1960-02-23 Donald G Schweitzer Method of forming a protective coating on ferrous metal surfaces
US3203811A (en) * 1960-10-20 1965-08-31 Boller Dev Corp Molten transition metal plating baths containing zinc ammine chlorides

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3930060A (en) * 1972-05-04 1975-12-30 Toyoda Chuo Kenkyusho Kk Method for forming a carbide layer of a V-a group element of the periodic table on the surface of an iron, ferrous alloy or cemented carbide article
US3922405A (en) * 1973-04-12 1975-11-25 Toyoda Chuo Kenkyusho Kk Method for forming of a carbide layer of a V-a group element of the periodic table on the surface of an iron, ferrous alloy or cemented carbide article
US3912827A (en) * 1973-11-13 1975-10-14 Toyota Chuo Kenkyusko Kk Method for forming a chromium carbide layer on the surface of an iron, ferrous alloy or cemented carbide article
US4158578A (en) * 1977-05-09 1979-06-19 Kabushiki Kaisha Toyota Chuo Kenkyusho Method for forming a carbide layer of a Va-Group element of the periodic table or chromium on the surface of a ferrous alloy article
US4202705A (en) * 1977-06-30 1980-05-13 Kabushiki Kaisha Toyoto Chuo Kenkyusho Treating bath, forming a mixed carbide layer of Va-Group elements on a ferrous alloy surface and resulting product
US4400222A (en) * 1980-06-17 1983-08-23 Hitachi Metals, Ltd. Method for treating surfaces
US4440581A (en) * 1980-07-02 1984-04-03 Degussa Aktiengesellschaft Process for the production of vanadium carbide coatings on iron
US4400224A (en) * 1981-04-20 1983-08-23 Kabushiki Kaisha Toyota Chuo Kenkyusho Method for forming a carbide layer on the surface of a ferrous alloy article or a cemented carbide article
US4804445A (en) * 1986-12-17 1989-02-14 Kabushiki Kaisha Toyota Chuo Kenkyusho Method for the surface treatment of an iron or iron alloy article
US5234721A (en) * 1989-05-26 1993-08-10 Rostoker, Inc. Method for forming carbide coating on various metals and their alloys
US20040018905A1 (en) * 2002-07-23 2004-01-29 Isamu Okabe Roller chain
US20060032207A1 (en) * 2002-07-23 2006-02-16 Tsubakimoto Chain Co. Process for making a roller chain
US20110132769A1 (en) * 2008-09-29 2011-06-09 Hurst William D Alloy Coating Apparatus and Metalliding Method
EP2829635A1 (en) 2013-07-23 2015-01-28 Semih Oncel Method for controlled production of diffusion based coatings by vacuum cathodic arc systems
CN116332678A (zh) * 2023-05-30 2023-06-27 中南大学 一种在碳材料表面制备碳化钽涂层的方法
CN116332678B (zh) * 2023-05-30 2023-08-11 中南大学 一种在碳材料表面制备碳化钽涂层的方法
CN116397228A (zh) * 2023-06-06 2023-07-07 中南大学 一种在石墨表面制备合金/碳化钽复合涂层的方法
CN116397228B (zh) * 2023-06-06 2023-08-22 中南大学 一种在石墨表面制备合金/碳化钽复合涂层的方法

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CA935074A (en) 1973-10-09
FR2068376A5 (enrdf_load_stackoverflow) 1971-08-20
GB1309155A (en) 1973-03-07
DE2053063B2 (de) 1976-06-10
DE2053063A1 (de) 1971-05-13

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