CN116867917A - Fe-Ni alloy with excellent surface properties, method for producing same, and die for CFRP - Google Patents

Fe-Ni alloy with excellent surface properties, method for producing same, and die for CFRP Download PDF

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CN116867917A
CN116867917A CN202280011344.5A CN202280011344A CN116867917A CN 116867917 A CN116867917 A CN 116867917A CN 202280011344 A CN202280011344 A CN 202280011344A CN 116867917 A CN116867917 A CN 116867917A
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mass
mgo
less
inclusions
cao
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桐原史明
水野建次
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Nippon Yakin Kogyo Co Ltd
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Nippon Yakin Kogyo Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/02—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling heavy work, e.g. ingots, slabs, blooms, or billets, in which the cross-sectional form is unimportant ; Rolling combined with forging or pressing
    • B21B1/024—Forging or pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B21B3/02—Rolling special iron alloys, e.g. stainless steel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • 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
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • 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
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04—Removing impurities by adding a treating agent
    • 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
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04—Removing impurities by adding a treating agent
    • C21C7/06—Deoxidising, e.g. killing
    • 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
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04—Removing impurities by adding a treating agent
    • C21C7/064—Dephosphorising; Desulfurising
    • 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
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04—Removing impurities by adding a treating agent
    • C21C7/068—Decarburising
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/02—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling heavy work, e.g. ingots, slabs, blooms, or billets, in which the cross-sectional form is unimportant ; Rolling combined with forging or pressing
    • B21B2001/028—Slabs

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  • Metallurgy (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Treatment Of Steel In Its Molten State (AREA)
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Abstract

The application relates to an Fe-Ni alloy consisting of C:0.001 to 0.2 mass% of Si:0.001 to 0.2 mass%, mn:0.005 to 0.7 mass% of Ni:30.0 to 45.0 mass percent of Cr:0.3 mass% or less, al:0.001 to 0.1 mass% of Ti:0.001 to 0.020 mass%, O:0.007 mass% or less, mg:0.0030 mass% or less, N:0.010 mass% or less, ca:0.0015 mass% or less, na:0.00005 to 0.001 mass% of Fe and unavoidable impurities, wherein CaO-SiO is contained 2 ‑Al 2 O 3 ‑MgO‑MnO‑Na 2 O-based composite oxideIs characterized by further comprising CaO, mgO, mgO.Al as an essential component 2 O 3 、MnO·SiO 2 、Na 2 More than 1 nonmetallic inclusion in O is taken as optional component, and CaO-SiO in all nonmetallic inclusions 2 ‑Al 2 O 3 ‑MgO‑MnO‑Na 2 The number ratio of O inclusions is 40% or more, thereby producing an Fe-Ni alloy excellent in surface properties.

Description

Fe-Ni alloy with excellent surface properties, method for producing same, and die for CFRP
Technical Field
The present application relates to an Fe-Ni alloy having excellent surface properties, and relates to a method for refining an Fe-Ni alloy, wherein the composition of slag and Mg, al, ca and Na in molten steel are controlled so as to be harmless to CaO-SiO in nonmetallic inclusions in molten steel 2 -Al 2 O 3 -MgO-MnO-Na 2 An Fe-Ni alloy excellent in surface properties, in which the number of inclusions on the surface is reduced, and a method for producing the same, and particularly relates to an Fe-Ni alloy suitable for a CFRP die.
Background
Carbon fiber reinforced composite materials (Carbon fiber reinforced plastic, CFRP) are materials having high strength and light weight, and are widely used in the fields ranging from the uses of golf clubs and the like to the automotive and aerospace industries. Particularly, in the case of being used in the aircraft industry or the automobile industry, invar alloy (Fe-36% ni) having a small thermal expansion coefficient is widely used as a mold because of the extremely high dimensional accuracy required (for example, refer to patent document 1).
Here, in the case of using invar as the mold for CFRP, since the mold surface is transferred to CFRP, the surface property of the mold itself is one of the very important factors, and it is necessary to have a surface as smooth as possible.
Patent document 2 proposes a method of performing plating treatment on the surface of a die with invar alloy to sufficiently smooth the die surface.
However, plating on the surface of the mold increases the cost, and it is difficult to plate a fine shape portion. In addition, although nonmetallic inclusions may affect the surface properties of the mold base material, no description is found about the amount of inclusions or the composition of inclusions.
Several techniques for making inclusions in invar harmless are disclosed.
In patent document 3, mgo—al as a non-stretching inclusion 2 O 3 Or MnO-MgO-SiO 2 The number of inclusions is controlled to 20% or less.
In addition, patent document 4 proposes controlling inclusions to be mno—sio 2 -Al 2 O 3 -CaO-MgO-Cr 2 O 3 -FeO-TiO 2 A method for producing an Fe-Ni alloy excellent in cleanliness.
However, patent documents 3 and 4 target shadow masks or lead frames, irrespective of the characteristics required for the CFRP mold.
Prior art literature
Patent literature
Patent document 1: japanese patent laid-open No. 8-269613,
patent document 2: japanese patent application laid-open No. 2014-205317,
patent document 3: JP-A2010-159737,
patent document 4: japanese patent laid-open No. 2003-073779.
