WO2016010226A1 - Cermet et procédé pour la préparation de celui-ci - Google Patents

Cermet et procédé pour la préparation de celui-ci Download PDF

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Publication number
WO2016010226A1
WO2016010226A1 PCT/KR2015/002161 KR2015002161W WO2016010226A1 WO 2016010226 A1 WO2016010226 A1 WO 2016010226A1 KR 2015002161 W KR2015002161 W KR 2015002161W WO 2016010226 A1 WO2016010226 A1 WO 2016010226A1
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cermet
titanium
carbon
weight
based material
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PCT/KR2015/002161
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English (en)
Korean (ko)
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송명훈
홍순형
이원혁
류호진
신영민
이준호
황금철
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주식회사 대화알로이테크
한국과학기술원
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Publication of WO2016010226A1 publication Critical patent/WO2016010226A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides

Definitions

  • the present invention relates to a cermet and a method for producing the same.
  • Cermet is a compound word of ceramic and metal, and metal and alloy are matrix in a wide range, and it includes ceramic particles, which have the advantages of metal and ceramic. .
  • the cermet material is distinguished from cemented carbide, which is the most widely used for cutting tool systems in manufacturing. Compared to cemented carbides in the prior art, there was a limitation in application due to the significantly lower strength and toughness.In order to solve this problem, an improved cermet was developed to increase the matrix content and compensate the decrease of hardness by strengthening the heat treatment on the matrix. It became.
  • the improved cermet is manufactured by mixing the ceramic particle powder with individual elemenet or alloyed powder and then forming sintering step. The abrasion resistance and toughness vary greatly depending on the manufacturing conditions.
  • the size of the product that can be manufactured because sintering is performed under conditions in which the matrix phase is changed into a liquid phase for sufficient wet of the matrix phase.
  • the cermet is manufactured in the form of a casting form and a desired product in the form of a pre-form having a large porosity, and the base alloy is made into a liquid form.
  • powder metallurgy demands high cost due to high base metal price and difficult machining, simple product shape, limited size, complicated stage, and high investment equipment cost compared to liquid phase. There is this.
  • the melt pressure impregnation method is capable of manufacturing large and near-net composites, and enables the design and cutting of characteristics by inclining the center and surface of the composite material, and the simple steps by the pressure impregnation step of the molten metal, and low cost.
  • each step has advantages and disadvantages, it is required to have excellent mechanical properties (tensile, compressive, abrasion, fatigue, creep, etc.) at room temperature and high temperature due to the excellent interfacial properties between the matrix and the formed reinforcement phase when manufacturing the metal composite material.
  • the present invention is to solve the problems of the related art, it is an object of the present invention to provide a cermet excellent in the mechanical properties at room temperature and high temperature because of the excellent interfacial properties between the base alloy and the formed reinforcement phase and its manufacturing method.
  • another object of the present invention is to produce a metal composite material at a low temperature (soaking temperature), significantly improving the life of the equipment installation step, less shape deformation during the manufacture of large products, the cermet that can significantly reduce material loss And a method for producing the same.
  • the carbon-based material Titanium-based materials; And an alloy base including at least one selected from the group consisting of Fe, Ni, Mo, Cr, Si, Mn, and Cu.
  • the carbon-based material and the titanium-based material may form a reinforcing phase including titanium carbide (TiC).
  • the reinforcing phase may include titanium carbide (TiC) formed by an in-situ reaction in the alloy matrix.
  • TiC titanium carbide
  • the reinforcing phase may have a particle size of 1.0 ⁇ m to 50 ⁇ m.
  • the reinforcement phase may be spherical.
  • the carbon-based material the group consisting of graphite, graphene, carbon black, diamond, diamond like carbon (DLC), fullerene (fullerene, C60), carbon fiber, carbon nanorods and carbon nanotubes (CNT) It may be to include at least one selected from.
  • the titanium-based material is at least one selected from the group consisting of iron titanium (FeTi), manganese titanium (MnTi), barium titanium (BaTi), strontium titanium (SrTi), nickel titanium (NiTi) and cobalt titanium (CoTi). It may be to include.
  • the mixing ratio of the carbon-based material / the titanium-based material may be 0.25 to 3.0.
