CN109694979B - Preparation of high-entropy alloy matrix composites by vacuum induction melting and method thereof - Google Patents
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 59
- 239000000956 alloy Substances 0.000 title claims abstract description 59
- 239000011159 matrix material Substances 0.000 title claims abstract description 34
- 238000002844 melting Methods 0.000 title claims abstract description 27
- 230000008018 melting Effects 0.000 title claims abstract description 27
- 230000006698 induction Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 15
- 238000000034 method Methods 0.000 title abstract description 16
- 230000002787 reinforcement Effects 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 claims abstract description 19
- 238000004321 preservation Methods 0.000 claims abstract description 15
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 7
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- 239000000843 powder Substances 0.000 claims description 26
- 239000002923 metal particle Substances 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 17
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- 229910052742 iron Inorganic materials 0.000 claims description 11
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- 239000000463 material Substances 0.000 claims description 10
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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- C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—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 carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
本发明公开了一种真空感应熔炼制备高熵合金基复合材料及其方法，所述复合材料为内生型，以AlMFeNiCu高熵合金为基体相，以（TiC）x为增强相，记为(TiC)x/(AlMFeNiCu)1‑x其中，M为Si或Co，x为0.1~0.2。其步骤为：按照原料配比称取反应试样原料；制备增强体试块；将原材料装入高频感应熔炼炉中、抽真空、通入氩气、真空熔炼、保温；将保温后的熔融液态合金倒入铜坩埚中冷却，取出，得到所述复合材料。本发明采用感应熔炼的方式合成内生性高熵合金基复合材料，合成的复合材料增强体与基体之间界面结合良好，增强体均匀分布于高熵合金基体中，此方法操作简单、安全可靠、节能省时、环境友好。
The invention discloses a high-entropy alloy-based composite material prepared by vacuum induction melting and a method thereof. The composite material is an endogenous type, and AlMFeNiCu high-entropy alloy is used as a matrix phase, and (TiC) x is used as a reinforcing phase, which is recorded as ( TiC) x /(AlMFeNiCu) 1-x wherein, M is Si or Co, and x is 0.1 to 0.2. The steps are: weighing the raw material of the reaction sample according to the raw material ratio; preparing a reinforcing body test block; loading the raw material into a high-frequency induction melting furnace, evacuating, introducing argon, vacuum melting and heat preservation; The liquid alloy is poured into a copper crucible to cool, and taken out to obtain the composite material. The invention adopts the induction melting method to synthesize the endogenous high-entropy alloy-based composite material, the interface between the synthesized composite material reinforcement and the matrix is well bonded, the reinforcement is evenly distributed in the high-entropy alloy matrix, and the method is simple to operate, safe, reliable, and reliable. Energy saving, time saving and environment friendly.
Description
Technical Field
The invention relates to a high-entropy alloy-based composite material and a preparation method thereof, in particular to an in-situ self-generated high-entropy alloy-based composite material prepared by vacuum induction melting and a method thereof, belonging to the field of material invention and preparation.
Technical background
The preparation method for preparing the high-entropy alloy-based composite material by the vacuum induction melting technology is characterized in that the composite material is prepared by heating and melting preparation raw materials by self in an induction heating mode. The preparation method is simple to operate and small in occupied space. The defects of low heating efficiency and small preparation quantity of the traditional process are overcome, and the vacuum induction melting can be used for batch production of materials. The automatic control type adjustable heating time, heating power, heat preservation time, heat preservation power and cooling time are provided; greatly improves the quality of the heated product and the heating repeatability, and simplifies the operation technology of workers. The high-entropy alloy-based composite material prepared by the method has high hardness, high wear resistance and corrosion resistance. In the process of forming the high-entropy alloy, a nano Cu phase can be formed between crystals, so that the yield strength of the material can be increased, and a certain toughening effect on the material can be achieved. The prepared high-entropy alloy-based composite material also has excellent performances in the aspects of conductivity and magnetic permeability. In addition, the high-entropy alloy-based composite material has good application prospects in the aspects of impact-resistant pieces and high-temperature-resistant dies.
