US3726670A - Nodular graphite cast iron containing calcium,rare earth metals and magnesium and a method for its production - Google Patents

Nodular graphite cast iron containing calcium,rare earth metals and magnesium and a method for its production Download PDF

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US3726670A
US3726670A US00092805A US3726670DA US3726670A US 3726670 A US3726670 A US 3726670A US 00092805 A US00092805 A US 00092805A US 3726670D A US3726670D A US 3726670DA US 3726670 A US3726670 A US 3726670A
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cast iron
nodular graphite
casting
rare earth
weight
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K Kusaka
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C35/00—Master alloys for iron or steel
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C37/00—Cast-iron alloys
    • C22C37/04—Cast-iron alloys containing spheroidal graphite

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  • Nodular graphite cast iron containing carbon in the range of from 3.2 to 4.2% by weight, silicon in the amount of from 1 to 4.5% by weight and in which the percent carbon plus one-third the percent silicon is equal to or greater than 4.0% is provided.
  • the nodular graphite cast iron is produced by adding to a molten iron having a sulphur content of less than 0.03% by weight, a nodular graphite cast iron additive consisting essentially of to 30% by weight of magnesium fluoride, from 10 to 30% by weight rare earth metal fluoride, and from 40 to 80% by weight calcium-silicon.
  • the present invention relates to nodular graphite cast iron containing calcium, rare earth metals, and magnesium as well as to the method for producing the nodular graphite cast iron.
  • the invention further relates to an additive composition useful in the production of such nodular graphite cast iron.
  • R represents rare earth metals.
  • Another object of this aspect of the invention is to provide a method of producing nodular graphite cast iron involving the minimum risk during the operation and 3,726,670 Patented Apr. 10, 1973 to obtain an inexpensive nodular graphite cast iron of excellent quality containing rare eartth metal magnesium and calcium, by dispensing with the use as additives of the expensive mischmetall of rare earth metals, magnesium alloys, etc., and using as additives the mixture of their respective fluorides (which are less expensive and easier to use), and calcium silicon powder instead.
  • Still another object of this aspect of the invention is to obtain a nodular graphite cast iron which is excellent in various respects (minimum drossy scum, etc.) to be stated hereinafter, by virtue of the characteristics of the nodular graphite cast iron of the invention which always contains calcium in a slight quantity, rare earth metal elements in an appreciably higher quantity, and magnesium on the contrary in a small quantity.
  • the pig iron contains elements detrimental to spheroidization of graphite such as titanium (Ti), bismuth (Bi), antimony (Sb), or lead (Pb), it has been well known that to control the harmful effect of these elements a small quantity of cerium (Ce) may be added in addition to making nodular graphite castings and that in such case the residual contents of the casting is 0.04% Mg, or above.
  • elements detrimental to spheroidization of graphite such as titanium (Ti), bismuth (Bi), antimony (Sb), or lead (Pb)
  • Ce cerium
  • nodular graphite castt iron in which the residual content of Mg is 0.040% and above, and to yet another proposal which defines the main contents of nodular graphite cast iron in the ranges of 0040- 0.50% Mg and 0.004-0.020% La.
  • the residual Mg content is more than 0.040%.
  • a nodular graphite casting having a residual Mg content ranging from 0.04% to 0.09% is subject to a greater change in the structure and hardness depending upon the difference in mass elfect.
  • Ce metal instead of Mg has been known in making nodular graphite castings, but Ce is more expensive and moreover the nodular graphite cast iron obtained by using Ce shows a far greater mass eifect than that of the Mg nodular graphite cast iron and such casting tend to give various difiiculties in service. This is well known in the art.
  • FIG. 1 is a diagram showing the comparative features of the casting made according to the first aspect of this invention and those made in the conventional method.
  • Curve I plots the relative change of the mass and Brinell hardness of a conventional nodular graphite cast iron containing Mg
  • curve II shows the relative change in the nodular graphite cast iron according to this first aspect of the invention containing calcium, rare earth metals and Mg, with the diameter (mm.) of the casting shown in the abscissa and Brinell hardness in the ordinate.
