US3546921A - Method of producing an initial thermal arrest in the cooling curve of hypereutectic cast iron - Google Patents

Method of producing an initial thermal arrest in the cooling curve of hypereutectic cast iron Download PDF

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US3546921A
US3546921A US658838A US3546921DA US3546921A US 3546921 A US3546921 A US 3546921A US 658838 A US658838 A US 658838A US 3546921D A US3546921D A US 3546921DA US 3546921 A US3546921 A US 3546921A
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sample
cast iron
carbon equivalent
cooling curve
temperature
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US658838A
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William T Bourke
Spencer Harris
Tom C Muff
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Harris Muff Inc
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Harris Muff Inc
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C1/00—Refining of pig-iron; Cast iron
    • C21C1/10—Making spheroidal graphite cast-iron
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20—Metals
    • G01N33/205—Metals in liquid state, e.g. molten metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S73/00—Measuring and testing
    • Y10S73/09—Molten metal samplers

Definitions

  • This invention relates to the monitoring of constituents of molten cast iron, and has for an object a method of determining the carbon equivalent of the iron as it existed in the molten state prior to processing and/or the me chanical and physical properties of the iron.
  • the principle of carbon equivalent determination by pyrometry is based upon the accurate measurement of the initial or liquidus thermal arrest temperature which occurs in a sample of molten cast iron as it begins to freeze.
  • the carbon equivalent (CE) may be defined a the total percent of carbon plus one-third of the total percent of silicon plus one-third of the total percent of phosphorus contained in a sample of cast iron, based upon the total weight of the sample.
  • the liquidus temperature for hypoeutectic cast irons i.e., cast iron having a carbon equivalent less than 4.35 percent, is easily observed. The heat liberated when austenite starts to precipitate produces an isothermal arrest of the cooling curve.
  • the temperature at which the liquidus thermal arrest occurs is related directly to the carbon equivalent of the metal and is not affected appreciably by normal amounts of manganese, chromium, nickel or other common contaminating elements.
  • the measurement of liquidus thermal arrest is consistently reproducible, and in actual foundry use is much faster and more reliable than chemical analysis.
  • the carbon and silicon contents are the two main variables in cast iron. as the phosphorus content is generally present in quantities low enough to be relatively ineffective for any given carbon equivalent.
  • the silicon content can be estimated on the basis of chill tests, thus leaving only the carbon content to be determined.
  • the carbon equivalent can be calculated from its relationship to the carbon equivalent. With this knowledge of the carbon content, a foundry will be aware, before pouring, whether the composition of the cast iron meets the required specifications.
  • a suitable expendable phase change detector device for use in determining the carbon equivalent of molten cast United States Patent 0 3,546,921 Patented Dec. 15, 1970 "ice iron is disclosed in U.S. Pat. No. 3,267,732, reissued a U.S. Re. Pat. No. 26,409.
  • the carbon equivalent technique involving the cooling curve test is also described in an article entitled Carbon Equivalent in Sixty Seconds, which appeared in the March 1962 issue of Modern Castings, at pages 37-39.
  • the present invention enables the carbon equivalent technique to be extended to hypereutectic iron up to the kish point, i.e., the temperature at which free graphite forms and floats out of molten hypereutectic cast iron as it cools, without resort to any dilution technique which changes the carbon equivalent of the cast iron sample from that of the melt.
  • Hypereutectic cast iron tends to product stable graphite when cooling from the melt to the freezing temperature of the cemenite through the formation of unstable iron carbide which immediately decomposes to iron and carbon (graphite). This causes complex heat effects resulting in a poorly defined arrest of the cooling curve. It has been discovered, however, that when the carbide is stabilized to retard complete graphite formation, simple freezing of iron carbide is achieved, causing an arrest of the cooling curve at the carbide forming temperature due to the higher heat of formation of iron carbide than of graphite.
  • any material having the characteristic of retarding primary graphite formation during cooling of the molten sample of the hypereutectic cast iron to its freezing temperature, which is inert with respect to the carbon equivalent of the hypereutectic cast iron melt with which it is combined (in the sense that it does not change the carbon equivalent of the sample from that of the melt) may be used as a stabilizer in the practice of the invention.