Disclosure of Invention
Problems to be solved by the application
In view of the above problems, an object of the present application is to provide an fe—ni alloy excellent in surface properties, particularly an fe—ni alloy excellent in suitability for CFRP die use, by controlling the composition of nonmetallic inclusions or the number of surface inclusions. In addition, a manufacturing method for realizing the alloy is also provided.
Means for solving the problems
The inventors have intensively studied to solve the above problems. First, test pieces of 10 cm. Times.10 cm were collected from various Fe-Ni alloys of 30mm in plate thickness. The test piece surface was mirror polished, and an area of 10mm×20mm was measured at a magnification of 200 times with an optical microscope to 200mm 2 Is dispersed in parallel with the rolling direction and is continuously arranged with non-components of 40 μm or moreNumber of metallic inclusions. In addition, composition analysis was performed using SEM/EDS for nonmetallic inclusions on these surfaces. The test piece was kept in an atmosphere having a humidity of 60% and a temperature of 40℃for 24 hours, the number of nonmetallic inclusions arranged continuously at least 40 μm was measured again, the composition of nonmetallic inclusions was measured by SEM/EDS, the surface of the test piece was washed with water, polishing was further performed to a depth of about 1 μm, and the number of pits exceeding a depth of 10 μm and a diameter of 40 μm was measured on the surface of the test piece by a 3D laser microscope at a depth of 10cm×10 cm. These measurements were analyzed in depth. As a result, it was found that, in CaO and Na 2 If the number of O inclusions is large, the number of pits exceeding a depth of 10 μm and having a diameter of 40 μm increases. This was found to be due to CaO and Na being present on the surface 2 The O inclusions react with moisture in the atmosphere to form hydrates as in the reaction formulae (formula 1) and (formula 2), and come off from the surface.
CaO+H 2 O＝Ca(OH) 2 (formula 1)
Na 2 O+H 2 O=2 NaOH. Condition (formula 2)
As a result of further intensive analysis, it was found that when nonmetallic inclusions were controlled to be inclusion forms that do not react with moisture in the atmosphere, pits having a depth of 10 μm and a diameter of 40 μm were not produced. That is, it was found that if nonmetallic inclusion is controlled to CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The vitreous inclusion of O system does not generate pits exceeding 10 μm in depth and 40 μm in diameter. Further, regarding the Fe-Ni alloy having the surface properties as described above, the relationship with the operating conditions has been studied intensively. Based on the findings obtained by this analysis, the present application has been completed.
That is, the present application is an fe—ni alloy having excellent surface properties, characterized by comprising C:0.001 to 0.2 mass% of Si:0.001 to 0.2 mass%, mn:0.005 to 0.7 mass% of Ni:30.0 to 45.0 mass percent of Cr:0.3 mass% or less, al:0.001 to 0.1 mass% of Ti:0.001 to 0.020 mass%, O:0.007 mass% or less, mg:0.0030 mass% or less, N:0.010 mass% or less, ca:0.0015 mass% below, na:0.00005 to 0.001 mass% of Fe and unavoidable impurities, and CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The non-metallic inclusion of the O-based composite oxide further contains CaO, mgO, mgO.Al as an essential component 2 O 3 、MnO·SiO 2 、Na 2 More than 1 nonmetallic inclusion in O is taken as optional component, and CaO-SiO in all nonmetallic inclusions 2 -Al 2 O 3 -MgO-MnO-Na 2 The number ratio of O inclusions is 40% or more.
In the alloy of the present application, it is further preferable that Nb:0.01 to 1.00 mass%.
In addition, in the nonmetallic inclusion, caO and Na 2 The number ratio of O inclusions is preferably 20% or less, mgO.Al 2 O 3 The number ratio of inclusions is preferably 20% or less, and MnO.SiO 2 The number ratio of inclusions is preferably 20% or less.
In addition, caO-SiO among the nonmetallic inclusions 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-based oxide is composed of CaO:20 to 60 mass percent of SiO 2 :10 to 40 mass% of Al 2 O 3 : less than 30 mass percent of MgO:5 to 50 mass% of Na 2 O is 0.001 to 1 mass% and the balance is MnO, mgO.Al 2 O 3 The MgO is: 10 to 40 mass% of Al 2 O 3 :60 to 90 mass percent.
In addition, among these nonmetallic inclusions, 200mm was found on the alloy surface 2 In the area of (2), nonmetallic inclusions having a width of 5 μm or more and 40 μm or more are dispersed parallel to the rolling direction and are arranged continuously, preferably 10 or less.
In addition, the application also provides a method for manufacturing the Fe-Ni alloy. The method for producing an Fe-Ni alloy having excellent surface properties is characterized by melting a raw material in an electric furnace, decarburizing the raw material in AOD and/or VOD, and then charging lime, fluorite, ferrosilicon and/or Al, and using a method comprising the steps of: 50 to 70 mass percent of SiO 2 :3 to 30 mass percent of MgO:3 to 15 massAmount of Al 2 O 3 : less than 5 mass percent of Na 2 O:0.001 to 1 mass% of CaO-Al composed of the balance F 2 O 3 -MgO-SiO 2 -Na 2 The O-F slag is deoxidized and desulfurized while being stirred with a large amount of Ar, and is cast by a continuous casting machine or a common ingot casting method to produce an ingot after temperature and composition adjustment while promoting floating of inclusions due to Ar stirring with LF, and is hot-forged to produce a slab, followed by hot rolling and cold rolling.