  • FIG. 2(a) shows the microstructure X200 of an etching of an example of a conventional Mg-nodular graphite cast iron
  • FIG. 2(b) shows the microstructure X200 of an etching of a typical example of a nodular graphite cast iron according to this first aspect of the invention.
  • FIG. 3 is a photo-micrograph comparing the mass effect of a conventional Mg-nodular graphite cast iron and that of the similar cast iron made by this invention, with A A; and A showing the conventional products and B B and B the ones made by the first aspect of this invention.
  • the process according to the first aspect of the invention comprises adding to molten iron in a ladle an addition agent made of a certain mixture in which there are mixed in various proportions the powder of magnesium fluoride (hereinafter expressed MgF rare earth metal fluoride (hereinafter expressed RE) and calcium-silicon alloy.
  • MgF rare earth metal fluoride hereinafter expressed RE
  • the chemical reaction can proceed even in the molten iron at a temperature from 1,400 C. to 1,500 C. Without any explosive hazard but generating only slight smoke and light and the castings thereby obtained are found to contain certain residual contents of Ca, R and Mg.
  • magnesium, calcium and rare earth metal are added directly to the molten iron, these metals will burn immediately and in case of magnesium, although it is an easy metal to add, will emit a blue-white blaze during burning which is liable to do harm to the eyes of the operator.
  • the addition agent is made from a mixture of fluorides of the metals and calcium-silicon powder instead of magnesium and rare earth metal and said addition agent is added to the molten iron before this is charged into the ladle, thus making operation more simple.
  • Adding to this addition agent can be made by any process, such as injection, dumping or pouring and this process needs no extra care as in the case of the conventional method of making nodular graphite cast iron using an Mg alloy.
  • R and Mg being in very fine particulate form, will disperse extensively in the molten iron and combine with S and O in the molten iron and seem to promote spheroidization of graphite.
  • the excellent quality nodular graphite casting made by this aspect of the invention which gives the minimum shrinkage cavity, drossy scum, mass effect and good castability, has residual contents of three elements of the casting as follows:
  • weight ratio between Mg and R is maintained by controlled addition of additive as under:
  • the casting obtained will show very little mass effect and it will make an excellent quality nodular graphite casting which is also excellent in other properties as explained later on.
  • the number of elements of the nodular graphite cast iron according to the present invention is limited to three, that is, Ca, Mg and R; so are their content ranges and also the content ratio of R/ Mg to a range between 1.0 and 0.4.
  • a great quantity of Ca-Si is mixed with the nodulizing agent according to the present invention, which is for the reduction of MgF and R1 in the agent, and which is also to have its element Ca remain in the cast iron as much as possible in a range between 0.002 and 0.025%, thus improving the low fluidity of the nodular graphite cast iron as the abovementioned effect of Ca addition.
  • the reason for prescribing said residual range is that whatever greater addition of Ca would increase with diificulty the residual content beyond the upper limit of 0.025%, and the residual content below the lower limit of 0.002% would hardly facilitate fluidity and nodulization.
  • the residual content of Ca in the cast iron in a residual range between 0.002 and 0.025% according to the present invention improves the low fluidity of nodular graphite cast iron, from the level of cast steel to that of ordinary cast iron or better.
  • the reason for prescribing the residual content of Mg in a range between 0.006 and 0.040% is to reduce the drossy scum in the cast iron and the shrinkage cavity to a minimum; and to attain nodulization of cast iron in cooperation with the co-additives of R and Ca, while it is not attainable with the exclusive use of Mg.
  • This range is justified, because a residual content beyond the upper limit of 0.04% would produce drossy scum and a shrinkage cavity on a greater scale in the cast iron, and cause chilling of the cast iron; and because a residual content below the lower limit of 0.006% would hardly facilitate nodulization even with the co-existence of R and Ca.
