WO2022102805A1 - Matériau composite à base de fe renforcé par des particules de tic et procédé pour la préparation de celui-ci - Google Patents

Matériau composite à base de fe renforcé par des particules de tic et procédé pour la préparation de celui-ci Download PDF

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Publication number
WO2022102805A1
WO2022102805A1 PCT/KR2020/015813 KR2020015813W WO2022102805A1 WO 2022102805 A1 WO2022102805 A1 WO 2022102805A1 KR 2020015813 W KR2020015813 W KR 2020015813W WO 2022102805 A1 WO2022102805 A1 WO 2022102805A1
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Prior art keywords
tic
composite material
reinforced
based composite
preform
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PCT/KR2020/015813
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English (en)
Korean (ko)
Inventor
조승찬
김정환
이상관
이상복
이영환
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한국재료연구원
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Publication of WO2022102805A1 publication Critical patent/WO2022102805A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/88—Metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D19/00—Casting in, on, or around objects which form part of the product
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
    • C04B41/4535—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied as a solution, emulsion, dispersion or suspension
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5144—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the metals of the iron group
    • 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

Definitions

  • the present invention relates to a TiC particle-reinforced Fe-based composite material in which mechanical properties are improved by dispersing TiC particles in a hard phase on an Fe alloy matrix, and a method for manufacturing the same.
  • the ceramic particle-reinforced Fe-based composite material is lighter and has excellent mechanical properties such as high temperature strength, abrasion resistance and high hardness by dispersing high hardness reinforcement materials such as TiC, TiB 2 and Al 2 O 3 as hard particles on the Fe alloy matrix. It is a composite material implemented.
  • TiC exhibits high hardness (92HRC), modulus of elasticity (439GPa), and high melting point (3160°C). It is used a lot.
  • TiC particle-reinforced Fe-based composite material has a lower density and superior structural strength than steel or tungsten carbide (WC) particle-reinforced metal composite, as well as excellent oxidation and corrosion resistance for high-temperature structural use in space, aviation, and military fields. It is suitable as a material, and due to its high hardness and wear resistance, it can be applied to various fields such as molds, rolling rolls, and tools.
  • the matrix may include various alloying elements in addition to Fe, and among them, an alloying element capable of improving the oxidation resistance of the composite material may be included.
  • TiC distributed in the matrix may act as a carbon source, and in this case, the oxidation resistance of the composite material may be deteriorated due to carbon supplied from TiC into the matrix. That is, when the alloy element for improving oxidation resistance contained in the matrix reacts with carbon supplied from TiC to form carbide and exists in the matrix, oxidation resistance may deteriorate.
  • the Fe alloy matrix is stainless steel containing Cr
  • carbon (C) supplied from TiC at a high temperature may react with Cr in the Fe alloy matrix to form Cr carbide.
  • Cr is an alloying element that can improve the oxidation resistance of the composite material by forming Cr oxide on the surface of the composite material. Therefore, if Cr contained in the matrix reacts with carbon supplied from TiC to form Cr carbide in the substrate, the content of Cr contributing to the formation of Cr oxide decreases accordingly. Therefore, while the formation of Cr oxide on the surface is suppressed, oxidation resistance deteriorates.
  • An object of the present invention is to solve various problems including the above problems, and to provide a method for improving the oxidation resistance of a TiC particle-reinforced Fe-based composite material.
  • these problems are exemplary and the scope of the present invention is not limited thereto.
  • a method for manufacturing a TiC particle-reinforced Fe-based composite material there is provided a method for manufacturing a TiC particle-reinforced Fe-based composite material.
  • the manufacturing method includes the steps of preparing a TiC preform; and impregnating the liquid Fe alloy into the TiC preform and then solidifying it.
  • the TiC preform may be a TiC sintered body manufactured by sintering a powder having a Ti oxide layer formed on at least a portion of the surface thereof.
  • the method for manufacturing the TiC preform includes: forming a Ti oxide layer on at least a portion of the surface by oxidizing the TiC powder; and sintering the oxidation-treated TiC powder.
  • the step of impregnating the Fe alloy in the liquid phase may be performed by a liquid phase pressure impregnation process.
  • the liquid Fe alloy may include Cr.
  • the liquid Fe alloy may be a molten metal of stainless steel.