Detailed Description
First, the reason why the chemical composition of the Fe-Ni alloy of the present application is limited will be described.
C:0.001 to 0.2 mass% or less
C is an element necessary to maintain the strength of the alloy. If the amount of C is less than 0.001 mass%, sufficient strength cannot be obtained, while if it exceeds 0.2 mass%, the thermal expansion coefficient increases, so the content of C is defined to be 0.001 to 0.2 mass%. Preferably 0.002 to 0.1 mass%. More preferably 0.003 to 0.05 mass%.
Si:0.001 to 0.2 mass%
Si is an element effective for deoxidization and has the function of controlling the composition of nonmetallic inclusion to CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The action of the O system. If the amount of Si is less than 0.001 mass%, the deoxidizing effect cannot be sufficiently obtained, and the nonmetallic inclusion composition cannot be controlled to CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 O is. On the other hand, if the Si content exceeds 0.2 mass%, the thermal expansion coefficient increases, the characteristics required for the fe—ni alloy sheet are not satisfied, mgO in the slag is reduced, and Mg is supplied to the molten steel. It reacts with Al to make nonmetallic inclusions become MgO-Al that are easily clustered 2 O 3 Spinel, causing surface defects. Accordingly, in the present application, the content of Si is defined to be 0.001 to 0.2 mass%. Within this range, it is preferably 0.002 to 0.19 mass%. More preferably 0.003 to 0.18 mass%.
Mn:0.005 to 0.7 mass%
Mn is an element effective for deoxidization, and has the function of controlling the composition of nonmetallic inclusion to CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The action of the O system. However, the element is also an element having an effect of increasing the thermal expansion coefficient of the fe—ni alloy, and from this viewpoint, it is desirable to have a concentration as low as possible. That is, if the Mn content is less than 0.005 mass%, the deoxidizing effect cannot be sufficiently obtained, and the composition of the nonmetallic inclusion cannot be controlled to CaO-SiO with a low melting point 2 -Al 2 O 3 -MgO-MnO-Na 2 O is. On the other hand, if the amount exceeds 0.7 mass%, the thermal expansion coefficient of the Fe-Ni alloy increases, and the quality required for the Fe-Ni alloy sheet cannot be satisfied. Therefore, in the present application, the content of Mn is defined to be 0.005 to 0.7 mass%. Preferably 0.01 to 0.65 mass%. More preferably 0.02 to 0.6 mass%.
Ni:30.0 to 45.0 mass percent
Ni is an element having a large influence on the thermal expansion coefficient, and it is known that the thermal expansion coefficient is minimized at about 36 mass% at 200 ℃ and about 42 mass% at 500 ℃. However, if the Ni content is less than 30 mass% or exceeds 45 mass%, the thermal expansion coefficient becomes large, and the required characteristics are not satisfied. Therefore, the Ni content is set to 30.0 to 45.0 mass%. Preferably 32.0 to 43.0 mass%. More preferably 35.0 to 42.0 mass%.
Cr:0.3 mass% or less
Cr is an element that increases the thermal expansion coefficient, and from this viewpoint, it is desirable to have a concentration as low as possible. Therefore, the content of Cr is set to 0.3 mass% or less. Preferably 0.25 mass% or less. More preferably 0.20 mass% or less.
Al:0.001 to 0.1 mass%
Al is a deoxidizing element, and plays a very important role in the present application. If the amount of Al is less than 0.001 mass%, deoxidization is insufficient, and thus the O concentration increases to more than 0.007 mass%, and the number of oxide inclusions increases, which causes surface defects. On the other hand, if the amount of Al exceeds 0.1 mass%, the ability to reduce MgO and CaO in the slag is too strong, and Mg and Ca in the steel exceeds 0.001 mass%. Because ofThe inclusion composition is CaO or MgO.Al 2 O 3 Is a main body. For this reason, al is defined to be 0.001 to 0.1 mass%. Preferably 0.0015 to 0.08 mass%, more preferably 0.002 to 0.07 mass%.
Ti:0.001 to 0.020% by mass
Ti is an element effective for deoxidization. If the amount is less than 0.001 mass%, the deoxidizing effect cannot be exhibited, and if it is not less than 0.020 mass%, tiN may be formed, causing surface defects. For this reason, ti is defined to be 0.001 to 0.020 mass%. Preferably 0.0012 to 0.015 mass%. More preferably 0.0015 to 0.010 mass%.
O: 0.007% by mass or less
O combines with the constituent components in the alloy to form inclusions. If these inclusions are coarse, they deteriorate the surface properties, and therefore, they need to be reduced as much as possible. If the content exceeds 0.007 mass%, coarse inclusions are generated, and therefore, ca is defined to be 0.007 mass% or less. Preferably 0.006 mass% or less, more preferably 0.005 mass% or less.