  • the carbonaceous material in the cermet may be 0.5% to 5.0% by weight.
  • the alloy base may include a tool steel system including at least one selected from the group consisting of Fe, STD 11, STD 61, SKH 2 and SKH 9; Or STS 430, STS 409, STS410, STS 440 (C), and STS 630 (17-4PH) may include a stainless alloy including at least one or more selected from the group consisting of.
  • the alloy base containing Fe is 3% by weight to 25% by weight of chromium (Cr), more than 0% by weight of nickel (Ni), 5% by weight or less, and 0.1% by weight of silicon (Si) in the alloy base containing Fe.
  • Cr chromium
  • Ni nickel
  • Si silicon
  • the reinforcing phase and the alloy base may be consistent.
  • the cermet may be one having a relative density of 90% or more.
  • a second aspect of the present invention provides a method for mixing a carbonaceous material, a titanium-based material and an alloy base including at least one metal selected from the group consisting of Fe, Ni, Mo, Cr, Si Mn, and Cu; Grinding the mixture; Compacting the ground mixture; And in-situ reaction sintering the molded product, which may include a method of manufacturing a cermet.
  • the in situ reaction sintering step may be to maintain for 0.5 hours to 24 hours in the temperature range of 1100 °C to 1400 °C and pressure range of 1 ⁇ 10 -3 Torr to 1 ⁇ 10 1 Torr.
  • the carbon-based material and the titanium-based material may be to form a reinforcement phase including TiC.
  • the reinforcing phase may have a particle size of 1.0 ⁇ m to 50 ⁇ m.
  • the reinforcement phase may be spherical.
  • the reinforcing phase and the alloy base may be consistent.
  • the cermet according to the present invention and a method for manufacturing the same are capable of mass-producing a cermet produced by in-situ reaction of a ceramic-reinforced phase (TiC) in an alloy matrix phase at a low cost, and interfacial properties between the matrix alloy and the formed reinforced phase
  • TiC ceramic-reinforced phase
  • the excellent cermet can be manufactured at room temperature and high temperature with excellent mechanical properties such as tension, compression, wear, fatigue, creep, and the like. It can proceed at a much lower temperature than the conventional sintering step, thereby providing excellent equipment life and shape stability of the cermet, and excellent wear resistance and strength.
  • FIG. 1 is a flow chart of a method for manufacturing a cermet according to an embodiment of the present invention.
  • the cermet according to the first aspect of the invention the carbon-based material; Titanium-based materials; And an alloy base including at least one selected from the group consisting of Fe, Ni, Mo, Cr, Si, Mn, and Cu.
  • the cermet according to an embodiment of the present invention may be a carbon-based material and the titanium-based material may form a reinforcing phase including titanium carbide (TiC). Therefore, the interfacial properties between the alloy base and the formed reinforcement phase are excellent, and mechanical properties such as tensile, compression, wear, fatigue, creep, etc. at room temperature and high temperature are excellent, and existing in liquid or semi-liquid base conditions. Compared with the sintering method, it has a high density even in a low solid state region.
  • TiC titanium carbide
  • the reinforcing phase may include titanium carbide (TiC) formed by an in-situ reaction in the alloy matrix.
  • TiC titanium carbide
  • the cermet according to an embodiment of the present invention can be manufactured in a manner that combines the advantages of the powder metallurgy step and the in-situ casting step, thereby significantly improving the life of the step equipment, the existing sintering step when manufacturing a large product There is less shape deformation, and material loss can be greatly reduced.
  • the reinforcing phase may have a particle size of 1.0 ⁇ m to 50 ⁇ m. If the particle size of the reinforcing phase is less than 1.0 ⁇ m, a relatively large number of matrix alloys may cause a binder phase aggregation, and if the particle size exceeds 50 ⁇ m, the wettability of the matrix alloy against the reinforcing phase may be lowered, leading to a lower toughness. As the interparticle distance increases, particle precipitation and dispersion strengthening effects (Orowan strengthening) may decrease.
  • the reinforcement phase may be spherical.
  • the surface area is small and can support higher applied stress, which has better mechanical properties, resulting in delayed dislocation movement during crack propagation and material deformation at high temperatures and reduced crack formation potential. Will have an impact.