  • the reason for the residual range of R is prescribed as above is because a residual content beyond the upper limit of 0.120% would cause chilling of the cast iron at great occurance rate irrespectively of the any content ratio of R/Mg; and because a residual content below the lower limit of 0.010% would not facilitate nodulization of cast iron even at the co-existence of Mg and Ca.
  • the reason for prescribing the content ratio of R/Mg between 1.0 and 4.0 is to make the residual content of R equal to or much greater than that of Mg, thereby facilitating nodulization, reducing drossy scum and shrinkage cavity, and also preventing chilling of the cast iron.
  • the effect obtainable from the content ratio of R/Mg being set between 1.0 and 4.0 is to prevent the chilling of the cast iron when being cast into products of, say, 3 mm., mm. and 20 mm. in thickness by making the ratio of R/Mg respectively about 1.0, to 1.20 and 3.0.
  • the three elements of Mg, R and Ca are added with the residual content of R/ Mg being set as mentioned above.
  • This is to obtain nodular graphite cast iron with its graphite fully nodulized, of low tendency to chill, of good fluidity, and with a presence of little drossy scum and shrinkage cavity, thus solving the problems occuring in conventional nodular graphite cast iron containing more thtan 0.04% Mg, as such the presence of large quantity of dead head metal due to a large amount of drossy scum and shrinkage cavity and the resulting low yields and high production costs of castings.
  • the use of the nodulizing agent of the present invention consisting of fluorides of Mg and R and great quantities of such Cafi i alloys are as formularized as MgF +RF +CaSi, makes it possible to easily retain the above mentioned three elements of Mg, R and Ca in the prescribed content ranges in cast iron by chemical raction, whereas the conventional additives produce causing strong flash light or big bounces of molten iron, making the method of the present invention easier.
  • the flux method using the additive of the present invention is to obtain nodular graphite castings with a minimum amount of drossy scum present and shrinkage cavity.
  • the addition of Mg, R and Ca, the three elements of the additive according to the present invention is made by means of the addition of such alloys as MgSi, Mg-R-Si, RCaSi, and misch metal, the following difficulties and disadvantages will occur: Because strong flash light and bounces of molten iron are produced when such alloy additives are injected, a special adding method for the prevention of them is needed; as R is greater than Mg in aflinity with oxygen, sulphur, etc., R in the alloy additive is lost through such reactions as deoxidization and desulphurization, prior to the effect of Mg, making it sometimes difficult to attain the prescribed residual content of R, therefore, a stage-by-stage-adding means or apparatus, that is, for adding R alloys into cast iron after the addition of Mg alloys is needed.
  • the addition according to the present invention is carried out by using the additive containing such flux as MgF, and RF that is prepared specially for this purpose, and also CaSi alloy for the reduction of the flux.
  • This method is very effective in solving problems to occur with the use of the abovementioned alloy additives.
  • the gist of the present invention lies in that the three elements of Mg, R and Ca are retained easily and efficiently respectively in the above prescribed residual contents in cast iron, which is shown by the effect obtained in actual operations conducted as preferred embodiments, as follows:
  • Additive (b) was added in a range between 0.5 and 2.5% according to the sulphur content of the molten iron (a), as follows:
  • the residual contents of Mg, R and Ga were respectively about 0.024%, 0.035% and 0.01%.
  • the nodulization rate of cast iron was Drossy scum and shrinkage cavity were present very little.
  • the R/Mg ratio of the molten iron obtained by means of the above treated was about 1.15, a casting having as this as about 3 mm. of thickness of its thinnest part, could be produced without chilling, Also, because of a Ca content of 0.010% of said molten iron, such thinnest part of as thin as about 3 mm. of said casting was produced very precisely as prescribed.
  • the constituents of the cast iron to which the present invention is is applicable are carbon in the range of from 3.2% to 4.2% by weight, silicon in the amount of from 1.0% to 4.5% by weight, and in which the percent carbon plus one-third the percent silicon is equal to or greater than 4.0% (C% /3 Si %;4.0%). This means that the thus-produced nodular graphite cast iron is an eutectic or hypereutectic cast iron.