Mg:0.0030 mass% or less
If the Mg content exceeds 0.0030 mass%, the nonmetallic inclusion becomes MgO, mgo—al easily 2 O 3 . MgO is not clustered and is a fine nonmetallic inclusion, and does not affect the surface quality, but MgO.Al 2 O 3 In the refining process of Fe-Ni molten steel, aggregates are easily coagulated to form clustered large inclusions, which cause surface defects of products. Therefore, the content is set to 0.0030 mass% or less in the present application. Preferably 0.0020 mass% or less. More preferably 0.0010 mass% or less.
N:0.010 mass% or less
N is an element that needs to be reduced as much as possible because it forms nitrides with various elements. Therefore, the content is set to 0.010 mass% or less in the present application. Preferably 0.009 mass% or less, more preferably 0.008 mass% or less.
Ca: less than 0.0015 mass percent
Ca is used for controlling nonmetallic inclusion as CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-type nonmetallic inclusion is a useful element. However, if the Ca exceeds 0.0015 mass%, the CaO concentration in the inclusions increases to become a hydrate, and the surface properties may be deteriorated. From such a viewpoint, the content of Ca is set to 0.0015 mass% or less. Preferably 0.0007 mass% or less. More preferably 0.0005 mass% or less.
Na:0.00005 to 0.001 mass%
Na is used for controlling nonmetallic inclusion as CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The glass inclusion of the O system is a very important component. If the content is less than 0.00005 mass%, the effect cannot be exhibited, and if the content is 0.001 mass% or more, na is generated 2 The O inclusions may adversely affect the surface properties. For this reason, na is defined to be 0.00005 to 0.001 mass%. Preferably 0.00008 to 0.0005 mass%. More preferably 0.00010 to 0.0003% by mass. Na is obtained by reducing Na in slag 2 O is supplied to the molten steel.
Nb:0.01 to 1.00 mass percent
In the Fe-Ni alloy of the present application, nb is preferably added as required in addition to the above-mentioned components. Nb in a small amount has an effect of reducing the coefficient of thermal expansion, and if it is in the range of 0.01 to 1.00 mass%, it is an element effective for improving the strength of the fe—ni alloy sheet. If the strength of the Fe-Ni alloy sheet having low thermal expansion characteristics is required to be improved, the thickness of the Fe-Ni alloy sheet can be reduced, and the material can be reduced in weight, which is suitable for a mold for CFRP. However, if it exceeds 1.00 mass%, the coefficient of thermal expansion increases instead. For this reason, when Nb is added, it is defined to be 0.01 to 1.00 mass%. Preferably in the range of 0.02 to 0.50 mass%. More preferably 0.10 to 0.30 mass%.
Nonmetallic inclusion
In the present application, caO-SiO is contained 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-based composite oxide may further contain CaO, mgO, mgO.Al as an essential nonmetallic inclusion 2 O 3 、MnO·SiO 2 、Na 2 More than 1 of O is used as optional nonmetallic inclusion. In this case, it is preferable that CaO-SiO be contained in all nonmetallic inclusions obtained by combining the necessary nonmetallic inclusions and optional nonmetallic inclusions 2 -Al 2 O 3 -MgO-MnO-Na 2 The number ratio of O inclusions is 40% or more. The basis for defining the number ratio of nonmetallic inclusions is shown below.
Except CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-based composite oxide further contains CaO, mgO, mgO.Al 2 O 3 、MnO·SiO 2 、Na 2 1 or more than 2 inclusions in O, caO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The number ratio of O inclusion is 40% or more
The Fe-Ni alloy according to the application uses CaO-SiO according to the content of Si, al, mg, ca, na in the alloy 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-based oxide is an essential component, and CaO, mgO, mgO.Al 2 O 3 、MnO·SiO 2 、Na 2 More than 1 kind of O is optional component and contains nonmetallic inclusion. Wherein, caO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-oxide is a very stable oxide, and therefore does not react with moisture in the atmosphere to form a hydrate and cause pits on the surface. If CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The content of O oxide is 40% or more in terms of the number ratio, and the number of surface pits is small, so that the content is defined as 40% or more in terms of the number ratio. Preferably 45% or more, more preferably 50% or more.
CaO and Na 2 The number ratio of O inclusions is 20% or less
Due to CaO and Na 2 O reacts with moisture in the atmosphere to form a hydrate and is detached from the surface, so that inclusions causing pits are preferably as small as possible. Thus, caO and Na are combined 2 The number ratio of O inclusions is set to 20% or less. Preferably 15% or less. More preferably 10% or less. Although MgO also forms hydrate Mg (OH) in the atmospheric environment 2 But with CaO and Na 2 In the present application, O is not particularly limited because O requires a long time to change into a hydrate and has a very small influence.
MgO·Al 2 O 3 The number ratio of inclusions is 20% or less
MgO·Al 2 O 3 Since agglomeration and coarsening of inclusions are the main causes of deterioration of surface properties, it is preferable to minimize the amount of inclusions as much as possible. Thus, mgO and Al are used as 2 O 3 The number ratio of inclusions is defined to be 20% or less. Preferably 15% or less, more preferably 10% or less.