  • the carbon-based material the group consisting of graphite, graphene, carbon black, diamond, diamond like carbon (DLC), fullerene (fullerene, C60), carbon fiber, carbon nanorods and carbon nanotubes (CNT) It may include at least one selected from, but is not limited thereto.
  • the titanium-based material is at least one selected from the group consisting of iron titanium (FeTi), manganese titanium (MnTi), barium titanium (BaTi), strontium titanium (SrTi), nickel titanium (NiTi) and cobalt titanium (CoTi). It may be to include, but is not limited thereto.
  • the mixing ratio of the carbon-based material / the titanium-based material may be 0.25 to 3.0.
  • the mixing ratio of the carbonaceous material / titanium material is less than 0.25, residual Ti, which does not form carbide, remains in the base alloy in oxide form and acts as inclusions to significantly lower the low temperature and high temperature properties. And, if it is more than 3.0, there may be a problem such that the sintered stability is impaired by remaining in the base alloy of excess carbon not participating in the reaction, and the manufactured sintered body also has brittleness.
  • the carbonaceous material in the cermet may be 0.5% to 5.0% by weight. If the carbonaceous material is less than 0.5% by weight, it is difficult to obtain a dense and compact sintered body with the above-mentioned problems due to the Ti residue not participating in the reaction, and if it is more than 5.0% by weight, it is local due to the residual in the base alloy of excess carbon. As a result of the significant melting, the sintering stability is lowered, including a phenomenon in which near-net product manufacturing is difficult, and the manufactured sintered body may be brittle.
  • the alloy base may include a tool steel system including at least one selected from the group consisting of Fe, STD 11, STD 61, SKH 2 and SKH 9; Or STS 430, STS 409, STS410, STS 440 (C), and STS 630 (17-4PH), but may include a stainless alloy system including at least one selected from the group consisting of, but is not limited thereto. .
  • the stainless alloy may be martensite type or precipitation hardening type.
  • the alloy base containing Fe is 3% by weight to 25% by weight of chromium (Cr), more than 0% by weight of nickel (Ni), 5% by weight or less, and 0.1% by weight of silicon (Si) in the alloy base containing Fe.
  • Cr chromium
  • Ni nickel
  • Si silicon
  • the cermet further includes at least one or more selected from the group consisting of chromium (Cr), nickel (Ni), silicon (Si), manganese (Mn), copper (Cu) and molybdenum (Mo), tensile strength, Hardness, toughness, stiffness, abrasion resistance, impact resistance, corrosion resistance and creep characteristics can be improved.
  • the reinforcing phase and the alloy base may be coherency.
  • Matching is related to the atomic array matching between newly formed particles (hardened phases, TiCs) and alloy bases.
  • good atomic arrangements have good mechanical properties, especially at high temperatures.
  • Precipitation hardening (including in situ reactivity) and mechanically alloying (MA) particles are coherent and thus have significantly better mechanical properties than the properties of the alloy matrix.
  • Ex-situ TiC mixing such as powder metallurgy (PM), exhibits an incoherent atomic arrangement of the reinforcement phase and matrix and is further degraded at the same content than that formed by in situ reactions. Will be shown.
  • the degree of consistency can be confirmed by directly observing the atomic arrangement by high magnification SEM, high magnification TEM, etc., or by changing the lattice parameter at the interface through XRD.
  • the cermet may be one having a relative density of 90% or more.
  • Relative density represents the degree of compactness (density). Since cermets are usually manufactured at a relative density (100%) close to true density, the closest to true density is tensile, compression, wear, fatigue, It is excellent in mechanical properties such as creep.
  • the alloy base comprising a carbon-based material, titanium-based material and at least one metal selected from the group consisting of Fe, Ni, Mo, Cr, Si Mn, Cu Mixing; Grinding the mixture; Compacting the ground mixture; And in-situ reaction sintering the molding.
  • FIG. 1 is a flow chart of a method for manufacturing a cermet according to an embodiment of the present invention.
  • the mixing step (S110), grinding step (S120), compression molding step (S130) and in situ reaction sintering step (S140) may include.
  • the carbon-based material the group consisting of graphite, graphene, carbon black, diamond, diamond like carbon (DLC), fullerene (fullerene, C60), carbon fiber, carbon nanorods and carbon nanotubes (CNT) It may include at least one selected from, but is not limited thereto.