Document I preparation of TiC-TiB by vacuum arc melting technology2The melting process of the CoCrCuFeNi composite reinforcement high-entropy alloy-based composite material is high in energy consumption, the amount of prepared samples has certain limitation, only a small amount of samples for arc heating can be prepared, and the CoCrCuFeNi composite reinforcement high-entropy alloy-based composite material cannot be used for batch production (Cheng J, Liu D, Liang X, et al]. Surface &Coatings Technology, 2015, 281(7): 109-. In the second document, a synthesis method of mixing powder blocks and metal blocks is adopted to prepare a FeCrCoNiCuTi/TiC high-entropy alloy composite material (Luxinhua, Harbin university of industry, 2008), and a prepared sample tissue reinforcement is non-uniformly distributed in a matrix, so that the interface bonding performance is poor, and although the wear resistance of the sample is improved, the yield strength is reduced to some extent.
Disclosure of Invention
The invention aims to provide an endogenous high-entropy alloy-based composite material prepared by a vacuum induction melting technology and a method thereof, and the process is simple to operate, safe, reliable, energy-saving, time-saving, environment-friendly and regular and fine TiB2The reinforced particles are generated by in-situ reaction, the surface is free from pollution, and the interface is clean.
The technical solution for realizing the purpose of the invention is as follows: the high-entropy alloy-based composite material is an endogenous composite material, takes AlMFeNiCu high-entropy alloy as a matrix phase and Takes (TiC)xFor the reinforcing phase, note (TiC)x/(AlMFeNiCu)1-xWherein M is Si or Co, and x is 0.1-0.2.
The method for preparing the endogenous high-entropy alloy-based composite material comprises the following steps:
firstly, weighing high-purity Al, M, Ni, Ti, Cu and Fe metal particles according to the composition of a target composite material, and pretreating the surfaces of the metal particles to remove surface oxide layers;
step two, preparing a reinforcement test block: weighing high-purity Ti powder, C powder and Fe powder according to the composition of a target composite material, ball-milling, mixing, drying, and preparing a reinforcement test block under certain pressure;
thirdly, the prepared sample is processed according to the formula (TiC)x/(AlMFeNiCu)1-xAl particles, a reinforcing body test block, Ni particles, Fe particles, M particles and Cu particles are sequentially added into the corresponding raw materials, and the vacuum degree reaches 10-3When the pressure is above Pa, introducing argon to keep the pressure not more than 10-1Pa, electrifying for induction melting, preliminarily heating to 950-1050 ℃, observing reaction in the furnace in an observation window, heating to 1450-1550 ℃, further heating to 2000-2200 ℃ when a test block to be reacted is basically melted, melting for 8-12 minutes, and repeatedly melting for 2-3 times;
step four, heat preservation and cooling: and after the temperature is preserved for 3-8 minutes, pouring the reaction molten alloy into a water-cooled copper crucible, and attaching the reinforcement particles to the surfaces of the fine-grain particles in the matrix for growing to obtain the fine-grain high-entropy alloy-based composite material.
Preferably, in the second step, the ball milling rotating speed is 250-300 p.r.m; the ball milling time is 6-8 h; the ball-to-material ratio (mass ratio of balls to powder) is 4.5: 1.
preferably, in the second step, the drying temperature is 110-120 ℃, the drying time is 2 hours, and the blank sample is extruded under 180 MPa.
Compared with the prior art, the invention has the following remarkable advantages: (1) the induction melting synthesis activation energy is lower than that of the conventional heating mode, the reaction temperature is lower, the reaction is rapid, the process operation is simple, safe and reliable, energy and time are saved, and the environment is friendly. (2) Because the temperature rise rate is high and the reaction process is short, the coarsening of the structure and the dendrite segregation are inhibited, the structure can be obviously refined by the method, meanwhile, because the reaction releases heat quickly, the self-stirring can be carried out, the high heat generated by the reaction can effectively purify the matrix, and the improvement of the performance of the material is facilitated. (3) The high-entropy alloy matrix phase generated by the reaction has amplitude modulation decomposition and lattice distortion effects so as to prevent the material from generating stress relaxation deformation due to lattice movement. (4) The high-entropy alloy-based composite material generated by the reaction has a single face-centered cubic structure, the material strength and the shaping are good, the structure is simple, no complex intermetallic compound phase is generated, and a regular single-phase or double-phase solid solution structure is formed.
