CN112831679B - Two-phase enhanced high-entropy alloy-based composite material and preparation method thereof - Google Patents
Two-phase enhanced high-entropy alloy-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a two-phase reinforced high-entropy alloy-based composite material and a preparation method thereof, wherein the composite material is obtained by vacuum arc melting and in-situ reaction in a matrix to generate a reinforced phase; the method comprises the following steps: firstly, using alloy elements with various components: designing components of Cr, Ni, Fe, Co, Si, Ti and C, mixing Si, Ti, C and Fe powder, ball-milling, drying, and performing cold extrusion by using a press to obtain a block to obtain a reinforcement test block; and then the reinforcement test block and Cr, Ni and Co particles are put into a vacuum melting furnace together for vacuum melting, and finally the TiC and SiC two-phase reinforced high-entropy alloy FeCrCoNi-based composite material is obtained. The invention adopts a vacuum induction melting method to generate an endogenous two-phase enhanced high-entropy alloy-based composite material, micro-nano two-phase dispersion distributed reinforcements refine crystal grains and strengthen a matrix through synergistic action, and the surface of the reinforcement generated by in-situ reaction is clean, the infiltration with the matrix alloy is good, the preparation method is simple to operate, and the energy consumption is small.
Description
Technical Field
The invention relates to a preparation method of a two-phase reinforced high-entropy alloy-based composite material, belonging to the field of material preparation.
Background
The high-entropy alloy-based composite material has excellent mechanical property, corrosion resistance and high-temperature resistance, and has important research value and wide application prospect. At present, most researches only adopt single-scale or single-phase particles to reinforce the high-entropy alloy-based composite material, and have limitations on enhancing the performance of the high-entropy alloy-based composite material, while multi-scale and multi-type reinforcing phases can enable the performance to be more excellent. TiC is a hard refractory ceramic, has good mechanical properties, high hardness and elastic modulus, SiC is widely applied and has excellent thermal properties, micron-sized TiC and nano-sized SiC are dispersed in a matrix, and grains can be refined, the toughness is improved and the matrix is reinforced through the micro-nano synergistic effect. The vacuum induction melting is a preparation method for heating raw materials to be melted by generating eddy current in a metal body by utilizing an electromagnetic induction heating principle under a vacuum condition, and the method has the advantages of short melting period, uniform alloy components and the like. The reinforced phase is generated in the matrix through in-situ reaction and is compounded with the matrix in situ, so that the surface of the reinforced phase is clean, the infiltration with the matrix alloy is good, and the distribution and the granularity of the reinforced phase are easy to control.
In the first document, an AlCrFeNi-TiC composite material is smelted by a non-consumable arc smelting furnace, and compared with an AlCrFeNi matrix alloy, the yield strength and the breaking strength of the AlCrFeNi-TiC composite material are improved, but the elastic deformation and the plastic deformation are reduced (Zhang Yi. A1crFeNi multi-principal element high-entropy alloy matrix composite material microstructure and performance research [ D ]. Harbin: Harbin university of industry, 2010). The literature also discloses a method for preparing a high-entropy alloy-based composite material (Rogal T, Kalite D, Tarasek A, et al. Effect of SiCNo-particles on microstructure and mechanical properties of CoCrFeMnNi high entropy alloy [ J ]. Journal of Alloys and semiconductors, 2017, 708: 344-.
Disclosure of Invention
The invention aims to provide a two-phase reinforced high-entropy alloy-based composite material and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows: a method for preparing a two-phase reinforced high-entropy alloy-based composite material by a vacuum melting method comprises the following steps:
firstly, weighing high-purity Cr, Ni and Co particles according to the composition of a target composite material;
secondly, weighing Si, Ti, C and Fe powder according to the composition of the target composite material, putting the powder into a ball mill, carrying out ball milling and mixing, drying, and then carrying out cold extrusion by adopting a press to obtain an enhanced test block;
thirdly, the metal particles weighed in the first step and the reinforcement test block prepared in the second step are put into a vacuum melting furnace together, and the vacuum melting furnace is vacuumized until the vacuum degree reaches 10-3Introducing argon gas for protection after Pa is higher than Pa, slowly raising the induced current to 500A, raising the induced current to 550A when the metal particles are molten, preserving the heat for 5-10 minutes, pouring the metal particles into a water-cooled copper crucible, slowly lowering the current to 350A, and cooling to room temperature to obtain the high-entropy alloy-based composite material.