MnO·SiO 2 The number ratio of inclusions is 20% or less
MnO·SiO 2 The inclusions are coarse nonmetallic inclusions, causing surface defects, and are therefore preferably as small as possible. Thus, mnO.SiO 2 The number ratio of inclusions is defined to be 20% or less. Preferably 15% or less, more preferably 10% or less.
For specified CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The reason for each component contained in the O-based oxide will be described.
CaO:20 to 60 mass percent of SiO 2 :10 to 40 mass% of Al 2 O 3 : less than 30 mass percent of MgO:5 to 50 mass% of Na 2 O:0.001 to 1 mass% with the balance of MnO
Basically, the above range is set so that CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-oxide has a melting point of about 1300 ℃ or lower and becomes a vitreous oxide. If the CaO content is less than 20 mass%, the melting point is increased, and if the CaO content exceeds 60 mass%, caO inclusions coexist. If SiO is 2 Below 10 mass% and above 40 mass%, the melting point increases. If Al is 2 O 3 If the content exceeds 30 mass%, mgO-Al 2 O 3 Inclusions coexist. If MgO is less than 5 mass% and exceeds 50 mass%, the melting point is increased. In addition, if Na 2 O is 0.001 mass% or more, the catalyst is obtainedTo reduce the melting point of the inclusions and to control the effect of the vitreous inclusions, if the content exceeds 1 mass%, pure Na is used 2 And O inclusions coexist. For the above reasons, caO:20 to 60 mass percent of SiO 2 :10 to 40 mass% of Al 2 O 3 : less than 30 mass percent of MgO:5 to 50 mass% of Na 2 O:0.001 to 1 mass% and the balance of MnO.
For a prescribed MgO/Al 2 O 3 The reason for the composition of (a) will be described.
MgO·Al 2 O 3 The MgO is: 10 to 40 mass% of Al 2 O 3 :60 to 90 mass percent
MgO·Al 2 O 3 Is a compound having a broad solid solution. The above-mentioned range is defined as a solid solution.
The reason why the number and size of nonmetallic inclusions on the surface are specified will be described.
200mm on the alloy surface 2 The nonmetallic inclusion with the width of more than 5 mu m and more than 40 mu m arranged continuously in the area of more than 10 nonmetallic inclusions
Inclusions present on the surface of the alloy have a great influence on the surface properties. In particular, nonmetallic inclusions having a width of 5 μm or more and 40 μm or more arranged in succession become starting points of surface defects such as linear defects, and thus it is desirable to make them as small as possible. However, if 200mm is formed on the alloy surface 2 The surface defects are less likely to occur when 10 nonmetallic inclusions having a width of 5 μm or more and 40 μm or more are continuously arranged in the area of (a) or less, and thus the surface defects are defined as described above. Preferably 8 or less, more preferably 5 or less. The number of inclusions having an interval of 20 μm or less arranged was 1 in one block connected to each other, and the number of inclusions having an interval exceeding 20 μm was other blocks.
Fe-Ni alloy with excellent surface properties characterized by excellent suitability for CFRP mold applications
The present application provides an Fe-Ni alloy which does not cause pits and has excellent surface properties. Therefore, it has excellent adaptability to CFRP mold applications.
Method of manufacture
In the present application, a method for producing an Fe-Ni alloy is also provided. The method comprises the steps of melting a raw material, melting Fe-Ni having a predetermined composition, decarburizing in AOD and/or VOD, controlling the N concentration to 0.010 mass% or less, and then charging lime, fluorite, ferrosilicon and/or Al, wherein CaO:50 to 70 mass percent of SiO 2 :3 to 30 mass percent of MgO:3 to 15 mass% of Al 2 O 3 : less than 5 mass percent of Na 2 O:0.001 to 1 mass% of CaO-SiO with the balance being F 2 -MgO-Al 2 O 3 -Na 2 The O-F slag is deoxidized and desulphurized while stirring with a large amount of Ar, ti is further added, after the concentration of Ti is controlled to a predetermined value, the temperature and composition are adjusted while promoting the floating of inclusions caused by Ar stirring with LF, and then cast ingot is produced by a continuous casting machine or a common cast ingot; further performing hot forging from the ingot to produce a slab; the surface of the slab was ground, heated at 1200 ℃ and hot rolled to a predetermined thickness, annealed and pickled to remove the oxide scale on the surface, and finally a plate having a predetermined thickness was produced. Thus, nonmetallic inclusions except CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-based composite oxide can be controlled to CaO, mgO, mgO.Al 2 O 3 、MnO·SiO 2 、Na 2 1 or more than 2 kinds of O. As a result, caO-SiO was obtained 2 -Al 2 O 3 -MgO-MnO-Na 2 The content of O oxide is more than 40% of Fe-Ni alloy by number proportion.
In the method for producing an Fe-Ni alloy according to the present application, as described above, the composition of slag is characteristic. Hereinafter, the basis for defining the slag composition as described above in the present application will be described.