  • a TiC particle-reinforced composite material is provided.
  • the TiC grain-reinforced composite material may include a matrix made of an Fe alloy; and a TiC reinforcement dispersed and distributed in the matrix.
  • a Ti oxide layer or a Ti composite oxide layer may be formed on at least a portion of the surface of the TiC reinforcing material.
  • the Fe alloy may include Cr.
  • it may be the stainless steel.
  • the Ti composite oxide layer may include Cr and Mn.
  • the alloy element for improving oxidation resistance in the matrix As the supply of carbon from TiC to the Fe alloy matrix is suppressed in the Ti oxide layer or Ti composite oxide layer formed on the surface of the TiC particles, the alloy element for improving oxidation resistance in the matrix The reaction of reacting with carbon to form carbide is inhibited. Therefore, as the content of the alloy element for improving oxidation resistance in the matrix that contributes to the formation of oxidation-resistant oxide on the surface does not decrease, it can contribute to the oxidation resistance of the composite material.
  • the oxidation resistance of TiC itself is improved by the Ti oxide layer or the Ti composite oxide layer formed on the TiC surface, which contributes to the improvement of the oxidation resistance of the composite material.
  • the scope of the present invention is not limited by these effects.
  • TiC oxidized TiC
  • SEM scanning electron microscope
  • EPMA Electron Probe X-ray Micro Analyzer
  • TiC (titanium carbide) particle-reinforced Fe-based composite material is manufactured by impregnating a liquid Fe alloy in a TiC preform.
  • the TiC preform may be a porous material including a large number of fine pores therein.
  • the TiC preform may be a porous sintered body prepared by sintering TiC powder.
  • the porosity of the preform may be in the range of 30 to 80% by volume.
  • the liquid Fe alloy may include one or more alloying elements in addition to Fe and may be a molten Fe alloy molten at a high temperature.
  • the alloying element may include Cr.
  • the present invention is not limited thereto, and other alloying elements in addition to Cr, for example, Mo, Ti, Mn, Fe, Cr, Ni, V, etc. may be added.
  • the liquid Fe alloy impregnated in the pores of the TiC preform is solidified in the preform to form a matrix, thereby forming a TiC particle-reinforced composite material.
  • carbon of TiC and an alloying element in the matrix may react to form carbide.
  • TiC powder having a Ti oxide layer formed on at least a portion of the surface in the preform manufacturing step is used.
  • the manufacturing of the TiC preform includes oxidizing the TiC powder to form a Ti oxide layer on at least a portion of the surface, and sintering the oxidized TiC powder.
  • the Ti oxide layer formed on the surface of the TiC powder serves as a barrier layer that blocks the supply of carbon from TiC to the matrix. Accordingly, the preform prepared by sintering TiC powder formed on the surface of Ti oxide can effectively suppress the supply of carbon from TiC to the matrix.
  • an alloying element for improving the oxidation resistance of a Fe-based composite material is contained in the matrix, such as Cr, the carbon supply to the matrix is suppressed, so that the reaction between carbon and the alloying element in the matrix is remarkably reduced. Due to this, as the alloying element is carbide and trapped in the matrix, it is possible to solve the problem of not contributing to the formation of the surface oxide layer improving oxidation resistance. As a result, the oxidation resistance property of the composite material is improved.
  • the effect of improving oxidation resistance in other aspects may appear. That is, on the surface of the TiC particle-reinforced Fe-based composite material, the TiC phase is exposed to the outside, and oxidation resistance at high temperature is improved by the Ti oxide layer formed on the surface of the TiC phase exposed to the outside, and as a result, the composite material oxidation resistance is improved.
  • This can be said to be an effect realized by using a porous material prepared using oxidation-treated TiC powder as a preform regardless of whether Cr is contained in the matrix.
  • the Ti oxide layer formed on the surface of the TiC powder may transition to the Ti composite oxide as the alloying elements in the matrix diffuse into the Ti oxide layer when the manufactured composite material is exposed to a high-temperature oxidizing atmosphere.
  • Cr, Mn, etc. when Cr, Mn, etc. are included as alloying elements in the matrix, Cr, Mn, etc. in the matrix diffuse into the Ti oxide layer on the TiC surface in a high-temperature oxidizing atmosphere, and these Cr and Mn react with the Ti oxide layer
  • a Ti composite oxide ((Ti, Cr, Mn) oxide) containing Cr and Mn.
  • This Ti composite oxide layer also performs the same role as the above-described Ti oxide layer.
  • the process of impregnating the liquid Fe alloy into the preform may be performed by a liquid processing infiltration process.
  • Liquid pressure impregnation is a process in which a preform is charged in a predetermined mold, a molten metal in which a metal alloy is melted is put into the mold, and then the molten metal is pressurized with gas pressure to perform impregnation into the preform.