Preferably, in the first step, Cr, Ni and Co particles with high purity and equal molar ratio are weighed.
Preferably, in the second step, the volume content of the reinforcement in the target composite material is 5-10%, preferably 10%.
Preferably, in the second step, the molar ratio of Si, Ti and C is 2.26:1:3.26, and the molar ratio of Fe to Co is 1: 1.
Preferably, in the second step, the ball powder ratio is 5: 1, the ball milling speed is 250p.r.m, and the ball milling time is 8 h.
Preferably, in the second step, the drying temperature is 110-120 ℃, the drying time is 1.5 hours, and the block is extruded under the pressure of 180 MPa.
Compared with the prior art, the invention has the following remarkable advantages: (1) and multi-scale and multi-type reinforcements are adopted, micron-scale TiC and nano-scale SiC are dispersed in the matrix, and grains are refined through the micro-nano synergistic effect to strengthen the matrix. (2) The surface of the reinforced phase generated by the in-situ reaction is clean and well infiltrated with the matrix alloy. Meanwhile, the distribution and the granularity of the reinforced phase are easy to control, and the elastic modulus and the strength of the material can be greatly improved while the material is ensured to have better plasticity. (3) The vacuum induction melting can volatilize impurity elements with vapor pressure higher than that of the matrix, is beneficial to degassing and homogenization of alloy components, and has low heating efficiency and energy consumption.
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 an SEM scan of the high entropy alloy based composite material of example 1 of the present invention.
Fig. 3 is an XRD diffraction pattern of the high-entropy alloy-based composite material of example 2 of the present invention.
Fig. 4 is an SEM scan of the high entropy alloy based composite material of example 2 of the present invention.
Fig. 5 is an SEM scanning photograph of the high-entropy alloy-based composite material of example 3 of the present invention.
Fig. 6 is an EDS energy spectrum analysis chart of the corresponding regions a, B in the SEM scan photograph of the high-entropy alloy-based composite material of example 3 of the present invention (where a corresponds to the region a, and B corresponds to the region B).
Detailed Description
The method for preparing the two-phase reinforced high-entropy alloy-based composite material by vacuum melting specifically comprises the following steps:
(1) weighing matrix particles: weighing high-purity Cr, Ni and Co metal particles according to component design;
(2) preparing a reinforcement test block: weighing Si, Ti, C and Fe powder according to the component design, putting the powder into a ball mill for ball milling and mixing, wherein the ball powder ratio is 5: 1, the ball milling speed is 250p.r.m, and the ball milling time is 8 h. Drying for 1.5 hours after ball milling, wherein the drying temperature is 110-120 ℃, and then extruding into blocks by adopting a press under the pressure of 180 MPa;
(3) Loading a sample, vacuumizing and introducing protective gas: the metal particles weighed in the first step and the reinforcement test block prepared in the second step are put into a vacuum melting furnace together, cooling water is introduced, a mechanical pump is started to pump vacuum to below 5Pa, and then a molecular pump is started to pump vacuum to 10 DEG-4Pa, then introducing argon to make the pressure reach 10-1Pa or so;
(4) heating and smelting: 1. a temperature-rising reaction stage: slowly raising induction current up to 500A, 2, alloying: the reaction sample emits white light, the metal particles are melted and alloyed, and 3, a reinforcement is generated: raising the induced current to 550A, and simultaneously carrying out electromagnetic stirring, wherein the reinforcement is melted into the high-entropy alloy matrix and is uniformly distributed to carry out in-situ reaction;
(5) and (3) heat preservation and cooling: and (3) after the temperature is kept for 5-10 minutes, pouring the molten sample into a water-cooled copper crucible, slowly reducing the current to 350A, and cooling to room temperature to obtain the high-entropy alloy-based composite material.