CaO:50 to 70 mass percent
The CaO concentration in the slag is an important element for efficient deoxidation and desulfurization and inclusion control. The concentration is adjusted by adding lime. If the CaO concentration exceeds 70 mass%, the activity of CaO in the slag increases, and the concentration of Ca reduced in the molten steel increases to more than 0.001 mass%, so that independent nonmetallic inclusions of CaO are generated, and pits are generated on the surface of the final product. Therefore, the upper limit is set to 70 mass%. On the other hand, if the CaO concentration is less than 50 mass%, deoxidation and desulfurization cannot be performed, and the ranges of the S concentration and the O concentration in the present application cannot be controlled. Therefore, the lower limit is set to 50 mass%. Thus, the CaO concentration is set to 50 to 70 mass%. Preferably 52 to 68 mass%. More preferably 55 to 65 mass%.
SiO 2 :3 to 30 mass percent
SiO in slag 2 It is an important element to ensure the optimal fluidity, and thus, it is required to be 3 mass%. However, if SiO 2 If the amount is too high to exceed 30 mass%, the oxygen concentration will also rise to exceed 0.007 mass%. SiO is used as a material 2 The concentration can be adjusted by the input amount of the ferrosilicon alloy. As described above, siO 2 The concentration is defined to be 3 to 30 mass%. Preferably 3 to 28 mass%. More preferably 3 to 25 mass%.
MgO:3 to 15 mass percent
MgO in the slag is an important element for controlling the concentration of Mg contained in the molten steel to the concentration range described in the claims, and is also an important element for controlling nonmetallic inclusion to the preferable composition of the present application. Therefore, the lower limit is set to 3 mass%. On the other hand, if the MgO concentration exceeds 15 mass%, the Mg concentration in the molten steel increases to produce MgO-Al 2 O 3 Becomes the starting point of surface defects such as linear defects. Therefore, the upper limit of the MgO concentration is set to 15 mass%. Preferably 4 to 14% by mass, more preferably 5 to 12% by mass. MgO in the slag is eluted into the slag by dolomite bricks or magnesia chrome bricks used in AOD refining or VOD refining to reach a predetermined range. Alternatively, waste bricks of dolomite bricks or magnesia chrome bricks may be added for control to a predetermined range.
Al 2 O 3 : less than 5 mass percent
If Al in slag 2 O 3 If the content is high, mgO/Al is formed 2 O 3 Inclusions of MgO-Al 2 O 3 Since the number ratio of inclusions exceeds 20%, it is necessary to reduce Al in slag as much as possible 2 O 3 Concentration. Therefore, the upper limit is set to 5 mass% or less. Preferably 4 mass% or less, more preferably 3 mass% or less.
Na 2 O:0.001 to 1 mass%
Na in slag 2 O has the function of controlling the inclusion composition to CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The effect of the O system is preferably 0.001 mass% or more. However, if the content exceeds 1 mass%, na is formed 2 O inclusion, thus Na 2 The O concentration is defined to be 0.001 to 1 mass%. Preferably 0.002 to 0.9 mass%. More preferably 0.003 to 0.5 mass%. Na is also described as 2 The O concentration can be controlled by adding sodium carbonate.
Examples
The following examples are given to further illustrate the constitution and operational effects of the present application, but the present application is not limited to the following examples. An electric furnace with a capacity of 60 tons is used for melting by taking ferronickel, pure nickel, scrap iron, fe-Ni alloy scraps and the like as raw materials. Then, decarburization is performed by oxygen blowing refining (oxidation refining) for removing C in AOD and/or VOD, and after the N concentration is controlled to 0.010 mass% or less, limestone, fluorite and sodium carbonate are charged to produce CaO-SiO 2 -Al 2 O 3 -MgO-Na 2 After the O-F slag is further charged with FeSi and/or Al to deoxidize, ar stirring is performed to desulfurize, and then Ti is added to control the Ti concentration. Then, the steel is tapped into a ladle, and temperature adjustment and composition adjustment are performed, whereby an ingot is produced by a continuous casting machine or a common ingot. Further, the ingot is hot forged to produce a slab.
The surface of the slab was ground, heated at 1200 ℃ and hot rolled from 200mm to 30mm, and subjected to an annealing and pickling step to produce a thick plate. Then, annealing and acid washing are performed to remove the oxide scale on the surface. The chemical composition of the Fe-Ni alloy obtained, the steel making process (EF: electric furnace, AOD: argon oxygen decarburization apparatus, VOD: vacuum oxygen decarburization apparatus, LF: ladle refining apparatus, CC: continuous casting machine, IC: ordinary ingot casting method), AOD or slag composition at the end of VOD refining are shown in Table 1. The nonmetallic inclusion composition, as well as morphology and quality evaluation of the inclusions, are shown in table 2.
(1) The chemical composition of the alloy and slag composition: quantitative analysis was performed using a fluorescent X-ray analyzer, and the oxygen concentration of the alloy was quantitatively analyzed by an inert gas pulse melting infrared absorption method.