Drawings
Fig. 1 is an XRD diffraction pattern of the high-entropy alloy-based composite material of example 1 of the present invention.
FIG. 2 is a SEM scanning photograph of the matrix of the high-entropy alloy-based composite material of example 1 of the invention.
FIG. 3 is an EDS spectrum analysis chart of SEM scanning of the matrix of the high-entropy alloy-based composite material of example 1 corresponding to the areas A, B and C (wherein a is the area A, B is the area B and C is the area C).
FIG. 4 is a SEM scanning picture of the high-entropy alloy-based composite material of example 2 of the invention (a is a low magnification, b is a high magnification)
Fig. 5 is an SEM micrograph of the high entropy alloy based composite of example 3.
Detailed Description
Example 1: (TiC)0.1/(AlSiFeNiCu)0.9Composite material
The method for preparing the endogenous high-entropy alloy-based composite material by vacuum induction melting specifically comprises the following steps:
(1) high-purity Al, Si, Ni, Fe and Cu metal particles are weighed according to the volume fraction of the reinforcement body of 10 percent, the surfaces of the metal particles are pretreated before use, a surface oxidation layer is taken out, and the oxidation layer is volatilized at high temperature to influence the smelting quality.
(2) Preparing a reinforcement test block: weighing high-purity Ti powder C and Fe powder according to the volume fraction of the reinforcement, and mixing to obtain ball powder with the mass ratio of 4.5: 1; the ball milling speed is 250-300 p.r.m; the ball milling time is 6-8 h. Drying at 110-120 deg.c for 2 hr, and extruding under 180MPa to form blank.
(3) Vacuumizing and introducing protective gas: after cooling water is boiled, the mixture is pumped by a mechanical pump to be vacuum<5Pa, then pumping to 10 ℃ by using a molecular pump-4Pa. After the pressure is stabilized, introducing protective gas (argon) to maintain the pressure at 10-1Pa or so, and then vacuumizing to 10 DEG-4Introducing argon after PaMake the air pressure reach 10-1And repeatedly applying Pa for 2-3 times.
(4) Adjusting the heating rate: 1. a temperature-rising reaction stage: firstly, adjusting output high-frequency current 400A, when the crucible is lightened, adjusting the output current to 350A, 2, and an enhancement body generation stage: after 5 minutes, an in-situ reaction occurs, heat is released to emit white light, and then the temperature is immediately raised to 1500 ℃ so that the reinforcing body test block is melted into the matrix. 3. Alloying: and adjusting the output current to enable the temperature to reach 1500-2000 ℃, melting and alloying the metal particles, rolling and stirring the alloy system from inside to outside in the induction self-stirring process, and uniformly distributing the reinforcement in the high-entropy alloy matrix.
(5) Step four, heat preservation and cooling: after the temperature is preserved for 5 minutes, the reaction melting alloy is poured into a water-cooled copper crucible, and the reinforcement particles are attached to the surfaces of the fine crystal particles in the matrix for growing to obtain the fine crystal high-entropy alloy-based composite material.
XRD detection is carried out on a sample, the figure 1 shows that the obtained high-entropy alloy-based composite material is a TiC-reinforced high-entropy alloy-based composite material, a part of SiC reinforcing phase and SEM (scanning electron microscope), EDS (electron Desorption) analysis sample composition is shown in the figure 2, the figure 3 shows that a main reinforcement is TiC, the growth is regular, the distribution is uniform, and a matrix is a two-phase structure rich in Fe, Ni and Si and rich in Al, Ni and Cu.
Example 2: (TiC)0.2/(AlSiFeNiCu)0.8Composite material
(1) Weighing high-purity Al, Si, Ni, Fe and Cu metal particles according to the volume fraction of the reinforcement body of 20%, pretreating the surfaces of the metal particles before use, taking out a surface oxidation layer, and volatilizing the oxidation layer at high temperature to influence the smelting quality.
(2) Preparing a reinforcement test block: weighing high-purity Ti powder C and Fe powder according to the volume fraction of the reinforcement, and mixing to obtain ball powder with the mass ratio of 4.5: 1; the ball milling speed is 250-300 p.r.m; the ball milling time is 6-8 h. Drying at 110-120 deg.c for 2 hr, and extruding under 180MPa to form blank.