  • stabilizer characterized by a high degree of carbide stabilizing power are readily soluble in and dispersable throughout the molten sample of iron and will produce a consistent, discernible thermal arrest temperature when the iron carbide transformation occurs.
  • Stabilizers exhibiting the foregoing characteristics include bismuth, boron, cerium, lead, magnesium, and tellurium. Such tabilizers need not be combined with the molten hypereutectic cast iron sample in elemental form but may be added in compound form, or in mixtures with other materials which do not change the carbon equivalent of the cast iron sample from that of the melt.
  • boron may be added in the form of ferroboron (FeB).
  • Cerium may be added in the form of misch metal (a mixture of rare earth elements, atomic numbers 57 through 71, in metallic form).
  • Magnesium may be added in the form of copper-magnesium (Cu-Mg) with the magnesium being about percent by weight.
  • graphitizing materials i.e., those promoting graphite formation during the Cooling of the hypereutectic cast iron sample should be avoided in the practice of the invention.
  • a material such as ferrosilicon (FeSi) is unsuitable since it not only promotes graphitization but also changes the carbon equivalent of the cast iron sample from that of the melt.
  • the amount of stabilizer used in the practice of the invention may vary within wide limits depending upon the particular stabilizer used, the carbon content of the sam ple, and the amount and kind of other constituents of the molten sample. Satisfactory curves may be obtained from cooling samples of cast iron containing as little as 0.05 weight percent (based upon the weight of the sample) of stabilizer.
  • the amount of stabilizer advantageously employed is the minimum amount required to obtain the desired retardation of primary graphite formation and accompanied arrest of the cooling curve at the carbide forming temperature. Although amounts of stabilizer as high a 0.4 percent have successfully been used, lesser amounts are generally preferred.
  • the addition of the stabilizers to molten cast iron samples in accordance with the invention may be accomplished in any manner so long as the temperature of the molten sample at the time of stabilizer addition is sufiiciently high to afford the production of the desired cooling curve.
  • the stabilizer may be added in pellet or particulate form to the molten sample immediately after after the sample is poured.
  • the stabilizer can be added to the sampling device prior to the introduction of the molten sample.
  • Other methods of combining the stabilizer with the sample will readily occur to those skilled in the art.
  • FIG. 1 is a cooling curve of a sample of hypereutectic cast iron produced in accordance with the present invention
  • FIG. 2 is a cooling curve of a sample of hypereutectic cast iron having the same composition as the sample of FIG. 1 but poured in conventional manner without an additive;
  • FIG. 3 is a graph showing the relationship of percent carbon equivalent of hypereutectic cast iron to initial thermal arrest temperature using carbide-stabilizing additives in accordance with the present invention.
  • FIG. 1 there is illustrated a cooling curve of a sample of hypereutectic cast iron obtained in accordance with the present invention by combining with the sample while in liquid state a stabilizer having the characteristic of retarding primary graphite formation during cooling of the sample to the freezing temperature.
  • thermocouple of chromel-alumel wires extends through a wall thereof and is adapted to have its hot junction completely surrounded by the sample when poured into the cup and below any shrinkage cavity formed in the sample upon cooling.
  • the thermocouple is adapted to be connected to a suitable chart recorder which traces the cooling curve of the sample as its temperature cools.
  • the electrical connection between the thermocouple of the detector and the temperature measuring circuit of the recorder is completed by plugging the contacts of the detector into he mating contacts of a stand which is adapted to support the detector in vertical position for receiving the sample.
  • cerium in the form of a one-gram pellet of mischmetal, was in serted in the cup prior to pouring the molten sample into the cup.
  • the sample had a Weight of about 500 grams.
  • the amount of stabilizer may vary throughout a wide range. For example, satisfactory curves have been produced by the addition of as little as one-fourth gram of mischmetal, and as much as two grams, to a SOD-gram molten sample of hypereutectic cast iron including 4.2 percent C, and 1.5 percent Si.