  • the titanium-based material is at least one selected from the group consisting of iron titanium (FeTi), manganese titanium (MnTi), barium titanium (BaTi), strontium titanium (SrTi), nickel titanium (NiTi) and cobalt titanium (CoTi). It may be to include, but is not limited thereto.
  • the mixing ratio of the carbon-based material / the titanium-based material may be 0.25 to 3.0.
  • the mixing ratio of the carbonaceous material / titanium material is less than 0.25, residual Ti, which does not form carbide, remains in the base alloy in oxide form and acts as inclusions to significantly lower the low temperature and high temperature properties. And, if it is more than 3.0, there may be a problem such that the sintered stability is impaired by remaining in the base alloy of excess carbon not participating in the reaction, and the manufactured sintered body also has brittleness.
  • the carbonaceous material in the cermet may be 0.5% to 5.0% by weight. If the carbonaceous material is less than 0.5% by weight, it is difficult to obtain a dense and compact sintered body with the above-mentioned problems due to the Ti residue not participating in the reaction, and if it is more than 5.0% by weight, it is local due to the residual in the base alloy of excess carbon. As a result of the significant melting, the sintering stability is lowered, including a phenomenon in which near-net product manufacturing is difficult, and the manufactured sintered body may be brittle.
  • the alloy base may include a tool steel system including at least one selected from the group consisting of Fe, STD 11, STD 61, SKH 2 and SKH 9; Or STS 430, STS 409, STS410, STS 440 (C), and STS 630 (17-4PH), but may include a stainless alloy system including at least one selected from the group consisting of, but is not limited thereto. .
  • the stainless alloy may be martensite type or precipitation hardening type.
  • the alloy base containing Fe is 3% by weight to 25% by weight of chromium (Cr), more than 0% by weight of nickel (Ni), 5% by weight or less, and 0.1% by weight of silicon (Si) in the alloy base containing Fe.
  • Cr chromium
  • Ni nickel
  • Si silicon
  • the cermet further includes at least one or more selected from the group consisting of chromium (Cr), nickel (Ni), silicon (Si), manganese (Mn), copper (Cu) and molybdenum (Mo), tensile strength, Hardness, toughness, stiffness, abrasion resistance, impact resistance, corrosion resistance and creep characteristics can be improved.
  • Grinding the mixture (S120) may be ground in a grinding vessel.
  • the grinding may be dry grinding or wet grinding, the dry grinding may include a dry ball mill, a dry jet mill step, and the wet grinding may include an ultrasonic wave, a wet ball mill, a wet jet mill step.
  • ball milling can be performed.
  • the ball mill is a ball milling jar of a material selected from tool steel, stainless steel, cemented carbide, silicon nitride, alumina and zirconia, and the like. It can be carried out using a ball of material selected from these. For example, a ball having a diameter of 5 to 30 mm may be used, and all balls having the same size may be used, or balls having two or more sizes may be used together.
  • the ratio of the mixture and the ball introduced into the ball milling vessel may be in the range of 1: 1 to 1: 100 by weight. If the weight ratio of the mixture and the ball is less than 1: 1, the amount of impurities incorporated by the wear of the ball and the ball milling container may increase more than necessary, and if it exceeds 1: 100, the milling effect is lowered and uniform. Mixture preparation can be difficult.
  • ball milling is performed by filling a ball mill container with ethyl alcohol, heptane (organic solvent), etc., followed by a shaker mill, a vibratory mill, a planetary mill, or an attritor mill. ) May be included.
  • the container containing the ball performs revolution and rotation at the same time to maximize the collision energy of the ball to make the powder more fine and can be carried out by using a planetary mill to uniform particle size.
  • the reason for filling the ethyl alcohol in the ball milling vessel is to prevent the oxidation of the powder by oxygen in the air during milling.
  • the ball is separated using a whisk, and heated through an external separate heat source such as a heater to evaporate the ethyl alcohol, when the naked eye confirms that all of the ethyl alcohol is evaporated, the powder burns. Further fixing may be carried out to immediately remove the heat source and to dry with residual heat to prevent it.