(3) Vacuumizing and introducing protective gas: after cooling water is boiled, the mixture is pumped by a mechanical pump to be vacuum<5Pa, and then vacuumizing by using a molecular pumpTo 10-4Pa. After the pressure is stabilized, introducing protective gas (argon) to maintain the pressure at 10-1Pa or so, and then vacuumizing to 10 DEG-4Introducing argon after Pa to make the pressure reach 10-1And repeatedly applying Pa for 2-3 times.
(4) Adjusting the heating rate: 1. a temperature-rising reaction stage: firstly, adjusting output high-frequency current 400A, when the crucible is lightened, adjusting the output current to 350A, 2, and an enhancement body generation stage: after 5 minutes, an in-situ reaction occurs, heat is released to emit white light, and then the temperature is immediately raised to 1500 ℃ so that the reinforcing body test block is melted into the matrix. 3. Alloying: and adjusting the output current to enable the temperature to reach 1500-2000 ℃, melting and alloying the metal particles, rolling and stirring the alloy system from inside to outside in the induction self-stirring process, and uniformly distributing the reinforcement in the high-entropy alloy matrix.
(5) Step four, heat preservation and cooling: after the temperature is preserved for 5 minutes, the reaction melting alloy is poured into a water-cooled copper crucible, and the reinforcement particles are attached to the surfaces of the fine crystal particles in the matrix for growing to obtain the fine crystal high-entropy alloy-based composite material.
It can be seen from fig. 4a that the microstructure of the sample prepared by the reaction has good compactness, and the reinforcing body particles are uniformly distributed in the matrix, and it can be seen from fig. 4b that the reinforcing body grows completely and the combination between the reinforcing body and the matrix is good.
Example 3: (TiC)0.1/(AlCoFeNiCu)0.9Composite material
(1) High-purity Al, Co, Ni, Fe and Cu metal particles are weighed according to the volume fraction of the reinforcement body of 10%, the surfaces of the metal particles are pretreated before use, a surface oxidation layer is taken out, and the oxidation layer is volatilized at high temperature to influence the smelting quality.
(2) Preparing a reinforcement test block: weighing high-purity Ti powder C and Cu powder according to the volume fraction of the reinforcement, and mixing to obtain ball powder with the mass ratio of 4.5: 1; the ball milling speed is 250-300 p.r.m; the ball milling time is 6-8 h. Drying at 110-120 deg.c for 2 hr, and extruding under 180MPa to form blank.
(3) Vacuumizing and introducing protective gas: after cooling water is boiled, the mixture is pumped by a mechanical pump to be vacuum<5Pa, pumping with molecular pumpHollow to 10-4Pa. After the pressure is stabilized, introducing protective gas (argon) to maintain the pressure at 10-1Pa or so, and then vacuumizing to 10 DEG-4Introducing argon after Pa to make the pressure reach 10-1And repeatedly applying Pa for 2-3 times.
(4) Adjusting the heating rate: 1. a temperature-rising reaction stage: after charging, firstly adjusting output high-frequency current 400A, when the crucible is shiny, adjusting the output current to 350A, 2, and an enhancement body generation stage: after 5 minutes, an in-situ reaction takes place, heat is released to give off white light, and then the temperature is immediately raised to 1700 ℃ to melt the reinforcement test block into the matrix. 3. Alloying: adjusting output current to enable the temperature to reach 1800-2000 ℃, melting and alloying metal particles, wherein in the process of induction self-stirring, the alloy system is stirred in a rolling manner from inside to outside, and the reinforcement bodies are uniformly distributed in the high-entropy alloy matrix.
(5) Step four, heat preservation and cooling: after the temperature is preserved for 5 minutes, the reaction melting alloy is poured into a water-cooled copper crucible, and the reinforcement particles are attached to the surfaces of the fine crystal particles in the matrix for growing to obtain the fine crystal high-entropy alloy-based composite material.
As can be seen from the SEM picture of the composite material in fig. 5, the black regular objects are reinforcement particles TiC. The dark areas are Co-rich phases and the matrix phase is white areas.
Claims (8)
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