  • a photomicrograph of the microstructure of a picrol etched sample of hypereutectic cast iron having the cooling curve illustrated in FIG. 1 showed the existence of carbon (graphite) in relatively small amounts.
  • FIG. 2 there is illustrated a cooling curve of a hypereutectic cast iron sample having the same composition and poured from the same ladle as the sample of FIG. 1 but poured into the cup of a carbon equivalent detector without the addition of a stabilizer.
  • This sample was poured concurrently with the sample of FIG. 1 but the cooling curve obtained from the sample not containing the stabilizer, as shown in FIG. 2, did not show a useful thennal arrest above the eutectic temperature arrest.
  • a photomicrograph of the microstructure of a picrol etched sample of hypereutectic cast iron which produced the cooling curve of FIG. 2 showed worm-like graphite flakes long and massive as compared to short and fine graphite flakes of the etched sample which produced the curve of FIG. 1, thus indicating the effect of the mischmetal additive in inhibiting or retarding the formation and/or growth of graphite during cooling of the sample to the freezing temperature.
  • the initial thermal arrest in the cooling curve of a sample of hypereutectic cast iron may be produced with various stabilizing additives having the characteristic of retarding primary graphite formation during cooling of the sample to the freezing temperature.
  • various stabilizers have been used to produce thermal arrest temperatures in samples of hypereutectic cast iron having percent carbon equivalent ranging from the eutectic point at 4.35 percent up to about 4.95 percent. The percent carbon equivalents for these various samples were determined from chemical analysis. By plotting the thermal arrest temperatures versus percent carbon equivalent of the samples, the curve of FIG. 3 was produced.
  • the following table of data shows the carbon equivalent of hypereutectic cast iron as determined from the correlation data of FIG. 3 and using carbide-stabilizing additives as compared to the percent carbon equivalent determined by chemical analysis.
  • phase-change detector device of the type disclosed in the aforesaid Pat. 3,267,732 and Re. 26,409 has been referred to specifically in describing the present invention, it is to be understood that any suitable phase-change detector device may be used.
  • Such detector devices will normally comprise a cup member open at the top for receiving the molten sample of cast iron and having a temperature-responsive means extending into the cup for disposition below the surface of the sample so that it may sense the temperature change of the sample as it cools.
  • the temperature sensing means may be of any suitable type, but will preferably be in the form of a thermocouple comprised of suitable materials depending upon the temperatures to be encountered.
  • Other suitable carbon equivalent detector devices are disclosed in US. Pat. No. 3,321,973, British Pat. No. 944,302 and the February 1962 article from Modern Castings entitled Gray Cast Iron Control By Cooling Curve Techniques, pages 91 to 98.
  • a method of producing an initial thermal arrest in the cooling curve of a possibly hypereutectic cast iron said curve being obtained by substantially continuously measuring and plotting a curve of the temperature while a sample of said iron is cooling from a molten to a solid state which comprises, adding to the sample of molten cast iron prior to any substantial cooling thereof a material inert with respect to the carbon equivalent thereof, in the sense that it does not change the carbon equivalent of the sample from that of the melt, which material retards primary graphite formation during cooling of said molten sample of said iron to its freezing temperature to insure an arrest of the cooling curve of said sample at the carbide forming temperature.
  • the added material includes at least one member of the group consisting of bismuth, boron, cerium, lead, magnesium, and tellurium.
  • step of adding to the sample a material inert with respect to the carbon equivalent of said molten cast iron is effected by including a quantity of said material on the inner surfaces of an open ended mold in which said molten sample is to be cast so that addition takes place when said sample is poured into said mold.
  • a method for producing an initial thermal arrest in the cooling curve of a sample of molten hypereutectic cast iron comprising sampling the melt, and
  • a method of determining the carbon equivalent of molten cast iron which consists in determining the temperature of the thermal arrest point on the cooling curve for a sample of said molten cast iron which corresponds to the liquidus temperature wherein identification of the arrest point is facilitated by the addition to said sample of said molten cast iron of a material inert with respect to the carbon equivalent of said molten cast iron and which functions as a carbide stabilizer.