  • the dried powder is spun in the form of a sponge and is crushed.
  • the powder is put in a grinder or mortar and pulverized, and the pulverized powder is put in a vacuum dryer, for example, after drying at a temperature of 65 ° C. or higher for 4 hours or more.
  • the pulverized powder can be obtained by filtering with a 63 ⁇ m eyepiece.
  • the powder (the resultant) synthesized by ball milling may be collected and molded into a predetermined shape to form a molded body.
  • zinc stearate may be applied as a lubricant to improve the lubricity on the mold wall of the compression molding machine.
  • the powder may be mixed with a binder in which 50 g of polyvinyl alcohol (PVA) or isopropyl alcohol (IPA) is dissolved in 1 l of distilled water, and the binder is 2.5 to 2.5 weight of the powder to be press-molded. 3 weight% can be mixed. The reason is that when the binder is less than 2.5% by weight, the molding is not good, and when the binder is more than 3% by weight, the binder flows out of the molded body.
  • PVA polyvinyl alcohol
  • IPA isopropyl alcohol
  • the powder in which the binder is well mixed is weighed and placed in the mold of the compression molding machine, and, for example, by pressing a pressure of 50 MPa, the powder compact can be press-molded. If the pressure is lower than 50 MPa, the density is lowered, so that the desired physical properties of the desired density cannot be obtained. If the pressure is higher than 50 MPa, the density is increased, but the overload is loaded, and cracks are likely to occur inside the molded body.
  • In-situ reaction sintering step (S140) may be performed in a vacuum or argon (Ar) atmosphere of 10 ⁇ 2 torr or less.
  • the in situ reaction sintering step may be to maintain for 0.5 hours to 24 hours in the temperature range of 1100 °C to 1400 °C and the pressure range of 1 ⁇ 10 -3 Torr to 1 ⁇ 10 1 Torr.
  • the sintering temperature is less than 1100 ° C.
  • the sintering pressure is less than 1 ⁇ 10 ⁇ 3 Torr
  • the sintering time is less than 0.5 hour, a sufficient sintering effect cannot be obtained
  • the sintering temperature is more than 1400 ° C., and the sintering pressure is 1
  • the result is underestimated because the particles of TiC occur abnormal grain growth to be the physical properties of hardness and flexural strength of the sintered body is lowered together.
  • the present invention may be characterized by undergoing a vacuum sintering process without pressure.
  • the pressure is increased by the pressurization, the control of the amount of carbon remaining in the sintered body due to the oxidation and the increase of the binder residue is virtually impossible, there may be a problem that is not industrially available.
  • the in situ reaction sintering step may further comprise a hot isostatic pressing (HIP) step.
  • HIP hot isostatic pressing
  • the sintered body is heated through a high temperature isostatic molding step, it plays a role of promoting densification. The characteristics are improved by removing defects such as residual pores, and a cermet of near-theoretical density can be manufactured.
  • the method may further include cooling to room temperature.
  • the carbon-based material and the titanium-based material may be to form a reinforcement phase including TiC. Therefore, the reinforcing phase (TiC) in the alloy matrix phase may be generated by the in-situ reaction.
  • the reinforcing phase may have a particle size of 30 ⁇ m to 150 ⁇ m.
  • the particle size of the reinforcing phase is less than 30 ⁇ m, a relatively large number of matrix alloys may cause a binder phase aggregation, and when the particle size exceeds 150 ⁇ m, the wettability of the matrix alloy against the reinforcing phase may be lowered, thereby lowering the toughness. have.
  • the reinforcement phase may be spherical.
  • the surface area can support higher applied stress, which has better mechanical properties, and delays the displacement of dislocations and the possibility of crack formation during material deformation at high temperatures. Will have an impact.
  • the reinforcing phase and the alloy base may be consistent. Such consistency can be directly observed by high magnification SEM, high magnification TEM, etc., or the change of lattice parameter at the interface through XRD to confirm the degree of consistency.
  • the cermet may be one having a relative density of 90% or more. Since cermets should be manufactured at relative density (100%), which is usually close to true density in terms of application characteristics, those close to true density are excellent in mechanical properties such as tensile, compression, wear, fatigue, and creep.