(2) Nonmetallic inclusion composition: in the case of continuous casting, a sample of Fe-Ni alloy was collected by a tundish immediately after the start of casting, and in the case of ordinary ingot casting, a sample of Fe-Ni alloy was collected by a runner connected to a mold, and the solidified sample was mirror-polished, and nonmetallic inclusions having a size of 20 points of 5 μm or more were randomly measured by SEM-EDS.
(3) The number ratio of each nonmetallic inclusion: the number ratio was evaluated based on the measurement result of (2).
(4) Distribution of number of inclusions: the obtained slab was hot-rolled from a thickness of 200mm to a thickness of 30mm (reduction: 98.5%), a test piece of 10cm X10 cm was collected from a Fe-Ni alloy plate having a thickness of 30mm, and the surface of the test piece was polished and polished to finish the surface. The number of nonmetallic inclusions dispersed in parallel with the rolling direction and continuously arranged at 40 μm or more in an area of 10mm×20mm was measured using an optical microscope at a magnification of 200 times on the surface of the polished sample.
(5) Pit evaluation: the sample subjected to the mirror finish in (4) above was kept in an atmosphere having a humidity of 60% and a temperature of 40℃for 24 hours, and then the surface of the test piece was washed with water, polished and polished to a depth of about 1. Mu.m, and then the number of pits exceeding a depth of 10 μm and a diameter of 40 μm was measured on the surface of the test piece of 10cm X10 cm by a 3D laser microscope. Here, the number of pits is 0, a, B, C, and D, respectively, and 1 to 2, 3 to 5, and 6 or more.
(6) Surface defect evaluation: measurement of 10m 2 Surface in Fe-Ni alloy sheet subjected to pickling and annealing to remove scale on the surfaceNumber of defects. If at 10m 2 The number of surface defects was 0, and it was evaluated as a, 1, B, 2, C, and 3 or more.
(7) And (3) comprehensive evaluation: the pit evaluation and the surface defect evaluation were scored as follows, and if the total score of the pit evaluation and the surface defect was 6 points, the score was a, if the score was 4 to 5 points, the score was B, if the score was 3 points, the score was C, if the score was 2 points or less, or the pit evaluation or the surface defect evaluation was D, the score was D.
Pit evaluation: A3B 2C 1D 0
Surface defect evaluation: A3B 2C 1D 0
TABLE 1
TABLE 2
Since examples 1 to 17 satisfy the scope of the present application, the surface defects were small, and the number of coarse pits exceeding the depth of 10 μm and the diameter of 40 μm on the sample surface was almost zero, so that good quality was obtained.
On the other hand, the comparative example was out of the scope of the present application. Hereinafter, examples will be described.
The Si concentration in comparative example 18 was as low as 0.0004 mass%, the Al concentration was as low as 0.0003 mass%, the deoxidization was not performed, and the O concentration was as low as 0.0121 mass%. Na is not supplied from slag to molten steel, and Na concentration is as low as 0.00001 mass%. As a result, large-sized MnO.SiO inclusions are formed in large amounts 2 Inclusions of 10m 2 More than 10 surface defects caused by inclusions are generated.
In comparative example 19, si concentration was as high as 0.370 mass%, al concentration was as high as 0.210 mass%, and deoxidation reaction was excessively performed, resulting in excessive conversion from the slag layer to molten steelCa, mg and Na were supplied in such a manner that the Ca concentration was as high as 0.0022 mass%, the Mg concentration was as high as 0.0038 mass%, and the Na concentration was as high as 0.0017 mass%. As a result, caO-containing independent nonmetallic inclusions and Na are produced in large amounts 2 The independent nonmetallic inclusions of O were observed on the surface of the sample after the adjustment to a large number of pits exceeding a depth of 10 μm and a diameter of 40. Mu.m. In addition, it was also observed that MgO.Al 2 O 3 Surface defects caused by inclusions.
Comparative example 20 excessive Na was supplied to slag 2 As a result, the Na concentration in the molten steel was as high as 0.002 mass%. As a result, the inclusions are expressed as Na 2 O was used as a main component, and a large number of pits exceeding a depth of 10 μm and a diameter of 40 μm were observed on the surface of the sample after adjustment.
Comparative example 21 where Na was not supplied to slag 2 The Na concentration in O and molten steel is as low as 0.00002 mass%, and the inclusions are made to contain no Na 2 CaO-SiO of O 2 -Al 2 O 3 MgO-MnO system. As a result, the melting point of the inclusions increases, and the inclusions cannot be finely dispersed during hot rolling, resulting in surface defects. In addition, since some of the inclusions were not glassy, pits exceeding a depth of 10 μm and a diameter of 40 μm were also observed on the surface of the sample after adjustment. Although the items of "inclusion number ratio" in comparative example 21 were all 0, inclusions were present in the items of "inclusion composition (mass%) 20 points" and "inclusion number distribution" by EDS analysis. This is because the inclusion of comparative example 21 does not contain Na 2 CaO-SiO of O5 component system 2 -Al 2 O 3 MgO-MnO system is present, and CaO-SiO which is not the 6-component system of the present application as the object of counting in the item of "inclusion count ratio 2 -Al 2 O 3 -MgO-Na 2 O-MnO system, and thus, no counting was performed.