  • the pig iron to which graphite spherodizing treatment was applied in this comparative test was made by melting 70% ductile pig iron, 30% steel scraps with fine quality coke and limestone.
  • the two types of the molten iron which had undergone the spheroidizing treatment by the conventional method and the method of this aspect of the invention were moulded, using CO process sand moulds, into five different sized column typed castings, of diameters, 30 mm., 50' mm., 70 mm., 100 mm., and 150 mm., and later analytical tests were made on each of them.
  • nodular graphite casting made by the conventional Mg alloy addition of diameter ranging from mm. to mm. will contain free ccrnentite and be much higher in Brinell hardness while more massive casting of diameter ranging from mm. to mm. will have a soft structure with ferrite deposited instead of free cementite.
  • nodular graphite castings produced by the convention Mg alloy addition method vary greatly in hardness and structure depending upon the difference in the mass efiect as is well known by the foundry engineers; (see C. K. Dono, p. 97, Iron Age, Feb. 24, 1949).
  • nodular graphite castings of this first aspect of the present invention though low in residual Mg contents, will make castings of softer structure rich in well spheroidized graphite and ferrite areas, and will be subject to considerably less change by the mass effect, as seen in Table II.
  • curve I shows the conventional nodular graphite casting and its hardness-diameter relation
  • curve II shows the new nodular graphite casting made by this invention and said relation.
  • FIG. 2 The structure of the two types of castings, each 50 mm. in diameter, as given in Table II are illustrated in FIG. 2 in which the photograph a shows the microstructure of the conventional casting and the photograph b shows that made as cast and after annealing, show that the casting made by this invention is much lower in hardness and higher in elongation.
  • the nodular graphite cast iron according to the present invention has excellent strength, hardness and elongation and low mass effect. This is considered to be due to the presence of Ca, Mg and R in the proper percentage as seen in the residual contents of the cast iron made by the method of this invention.
  • Tables IV and V show the results of tests made on the seoond groups of examples of this invention.
  • compositions of addition agents as well as the relation between shrinkage cavity of the castings and their residual contents of Ca, Mg and R.
  • the addition agent used in making nodular graphite casting of this invention is the mixture, in certain proportion, of the three ingredients, RF MgF, and Ca-Si powder
  • this example also discloses some subsidiary agents which may be used in addition to the main components, RF MgF and Ca--Si within the scope of the first aspect of this invention.
  • Fe balance Fe-Si: (S
  • the addition agent No. I is a control specimen of a composition in range other than that of this invention
  • the pig iron used in the second example was melted in an acid lined cupola combining ductile pig iron 80% and steel scraps 20% and adding for fuel coke 16% and CaC, lump 2%, and the molten iron was poured into a ladle 100 kg. in capacity.
  • the tapping temperature was between 1,500 C. and 1,530 C. and the percentage of S in the molten iron ranged from 0.045% to 0.058%.
  • each of the addition agents as enumerated in Table IV was added to the molten iron contained in the ladle by injection using N gas and the quantity of the agent added was 2% for the molten iron. After the temperature of the molten iron went down to about 1,400" C., the molten metal was cast in a sand mould and thus a column-shaped specimen casting was made. In this way, all specimen castings, in column shape, 50 mm. in diameter and 250 mm. in height, were prepared by casting with addition of each of the addition agents as given in Table IV.
  • the castings lower in R/Mg TABLE V.GHEMICAL COMPOSITION AND DEPTH OF GRAPHITE CASIIN S those containing, in addition to the above three, small quantities of one or more than two of supplementary components such as CaF Mg-Qi, FeSi and CaC are used.
  • small amounts of CaF NaF and KP may be used as partial substitutes for RF and MgF the main components of the addition agents of this invention; an alloy similar to Ca-Si alloy (such as MgSi, Fe-Si, R--MgSi [rare-earth bearing MgSi alloy]) may partially replace Ca-Si.
  • a small amount of CaC may also be used as partial substitute for Ca-Si.