  • the cermet according to the present invention and a method for producing the same have excellent interfacial properties between the matrix alloy and the formed reinforcing phase, and thus excellent mechanical properties at room temperature and high temperature. It can proceed at much lower temperatures than the conventional sintering step, resulting in excellent plant life and cermet shape stability.
  • Ti powder and graphite powder have a C / Ti ratio of 1.5, as shown in Table 1 below, and 78.3 wt% of STD-11, 16.0 wt% of TiH 2 , and 5.8 wt% of carbon source as a base alloy.
  • the mixture was mixed to form a whole mixed powder.
  • the ball mill process was carried out on the ball mill apparatus for 20 hours at an optimum rotation speed of about 150 rpm considering the drop of the ball. Was carried out.
  • the pulverized powder is collected, charged into a hydraulic press and molded at a pressure of 50 MPa, and the molded body is sintered in a vacuum atmosphere of 5 ⁇ 10 -2 Torr for 2 hours in a vacuum furnace where the temperature is maintained at 1250 ° C., followed by a sintering furnace. It cooled to room temperature inside.
  • a sintered compact having a spherical TiC, a density of 6.85 g / cm 3 and a relative density of 98.2% was prepared.
  • Example 2 Same as Example 1 except that the C / Ti ratio was 1.0, the base alloy STD-11 content was 60.7 wt%, the TiH 2 was 31.7 wt%, the carbon source was 7.6 wt%, and the sintering temperature was set at 1280 ° C.
  • Spherical TiC, density 6.20 g / cm 3 which was prepared in the same manner as in Example 1 except that 48.9 wt% of Fe-34Ti was added without adding TiH 2 to 48.9 wt% of the known alloy STD-11. And a sintered compact having a relative density of 95.8% were prepared.
  • the sintered bodies of Examples 1 to 5 had a spherical TiC shape and excellent physical properties of density and relative density, compared to the sintered bodies of Comparative Example 1.
  • the relative densities of Examples 1 to 5 were close to true densities.

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Abstract

La présente invention concerne un cermet et un procédé pour la préparation de celui-ci. Un cermet selon un mode de réalisation de la présente invention peut comprendre : un matériau à base de carbone ; un matériau à base de titane ; et une matrice d'alliage contenant au moins un élément choisi dans le groupe constitué par Fe, Ni, Mo, Cr, Si, Mn et Cu.
PCT/KR2015/002161 2014-07-15 2015-03-06 Cermet et procédé pour la préparation de celui-ci WO2016010226A1 (fr)

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KR101736108B1 (ko) * 2015-06-09 2017-05-17 주식회사 대화알로이테크 써멧의 주조식 제조방법 및 그에 의해 제조된 써멧
CN106756388A (zh) * 2016-12-26 2017-05-31 苏州新锐合金工具股份有限公司 增韧Ti（C，N）基金属陶瓷复合材料的制备工艺
KR101935386B1 (ko) 2017-05-18 2019-01-07 주식회사 대화알로이테크 가압 함침용 강화재 예비성형체의 부유 방지 방법 및 부유 방지용 몰드
KR101935389B1 (ko) * 2017-05-18 2019-04-03 주식회사 대화알로이테크 탄화물 체적율이 제어된 내마모용 써멧 및 그 제조방법
KR102478654B1 (ko) * 2017-07-11 2022-12-16 한국재료연구원 계면 물질을 포함하는 복합재료 및 이의 제조방법
KR102148026B1 (ko) * 2018-07-26 2020-08-26 주식회사 디에이티신소재 이종재료 접합 및 가압 함침 공정을 이용하여 제조된 압연롤 및 그 제조방법
KR102271297B1 (ko) * 2018-12-12 2021-06-29 주식회사 포스코 티타늄-탄소 복합체, 이의 제조 방법 및 이를 포함하는 소결체
KR102120015B1 (ko) * 2019-09-19 2020-06-09 재단법인 경북하이브리드부품연구원 나노 다이아몬드 분말 및 금속 분말을 이용한 금속 매트릭스 소결체 및 이의 제조방법
KR102258486B1 (ko) * 2020-07-13 2021-05-31 주식회사 경진 스테인레스 스틸 분말을 사용하여 향상된 내식성을 갖는 소결 제품을 제조하는 방법

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