Example 1: FeCrCoNi-2.5vol% TiC-2.5vol% SiC reaction system
(1) Weighing matrix particles: weighing high-purity Cr, Ni and Co metal particles according to the volume fraction of TiC being 2.5% and the volume fraction of SiC being 2.5%;
(2) preparing a reinforcement test block: weighing Si, Ti, C and Fe powder according to the component design, putting the powder into a ball mill for ball milling and mixing, wherein the ball powder ratio is 5: 1, the ball milling speed is 250p.r.m, and the ball milling time is 8 h. Drying for 1.5 hours after ball milling, wherein the drying temperature is 110-120 ℃, and then extruding into blocks by adopting a press under the pressure of 180 MPa;
(3) Loading a sample, vacuumizing and introducing protective gas: the metal particles weighed in the first step and the reinforcement test block prepared in the second step are put into a vacuum melting furnace together, cooling water is introduced, a mechanical pump is started to pump vacuum to below 5Pa, and then a molecular pump is started to pump vacuum to 10 DEG-4Pa, then introducing argon to make the pressure reach 10-1Pa is about;
(4) heating and smelting: 1. a temperature-rising reaction stage: slowly raising induction current up to 500A, 2, alloying: the reaction sample emits white light, the metal particles are melted and alloyed, and 3, a reinforcement is generated: increasing the induced current to 550A, and simultaneously carrying out electromagnetic stirring, wherein the reinforcement is melted into the high-entropy alloy matrix and is uniformly distributed to carry out in-situ reaction;
(5) and (3) heat preservation and cooling: and (3) after preserving the heat for 5-10 minutes, pouring the molten sample into a water-cooled copper crucible, slowly reducing the current to 350A, and cooling to room temperature to obtain the high-entropy alloy-based composite material.
XRD detection is carried out on the sample, as shown in figure 1, the obtained high-entropy alloy-based composite material is TiC and SiC two-phase reinforced high-entropy alloy-based composite material, and SEM detection and analysis are carried out on the sample, as shown in figure 2, the content of the reinforced phase is less.
Example 2: FeCrCoNi-7vol% TiC-3vol% SiC reaction system
(1) Weighing matrix particles: weighing high-purity Cr, Ni and Co metal particles according to the volume fraction of TiC of 7% and the volume fraction of SiC of 3%;
(2) Preparing a reinforcement test block: weighing Si, Ti, C and Fe powder according to the component design, putting the powder into a ball mill for ball milling and mixing, wherein the ball powder ratio is 5: 1, the ball milling speed is 250p.r.m, and the ball milling time is 8 h. Drying for 1.5 hours after ball milling, wherein the drying temperature is 110-120 ℃, and then extruding into blocks by adopting a press under the pressure of 180 MPa;
(3) loading a sample, vacuumizing and introducing protective gas: the metal particles weighed in the first step and the reinforcement test block prepared in the second step are put into a vacuum melting furnace together, cooling water is introduced, a mechanical pump is started to pump vacuum to below 5Pa, and then a molecular pump is started to pump vacuum to 10 DEG-4Pa, then introducing argon to make the pressure reach 10-1Pa is about;
(4) heating and smelting: 1. a temperature-rising reaction stage: slowly raising induction current up to 500A, 2, alloying: the reaction sample emits white light, the metal particles are melted and alloyed, and 3, a reinforcement is generated: raising the induced current to 550A, and simultaneously carrying out electromagnetic stirring, wherein the reinforcement is melted into the high-entropy alloy matrix and is uniformly distributed to carry out in-situ reaction;
(5) and (3) heat preservation and cooling: and (3) after the temperature is kept for 5-10 minutes, pouring the molten sample into a water-cooled copper crucible, slowly reducing the current to 350A, and cooling to room temperature to obtain the high-entropy alloy-based composite material.
XRD detection is carried out on the sample, as shown in figure 3, the obtained high-entropy alloy-based composite material is TiC and SiC two-phase reinforced high-entropy alloy-based composite material, SEM detection and analysis are carried out on the sample, as shown in figure 4, the reinforced phase distribution is found to be uniform.