  • the rare earth metal oxides separated from monazite sand, etc. consist of about Ce O 25% n.0,, and 25% other rare earth expressed by Dy O
  • RG1 made of these rare earth metal oxides, and the mischmetal made of RF; or their salts are of composition generally in the proportions 50% Ce, 25 La, and 25 Dy.
  • Control specimen casting I 3.4 2. 6 0. 006 0.011 0. 052 0. 21 112 II 3. 5 2. 6 0. 013 0. 041 0. 02B 1. 46 6g Castings according to this lnveution..-.:-.
  • the casting in which addition agent No. I was used is excluded from this invention because the residual contents are not as specified, even the residual Mg being slightly in excess of the residual Mg content of the castings of this invention.
  • the castings in which addition agents, Nos. II-V, are used are included within the range of the nodular graphite casting according to this aspect of the invention because they contain a small quantity of Ca, their Mg/R ratios are within the range of l.0/l.0-4.0, and moreover the Mg contents are below 0.04%.
  • RF composed of 50% Ce, 25 La and 25 Dy
  • the fluorides obtained by treating rare earth metal oxides is used.
  • a precipitate may be made by carefully controlling the pH value of the solution in which two groups of fluorides can be separated with relative ease as follows:
  • these two groups of RE are prepared and MgF and CaSi are both mixed with each of them so that two types of addition agent are prepared.
  • addition agents By adding these addition agents to the molten iron, excellent quality nodular graphite castings are obtained, all of them showing alike good results in shrinkage cavity and mass effect.
  • the casting in which the Ce-enriched addition agent was used has less ferrite area and the casting in which La-enriched RF;
  • a third group of examples is as follows.
  • Casting Type (1) is excluded from the casting according to this aspect of the invention because this type of casting is high in Mg residual content and low in R content and R/Mg ratio is 0.27 while casting type (2) is included in the scope of the invention.
  • the castings of this aspect of the invention can make excellent castings having good nodular graphite not only with grey cast iron but also with chilled castings.
  • Ductile pig iron of this grade as well as those containing components other than those stated above can be proceed with the same good effect by the method of this invention.
  • this method will appear more uneconomic because the castings according to this invention contain a higher percentage of the more expensive R and a lower percentage of Mg compared with conventional nodular graphite castings in which Mg alloy is used and their Mg residual contents range from 0.04 to 0.09%.
  • the castings of this invention Compared with the conventional nodular graphite castings in which more Mg alloy is used, the castings of this invention give much improved yield as shown in Table IX and consequently the production cost of nodular graphite casting is reduced because they give no deep shrinkage cavity and thereby minimize the wastage in dead head metal and the like.
  • All of the castings obtained according to this aspect whether they are grey cast iron, alloy cast iron, white pig iron or cast iron of common composition, have a good nodular graphite and they are excellent quality castings with minimized shrinkage cavity, drossy scum, mass efl'ect and good castability.
  • a method for producing nodular graphite cast iron consisting essentially of carbon in the range of 3.2 to 4.3% by weight, silicon in the range of 1.0 to 4.5% by weight, calcium, a rare earth metal, magnesium, and the balance being iron, wherein the percentage of carbon plus one-third the percentage of silicon is equal to or greater than 4.0% by weight of the cast iron, comprising using an additive in powdered form consisting essentially of a mixture of -30% by weight of the fluorides of a rare earth metal, 10-30% by weight of magnesium fluoride, and 40-80% by weight of calcium-silicon by adding said mixture together in a single stage to the cast iron in the molten state, in such amounts that the finished nodular graphite cast iron has a residual content of the calcium, rare earth metal, and magnesium in the ranges of:
  • rare earth metal 0.010 to 0.12%, and magnesium0.006 to 0.04%
  • a nodular graphite cast iron consisting essentially of carbon in the range of from 3.2 to 4.3% by weight, silicon in the range of from 1.0 to 4.5% by weight, wherein silicon is equal to or greater than 4.0% by weight of the cast iron, calcium in the range of 0.002 to 0.025%, magnesium in the range of 0.006 to 0.040%, and a rare earth metal in the range of 0.010 to 0.12%, and the weight ratio of Mg:R being within the range of 1.0: 1.0 to 4.0, whereby the ratio of the Mg:R within the aforesaid range increases in proportion to the thickness of the castings produced from said cast iron, said nodular graphite cast iron possessing a soft structure, high elongation characteristics, low mass etfect and high tensile strength as a result of the magnesium, rare earth metal and calcium being present in the proportions claimed.