The concentrations of Ti and N in comparative example 22 were as high as 0.036 mass% and 0.012 mass%, and a large number of surface defects due to TiN were observed on the surface of the Fe-Ni alloy sheet.
Comparative example 23 was conducted by directly supplying Mg to molten steel, and Mg was as high as 0.0033 mass%. As a result, it is matched with Al in slag 2 O 3 Reaction to produceA large amount of MgO/Al 2 O 3 Inclusions. As a result, mgO.Al 2 O 3 The ratio increases and a large number of surface defects are detected.
The Mn charged in comparative example 24 was not retained, and the Mn concentration was as low as 0.003%. As a result, the deoxidation was not sufficiently performed, and the oxygen concentration was as high as 0.008%. In addition, the inclusion composition also becomes CaO-SiO containing no MnO 2 -MgO-Al 2 O 3 -Na 2 O is. As a result, the melting point of the inclusions increases, the number of inclusions increases, and a large number of surface defects caused by the inclusions are detected.
Industrial applicability
The technique of the present application can obtain an Fe-Ni alloy excellent in surface properties, particularly an Fe-Ni alloy excellent in adaptability to CFRP mold applications, by controlling the composition of nonmetallic inclusions or the number of inclusions on the surface.

Claims (9)

  1. An fe-Ni alloy characterized by the composition of C:0.001 to 0.2 mass% of Si:0.001 to 0.2 mass%, mn:0.005 to 0.7 mass% of Ni:30.0 to 45.0 mass percent of Cr:0.3 mass% or less, al:0.001 to 0.1 mass% of Ti:0.001 to 0.020 mass%, O:0.007 mass% or less, mg:0.0030 mass% or less, N:0.010 mass% or less, ca:0.0015 mass% or less, na:0.00005 to 0.001 mass% of Fe and unavoidable impurities, and CaO-SiO 2 -Al 2 O 3 -MgO-MnO-Na 2 The non-metallic inclusion of the O-based composite oxide further contains CaO, mgO, mgO.Al as an essential component 2 O 3 、MnO·SiO 2 、Na 2 More than 1 nonmetallic inclusion in O is taken as optional component, and CaO-SiO in all nonmetallic inclusions 2 -Al 2 O 3 -MgO-MnO-Na 2 The number ratio of O inclusions is 40% or more.
  2. 2. The Fe-Ni alloy according to claim 1, comprising Nb:0.01 to 1.00 mass%.
  3. 3. The Fe-Ni alloy according to claim 1 or 2, wherein CaO and Na are contained in the total nonmetallic inclusions 2 The number ratio of O inclusions is 20% or less.
  4. 4. The Fe-Ni alloy according to any one of claims 1 to 3, wherein MgO-Al is among all nonmetallic inclusions 2 O 3 The number ratio of inclusions is 20% or less.
  5. 5. The Fe-Ni alloy according to any one of claims 1 to 4, wherein MnO.SiO among the nonmetallic inclusions 2 The number ratio of inclusions is 20% or less.
  6. 6. The Fe-Ni alloy according to any one of claims 1 to 5, wherein the CaO-SiO is 2 -Al 2 O 3 -MgO-MnO-Na 2 The O-based oxide is composed of CaO:20 to 60 mass percent of SiO 2 :10 to 40 mass% of Al 2 O 3 : less than 30 mass percent of MgO:5 to 50 mass% of Na 2 O is 0.001 to 1 mass% and the balance is MnO, wherein the MgO.Al 2 O 3 The MgO is: 10 to 40 percent of Al 2 O 3 ：60～90％。
  7. 7. The Fe-Ni alloy according to any one of claims 1 to 6, wherein when a slab having a thickness of 200mm is hot-rolled to a thickness of 30mm, the thickness of the slab is 200mm on the surface of the alloy 2 In the area of (2), nonmetallic inclusions having a width of 5 μm or more and 40 μm or more are dispersed parallel to the rolling direction and are continuously arranged, and the number of nonmetallic inclusions is 10 or less.
  8. A mold for CFRP comprising the Fe-Ni alloy according to any one of claims 1 to 7.
  9. 9. A process for producing an Fe-Ni alloy having excellent surface properties, which comprises the process for producing an Fe-Ni alloy according to any one of claims 1 to 7, characterized by usingThe raw materials were melted in an electric furnace, and then, after decarburization in AOD and/or VOD, lime, fluorite, ferrosilicon and/or Al were charged, and CaO:50 to 70 percent of SiO 2 ：3～30％、MgO：3～15％、Al 2 O 3 : less than 5% of Na 2 O:0.001 to 1 percent of CaO-Al composed of the balance of F 2 O 3 -MgO-SiO 2 -Na 2 The O-F slag is deoxidized and desulfurized while stirring with Ar, and is cast by a continuous casting machine or a common ingot casting method to produce an ingot after temperature and composition adjustment while promoting the floating of inclusions caused by Ar stirring with LF, and hot-forged to produce a slab, followed by hot-rolling and cold-rolling.
CN202280011344.5A 2021-03-12 2022-02-18 Fe-Ni alloy with excellent surface properties, method for producing same, and die for CFRP Pending CN116867917A (en)

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