  • the liquid pressure impregnation apparatus 10 includes a chamber 17 , a lower mold 12 and an upper mold 13 disposed inside the chamber 17 .
  • the chamber 17 is designed to create a vacuum state by a connected vacuum pump (not shown), and to increase the pressure inside the chamber 17 by introducing gas through the gas inlet 18 to enable pressurization.
  • Both the lower mold 11 and the upper mold 13 can be heated by the heater 14 .
  • the preform 12 is charged in the lower mold 12 , and the molten metal 15 used for impregnation is disposed in the upper mold 13 .
  • a liquid pressure impregnation method according to an embodiment of the present invention will be described step by step with reference to FIGS. 8 to 10 .
  • the metal to be melted is charged in the state in which the molten metal outlet 19 at the lower part of the upper mold 13 is closed with the gate rod 15 in the upper mold 13, and the preform 12 is placed in the lower mold 11 as shown in FIG. insert
  • the upper mold 13 is heated with a heater 14 while maintaining the inside of the chamber 17 in a vacuum state at a preset level to melt the metal charged in the upper mold 13 to form the molten metal 16 . .
  • the gate rod 15 in the upper mold 13 is opened and the molten metal 16 is put into the lower mold 11 in which the preform 12 is loaded through the molten metal outlet 19 .
  • an inert gas such as Ar is introduced into the chamber 17 through the gas inlet 18 to create a pressurized environment, and then the molten metal 16 is impregnated with the preform 12 under pressure by maintaining it for a certain period of time. After the pressure impregnation is completed, the composite material 20 is manufactured by cooling the molten metal to solidify.
  • a TiC powder specimen having an average particle size of 3.2 ⁇ m was charged into a heat treatment furnace and then oxidized at 1400° C. in an atmospheric atmosphere to form TiO 2 on the surface of the TiC powder.
  • TiC oxidized TiC
  • SEM scanning electron microscope
  • Ti and oxygen (O) are mainly detected as a result of surface component analysis of TiC powder by oxidation treatment. From this, it can be confirmed that the surface of the TiC powder is oxidized to become Ti oxide.
  • FIG. 2 shows the results of X-ray diffraction analysis of the same specimen. Referring to FIG. 2 , it was confirmed that a TiO 2 diffraction peak having TiC and a rutile phase was observed, and from this, it can be seen that a TiO 2 layer was formed on the surface while maintaining the crystal structure of the TiC powder.
  • the oxidation-treated TiC powder was applied with 80 MPa pressure using a uniaxial pressure molding machine to form a preform with a diameter of 100 mm and a height of 50 mm, and sintered in an argon atmosphere at 1400° C. for 2 hours.
  • the volume ratio of TiC was about 60% A TiC preform was fabricated.
  • Liquid pressure impregnation was performed using the liquid pressure impregnation apparatus shown in FIGS. 8 to 10 .
  • stainless steel SUS431 was used as the Fe alloy.
  • SUS431 was charged in the upper mold 13 and TiC preform 12 was charged in the lower mold 11 .
  • the gate rod 15 in the upper mold 13 is opened, and the SUS431 molten metal 16 is introduced through the molten metal outlet 19 into the lower mold 11 in which the TiC preform 12 is charged.
  • a TiC/SUS composite material was manufactured by introducing Ar gas (arrow) into the chamber 17 to create a pressurized environment and maintaining it for a predetermined time.
  • the particle-form TiC (31) reinforcing material is uniformly distributed throughout the US431 matrix (32), and most of TiC exhibits a size of 10 ⁇ m or less.
  • oxidized TiC/SUS431 represents an example, and TiC/SUS431 represents a comparative example.
  • the Example of the present invention shows a small change in weight over time compared to the Comparative Example, and from this, it can be confirmed that the oxidation resistance of the Example is superior to that of the Comparative Example.
  • FIG. 5 shows the results of analyzing the comparative example in which the oxidation test is completed by EPMA
  • FIG. 6 shows the results of analyzing the example in which the oxidation test is completed by EDS.
  • a complex oxide such as TiO 2 , Cr 2 O 3 , and MnO 2 is formed on the surface of the TiC particle. It is believed that during the oxidation test process, Cr and Mn in SUS431 as a matrix diffuse into Ti oxide formed on the surface of TiC particles to form Ti composite oxide.
  • FIG. 7 is an X-ray diffraction analysis result of an example in which the oxidation test is completed. Referring to FIG. 7 , diffraction peaks of TiO 2 and Cr 2 O 3 were found on the surface, and it can be confirmed that Ti oxide and Cr oxide were formed on the surface thereof. It can be seen that oxidation resistance is improved due to the oxide layer formed on the surface.
  • the oxidation resistance of TiC itself is improved by the Ti oxide layer or the Ti composite oxide layer formed on the surface of TiC, which contributes to the improvement of the oxidation resistance of the composite material.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