Example 3: FeCrCoNi-3vol% TiC-7vol% SiC reaction system
(1) Weighing matrix particles: weighing high-purity Cr, Ni and Co metal particles according to the volume fraction of TiC being 3% and the volume fraction of SiC being 7%;
(2) preparing a reinforcement test block: weighing Si, Ti, C and Fe powder according to the component design, putting the powder into a ball mill for ball milling and mixing, wherein the ball powder ratio is 5: 1, the ball milling speed is 250p.r.m, and the ball milling time is 8 h. Drying for 1.5 hours after ball milling, wherein the drying temperature is 110-120 ℃, and then extruding into blocks by adopting a press under the pressure of 180 MPa;
(3) loading a sample, vacuumizing and introducing protective gas: the metal particles weighed in the first step and the reinforcement test block prepared in the second step are put into a vacuum melting furnace together, cooling water is introduced, a mechanical pump is started to pump vacuum to below 5Pa, and then a molecular pump is started to pump vacuum to 10 DEG-4Pa, then introducing argon to make the pressure reach 10-1Pa is about;
(4) heating and smelting: 1. a temperature-rising reaction stage: slowly raising induction current up to 500A, 2, alloying: the reaction sample emits white light, the metal particles are melted and alloyed, and 3, a reinforcement is generated: increasing the induced current to 550A, and simultaneously carrying out electromagnetic stirring, wherein the reinforcement is melted into the high-entropy alloy matrix and is uniformly distributed to carry out in-situ reaction;
(5) And (3) heat preservation and cooling: and (3) after the temperature is kept for 5-10 minutes, pouring the molten sample into a water-cooled copper crucible, slowly reducing the current to 350A, and cooling to room temperature to obtain the high-entropy alloy-based composite material.
The sample was subjected to SEM and EDS inspection as shown in FIGS. 5 and 6, and it was found that the polygonal phase with a well-defined edge angle was TiC and the circular-like phase was SiC.
Claims (5)
1. A method for preparing a two-phase reinforced high-entropy alloy-based composite material by a vacuum melting method is characterized by comprising the following steps of:
firstly, weighing high-purity Cr, Ni and Co particles according to the composition of a target composite material;
secondly, weighing Si, Ti, C and Fe powder according to the composition of the target composite material, putting the powder into a ball mill, carrying out ball milling and mixing, drying, and then carrying out cold extrusion by adopting a press to obtain an enhanced test block;
thirdly, the metal particles weighed in the first step and the reinforcement test block prepared in the second step are put into a vacuum melting furnace together, and the vacuum melting furnace is vacuumized until the vacuum degree reaches 10-3Introducing argon gas for protection after Pa is higher than Pa, slowly raising the induced current to 500A, raising the induced current to 550A when the metal particles are molten, preserving the heat for 5-10 minutes, pouring the metal particles into a water-cooled copper crucible, slowly lowering the current to 350A, and cooling to room temperature to obtain the high-entropy alloy-based composite material;
In the first step, Cr, Ni and Co particles with high purity and equal molar ratio are weighed;
the volume content of the reinforcement TiC and SiC in the target composite material is 10 percent;
the molar ratio of Fe to Co is 1: 1.
2. The method of claim 1, wherein the Si, Ti, C molar ratio is 2.26:1: 3.26.
3. The method of claim 1, wherein in the second step, the ball to powder ratio is 5: 1, the ball milling speed is 250p.r.m, and the ball milling time is 8 h.
4. The method of claim 1, wherein in the second step, the drying temperature is 110 to 120 ℃ and the drying time is 1.5 hours, and the block is extruded under a pressure of 180 MPa.
5. A dual phase reinforced high entropy alloy based composite produced by the method of any one of claims 1 to 4.
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| CN110157971A (en) * | 2019-06-06 | 2019-08-23 | 南京理工大学 | A kind of induction melting method of In-sltu reinforcement high-entropy alloy composite material |
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| CN110157971A (en) * | 2019-06-06 | 2019-08-23 | 南京理工大学 | A kind of induction melting method of In-sltu reinforcement high-entropy alloy composite material |
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