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  • Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Biochemistry (AREA)
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  • Investigating And Analyzing Materials By Characteristic Methods (AREA)
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  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
US658838A 1967-08-07 1967-08-07 Method of producing an initial thermal arrest in the cooling curve of hypereutectic cast iron Expired - Lifetime US3546921A (en)

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JP (1) JPS5036199B1 (xx)
BE (1) BE719176A (xx)
CH (1) CH530002A (xx)
DE (1) DE1798004C3 (xx)
DK (1) DK143916C (xx)
ES (1) ES356928A1 (xx)
FI (1) FI49320C (xx)
FR (1) FR1579162A (xx)
GB (1) GB1221129A (xx)
NL (1) NL145047B (xx)
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Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4846393A (xx) * 1971-10-11 1973-07-02
US3774441A (en) * 1971-05-06 1973-11-27 Edelstahl Kombinet Hennigsdorf Method and apparatus for the thermal analysis of metallic melts
US3824837A (en) * 1968-11-30 1974-07-23 Nippon Kokan Kk Method of rapidly determining the solidus line of molten steel
US3891834A (en) * 1974-05-22 1975-06-24 Ford Motor Co Cooling curve computer
US3946594A (en) * 1973-10-02 1976-03-30 Electro-Nite Co. Disposable phase change device
US4008604A (en) * 1976-04-07 1977-02-22 Deere & Company Determination of carbon analysis in irons
US4046509A (en) * 1970-04-27 1977-09-06 Stig Lennart Backerud Method for checking and regulating the conditions of crystallization in the solidification of melts
US4059996A (en) * 1975-11-20 1977-11-29 Electro-Nite Co. Molten metal sample cup containing blob for promoting carbide formation
US4166738A (en) * 1976-09-09 1979-09-04 Electro-Nite Co. Method for the treatment of nodular or vermicular cast iron samples
US4274284A (en) * 1980-04-14 1981-06-23 Leeds & Northrup Company Expandable phase change detector device
EP0034766A2 (de) * 1980-02-20 1981-09-02 Electro-Nite N.V. Verfahren zur Entnahme von Proben aus Roheisen-Schmelzen
US4515485A (en) * 1983-01-21 1985-05-07 Electro-Nite Co. Molten metal sample cup
US4913878A (en) * 1988-02-05 1990-04-03 General Signal Corporation Method of testing the magnesium content of magnesium-treated cast iron
EP0436063A1 (en) * 1990-01-05 1991-07-10 Heraeus Electro-Nite International N.V. Method and apparatus for introducing uniform quantities of a material into a metallurgical sample
US5447080A (en) * 1993-05-26 1995-09-05 Midwest Instrument Co., Inc. Additive for molten metal sampler
AU664534B2 (en) * 1990-05-16 1995-11-23 Metec Corporation Method of determining the carbon equivalent, carbon content and silicon content of molten cast iron
US5503475A (en) * 1992-10-23 1996-04-02 Metec Corporation Method for determining the carbon equivalent, carbon content and silicon content of molten cast iron
US5948350A (en) * 1998-02-11 1999-09-07 Midwest Instrument Co., Inc. Device for dispensing additive in molten metal sample mold
FR2777995A1 (fr) * 1998-04-23 1999-10-29 Nippon Sublance Probe Engineer Procede d'analyse thermique de fonte a graphite spheroidal
US6155122A (en) * 1998-04-07 2000-12-05 Midwest Instruments Co., Inc. Additive for molten metal sampler
US20100000303A1 (en) * 2006-09-29 2010-01-07 Anant Kashinath Kakatkar Apparatus and method for determining the percentage of carbon equivalent, carbon and silicon in liquid ferrous metal
EP2733488A1 (en) 2012-11-15 2014-05-21 Heraeus Electro-Nite International N.V. Detection device for molten metal
EP3339848A1 (en) * 2016-12-23 2018-06-27 Casa Maristas Azterlan Method to determine the carbon equivalent content of a cast iron alloy having a hypereutectic composition and equipment to carry it out

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2380552A1 (fr) * 1977-02-09 1978-09-08 Electro Nite Procede pour la determination de la teneur en carbone et de l'equivalent carbone de fontes nodulaires
SE469712B (sv) * 1990-10-15 1993-08-30 Sintercast Ltd Foerfarande foer framstaellning av gjutjaern med kompakt grafit
DE102011055950B4 (de) 2011-12-01 2020-03-26 Fritz Winter Eisengiesserei Gmbh & Co. Kg Probentiegel und Verfahren zur Thermoanalyse einer Gießschmelzenprobe

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3375106A (en) * 1965-02-02 1968-03-26 American Standard Inc Determination of carbon equivalence of hypereutectic cast iron
US3415307A (en) * 1966-03-03 1968-12-10 United States Pipe Foundry Process for casting ductile iron

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3375106A (en) * 1965-02-02 1968-03-26 American Standard Inc Determination of carbon equivalence of hypereutectic cast iron
US3415307A (en) * 1966-03-03 1968-12-10 United States Pipe Foundry Process for casting ductile iron

Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3824837A (en) * 1968-11-30 1974-07-23 Nippon Kokan Kk Method of rapidly determining the solidus line of molten steel
US4046509A (en) * 1970-04-27 1977-09-06 Stig Lennart Backerud Method for checking and regulating the conditions of crystallization in the solidification of melts
US3774441A (en) * 1971-05-06 1973-11-27 Edelstahl Kombinet Hennigsdorf Method and apparatus for the thermal analysis of metallic melts
JPS4846393A (xx) * 1971-10-11 1973-07-02
JPS5325274B2 (xx) * 1971-10-11 1978-07-26
US3946594A (en) * 1973-10-02 1976-03-30 Electro-Nite Co. Disposable phase change device
US3891834A (en) * 1974-05-22 1975-06-24 Ford Motor Co Cooling curve computer
US4059996A (en) * 1975-11-20 1977-11-29 Electro-Nite Co. Molten metal sample cup containing blob for promoting carbide formation
US4008604A (en) * 1976-04-07 1977-02-22 Deere & Company Determination of carbon analysis in irons
US4166738A (en) * 1976-09-09 1979-09-04 Electro-Nite Co. Method for the treatment of nodular or vermicular cast iron samples
EP0034766A2 (de) * 1980-02-20 1981-09-02 Electro-Nite N.V. Verfahren zur Entnahme von Proben aus Roheisen-Schmelzen
EP0034766A3 (de) * 1980-02-20 1982-05-12 Electro-Nite N.V. Verfahren zur Entnahme von Proben aus Roheisen-Schmelzen
US4362562A (en) * 1980-02-20 1982-12-07 Electro-Nite Method for taking samples from pig-iron melts
US4274284A (en) * 1980-04-14 1981-06-23 Leeds & Northrup Company Expandable phase change detector device
US4515485A (en) * 1983-01-21 1985-05-07 Electro-Nite Co. Molten metal sample cup
US4913878A (en) * 1988-02-05 1990-04-03 General Signal Corporation Method of testing the magnesium content of magnesium-treated cast iron
EP0436063A1 (en) * 1990-01-05 1991-07-10 Heraeus Electro-Nite International N.V. Method and apparatus for introducing uniform quantities of a material into a metallurgical sample
US5057149A (en) * 1990-01-05 1991-10-15 Electronite International, N.V. Method and apparatus for introducing uniform quantities of a material into a metallurgical sample
AU664534B2 (en) * 1990-05-16 1995-11-23 Metec Corporation Method of determining the carbon equivalent, carbon content and silicon content of molten cast iron
US5503475A (en) * 1992-10-23 1996-04-02 Metec Corporation Method for determining the carbon equivalent, carbon content and silicon content of molten cast iron
US5447080A (en) * 1993-05-26 1995-09-05 Midwest Instrument Co., Inc. Additive for molten metal sampler
US5524497A (en) * 1993-05-26 1996-06-11 Midwest Instrument Co., Inc. Additive for molten metal sampler
US5948350A (en) * 1998-02-11 1999-09-07 Midwest Instrument Co., Inc. Device for dispensing additive in molten metal sample mold
US6155122A (en) * 1998-04-07 2000-12-05 Midwest Instruments Co., Inc. Additive for molten metal sampler
FR2777995A1 (fr) * 1998-04-23 1999-10-29 Nippon Sublance Probe Engineer Procede d'analyse thermique de fonte a graphite spheroidal
BE1015189A3 (xx) * 1998-04-23 2004-11-09 Nippon Sublance Probe Engineer
US20100000303A1 (en) * 2006-09-29 2010-01-07 Anant Kashinath Kakatkar Apparatus and method for determining the percentage of carbon equivalent, carbon and silicon in liquid ferrous metal
EP2733488A1 (en) 2012-11-15 2014-05-21 Heraeus Electro-Nite International N.V. Detection device for molten metal
US9719976B2 (en) 2012-11-15 2017-08-01 Heraeus Electro-Nite International N.V. Method for detecting phase change temperatures of molten metal
US10371686B2 (en) 2012-11-15 2019-08-06 Heraeus EIectro-Nite International N.V. Detection device for molten metal
EP3339848A1 (en) * 2016-12-23 2018-06-27 Casa Maristas Azterlan Method to determine the carbon equivalent content of a cast iron alloy having a hypereutectic composition and equipment to carry it out

Also Published As

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ES356928A1 (es) 1970-02-16
NL6811188A (xx) 1969-02-11
BE719176A (xx) 1969-01-16
GB1221129A (en) 1971-02-03
JPS5036199B1 (xx) 1975-11-21
SE342508B (xx) 1972-02-07
DE1798004C3 (de) 1974-11-21
DE1798004B2 (de) 1974-04-18
FI49320B (xx) 1975-01-31
CH530002A (de) 1972-10-31
DE1798004A1 (de) 1972-03-02
DK143916B (da) 1981-10-26
NO123432B (xx) 1971-11-15
FI49320C (fi) 1975-05-12
DK143916C (da) 1982-04-13
NL145047B (nl) 1975-02-17
FR1579162A (xx) 1969-08-22

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