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  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3997338A (en) * 1974-03-22 1976-12-14 Centre De Recherches Scientifiques Et Techniques De L'industrie Des Fabrications Metalliques, En Abrege C.R.I.F. Gray cast iron
US4033766A (en) * 1975-04-17 1977-07-05 Ford Motor Company Continuous stream treatment of ductile iron
US4057098A (en) * 1975-07-07 1977-11-08 Boris Pavlovich Platonov Method of producing thin-walled castings
JPS5365215A (en) * 1976-11-25 1978-06-10 Kubota Ltd Cast iron with high damping capacity
US4236944A (en) * 1977-10-24 1980-12-02 Sandvik Aktiebolag Cast iron especially suited for ingot molds
RU2156809C1 (ru) * 2000-01-21 2000-09-27 Общество с ограниченной ответственностью "Экономист" Способ получения высокопрочного чугуна
RU2156810C1 (ru) * 2000-01-21 2000-09-27 Общество с ограниченной ответственностью "Экономист" Способ получения высокопрочного чугуна с шаровидным и вермикулярным графитом
RU2267542C1 (ru) * 2004-07-19 2006-01-10 Брянская государственная инженерно-технологическая академия (БГИТА) Чугун, способ его получения и способ термической обработки отливок из него
RU2415949C2 (ru) * 2009-05-13 2011-04-10 ГОСУДАРСТВЕННОЕ ОБРАЗОВАТЕЛЬНОЕ УЧРЕЖДЕНИЕ ВЫСШЕГО ПРОФЕССИОНАЛЬНОГО ОБРАЗОВАНИЯ "Брянский государственный технический университет" Способ получения чугуна с шаровидным графитом и аустенитно-ферритной металлической матрицей

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3997338A (en) * 1974-03-22 1976-12-14 Centre De Recherches Scientifiques Et Techniques De L'industrie Des Fabrications Metalliques, En Abrege C.R.I.F. Gray cast iron
US4033766A (en) * 1975-04-17 1977-07-05 Ford Motor Company Continuous stream treatment of ductile iron
US4057098A (en) * 1975-07-07 1977-11-08 Boris Pavlovich Platonov Method of producing thin-walled castings
JPS5365215A (en) * 1976-11-25 1978-06-10 Kubota Ltd Cast iron with high damping capacity
US4236944A (en) * 1977-10-24 1980-12-02 Sandvik Aktiebolag Cast iron especially suited for ingot molds
RU2156809C1 (ru) * 2000-01-21 2000-09-27 Общество с ограниченной ответственностью "Экономист" Способ получения высокопрочного чугуна
RU2156810C1 (ru) * 2000-01-21 2000-09-27 Общество с ограниченной ответственностью "Экономист" Способ получения высокопрочного чугуна с шаровидным и вермикулярным графитом
RU2267542C1 (ru) * 2004-07-19 2006-01-10 Брянская государственная инженерно-технологическая академия (БГИТА) Чугун, способ его получения и способ термической обработки отливок из него
RU2415949C2 (ru) * 2009-05-13 2011-04-10 ГОСУДАРСТВЕННОЕ ОБРАЗОВАТЕЛЬНОЕ УЧРЕЖДЕНИЕ ВЫСШЕГО ПРОФЕССИОНАЛЬНОГО ОБРАЗОВАНИЯ "Брянский государственный технический университет" Способ получения чугуна с шаровидным графитом и аустенитно-ферритной металлической матрицей

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DE1458423A1 (de) 1968-12-19
BE618166A (fr) 1962-09-17

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