La présente invention a pour objet un procédé pour l'amélioration de la résistance à l'oxydation d'un matériau composite à base de Fe renforcé par des particules de TiC. Selon un aspect, la présente invention concerne un procédé pour la préparation d'un matériau composite à base de Fe renforcé par des particules de TiC. Le procédé de préparation comprend les étapes consistant à : préparer une préforme en TiC ; et imprégner la préforme en TiC d'un alliage de Fe liquide, puis solidifier celui-ci. Selon un mode de réalisation de la présente invention, la préforme en TiC peut être un corps fritté en TiC fabriqué par frittage d'une poudre dans laquelle une couche d'oxyde de Ti est formée sur au moins une partie de sa surface.
PCT/KR2020/015813 2020-11-10 2020-11-11 Matériau composite à base de fe renforcé par des particules de tic et procédé pour la préparation de celui-ci WO2022102805A1 (fr)

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KR1020200149691A KR20220063626A (ko) 2020-11-10 2020-11-10 TiC 입자 강화 Fe계 복합재료 및 그 제조방법
KR10-2020-0149691 2020-11-10

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005076052A (ja) * 2003-08-28 2005-03-24 Daido Steel Co Ltd 剛性および強度が向上したチタン合金
JP2011058045A (ja) * 2009-09-10 2011-03-24 Jfe Steel Corp 粒子分散強化鋼およびその製造方法
US20180119257A1 (en) * 2014-08-28 2018-05-03 Deutsche Edelstahlwerke Specialty Steel Gmbh & Co. Kg Steel with High Wear Resistance, Hardness and Corrosion Resistance as well as Low Thermal Conductivity
KR20180126829A (ko) * 2017-05-18 2018-11-28 주식회사 대화알로이테크 탄화물 체적율이 제어된 내마모용 써멧 및 그 제조방법
CN109112338B (zh) * 2018-10-17 2020-10-30 四川铭泰顺硬质合金有限公司 一种硬质合金体的制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005076052A (ja) * 2003-08-28 2005-03-24 Daido Steel Co Ltd 剛性および強度が向上したチタン合金
JP2011058045A (ja) * 2009-09-10 2011-03-24 Jfe Steel Corp 粒子分散強化鋼およびその製造方法
US20180119257A1 (en) * 2014-08-28 2018-05-03 Deutsche Edelstahlwerke Specialty Steel Gmbh & Co. Kg Steel with High Wear Resistance, Hardness and Corrosion Resistance as well as Low Thermal Conductivity
KR20180126829A (ko) * 2017-05-18 2018-11-28 주식회사 대화알로이테크 탄화물 체적율이 제어된 내마모용 써멧 및 그 제조방법
CN109112338B (zh) * 2018-10-17 2020-10-30 四川铭泰顺硬质合金有限公司 一种硬质合金体的制备方法

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