CN108213422B - Preparation method of carbon-containing high-entropy alloy composite material - Google Patents
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Abstract
The invention discloses a preparation method of a carbon-containing high-entropy alloy composite material, which comprises the following steps: (1) preparing high-entropy pre-alloy powder; the high-entropy pre-alloy powder consists of at least four metal elements of Fe, Co, Cr, Ni and Mn and C element; (2) and carrying out selective laser melting molding on the high-entropy pre-alloy powder, and carrying out subsequent heat treatment on the molded part to obtain the carbon-containing high-entropy alloy. The invention adopts high-entropy alloy with excellent plasticity, such as FeCoCrNi and the like as a matrix, and can ensure that the alloy still has better plasticity after laser melting forming in a selected area; meanwhile, a gap element C is introduced, so that the yield strength and the ultimate strength of the matrix are obviously improved through solid solution strengthening; the supercooling degree in the selective laser melting process is very high, the interstitial element C is uniformly dissolved in the matrix in a solid mode, no coarse carbide is segregated in a segregation mode, and therefore the plasticity of the material is guaranteed. The preparation method adopts a selective laser melting mode to obtain a high-density (more than 99%) product.
Description
Technical Field
The invention belongs to the field of alloys, and particularly relates to a method for preparing a carbon-containing high-entropy alloy composite material by adopting a selective laser melting technology.
Background
High entropy alloys refer to alloys in which at least four and more transition group alloying elements are combined together in equimolar or near equimolar proportions. Although the composition of the high entropy alloy is relatively complex, a single phase supersaturated solid solution can be formed. The high-entropy alloy has good mechanical property, corrosion resistance and oxidation resistance.
Interstitial carbon element is added into the high-entropy alloy, so that the method is a good method for strengthening the high-entropy alloy. At present, the high-entropy alloy is mainly prepared by methods such as vacuum arc melting and the like. However, the cooling speed of smelting is low, coarse hard carbide in the carbon-containing high-entropy alloy is easy to segregate at the grain boundary, and the mechanical property of the material is damaged. And parts with complex structures are not easy to form by casting, so that the requirements of some practical applications of the high-entropy alloy are not facilitated. In order to better apply the carbon-containing high-entropy alloy to engineering, it is particularly important to research the additive manufacturing method to prepare carbon-containing high-entropy alloy parts with complex shapes and uniform tissues.
The selective laser melting is used as one of additive manufacturing modes, so that a workpiece with a very complex shape can be manufactured, and the problems of difficult material processing, low material utilization rate and the like are solved; in addition, the selective laser melting process has the characteristic of high cooling speed, so that the material prepared by the technology has the advantages of fine and uniform tissue, uniform element distribution in the material and good mechanical property.
The materials prepared by selective laser melting have complex shapes, so the available strengthening modes are limited. Researchers have closed microcracks and microporosities in selective laser melted samples by hot isostatic pressing, thereby further improving the mechanical properties of selected laser melted samples. But the process of improving the performance of the sample by adopting the hot isostatic pressing increases the industrial energy consumption, reduces the precision of the product and weakens the engineering significance of the selective laser melting.
Aiming at the problem of difficult subsequent strengthening of selective laser melting parts, the technical personnel in the field are in urgent need to solve the problems that a high-entropy alloy which is low in cost and suitable for selective laser melting subsequent strengthening is sought, the printing and heat treatment process of the high-entropy alloy selective laser melting technology is explored, and the mechanical property of the material is further improved.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art and provide a method for preparing carbon-containing high-entropy alloy by adopting a selective laser melting technology.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the preparation method of the carbon-containing high-entropy alloy composite material comprises the following steps:
(1) preparing high-entropy pre-alloy powder; the high-entropy pre-alloy powder consists of at least four metal elements of Fe, Co, Cr, Ni and Mn and C element;
(2) and carrying out selective laser melting molding on the high-entropy pre-alloy powder, and carrying out subsequent heat treatment on the molded part to obtain the carbon-containing high-entropy alloy.
In the preparation method, the mole percentage of carbon atoms in the high-entropy pre-alloyed powder is preferably not higher than 5%.
In the preparation method, the preferred mol percent of carbon atoms in the high-entropy pre-alloyed powder is 1-4%.
In the preparation method, the high-entropy pre-alloy powder is preferably prepared by taking the metal simple substance and the metal carbide as raw materials.
In the above preparation method, preferably, the metal simple substance is selected from at least four of simple substances of Fe, Co, Cr, Ni and Mn; the metal carbide is one of chromium carbide, cementite and nickel carbide.
In the above production method, preferably, the heat treatment includes annealing, and precipitation strengthening is performed after the annealing.
In the above preparation method, preferably, the annealing conditions are as follows: heating the part to 350-450 ℃ within 1-2 h, preserving the heat for 2-5 h, and keeping the vacuum degree higher than 9 multiplied by 10
-3And cooling to below 100 ℃ along with the furnace under the condition of Pa.
In the above production method, preferably, the precipitation hardening conditions are: and heating the part to 800-1000 ℃, preserving the heat for 15-50 min, taking out the part, and cooling the part to room temperature in air.
In the preparation method, the scanning is preferably checkerboard type layer-by-layer scanning; the deflection angle is 50 ~ 70 when scanning layer by layer.
In the preparation method, preferably, the process conditions of the selective laser melting are as follows: the scanning laser power is 300-400W, the scanning speed is 600-2000 mm/s, the spot diameter is 70-100 μm, the scanning distance is 90-130 μm, and the powder spreading layer thickness is 30-50 μm.
According to the preparation method, preferably, when the selective laser melting is carried out, the oxygen content in the cavity is lower than 2000ppm, and the pressure in the cavity is 30-40 mbar; the substrate preheating temperature was 100 ℃.
The preparation method preferably comprises the following steps:
(1) taking metal carbide and metal simple substance as raw materials to prepare high-entropy pre-alloy powder;
(2) establishing a three-dimensional model of a part to be prepared on a computer, guiding the three-dimensional model into selective laser melting molding equipment, and setting molding process parameters;
(3) placing the high-entropy pre-alloy powder prepared in the step (1) into a powder supply cylinder in selective laser melting forming equipment, and introducing inert gas into a working cavity to preheat a metal substrate;
(4) and carrying out selective laser melting forming, and annealing and precipitation strengthening on the formed part.
The above preparation method, preferably, the method for preparing the high-entropy pre-alloyed powder is one of a gas atomization method, a centrifugal atomization method and a spheroidization method.
According to the preparation method, the particle size of the prepared high-entropy pre-alloy powder is preferably 15-45 mu m.
Compared with the prior art, the invention has the advantages that:
(1) the invention adopts high-entropy alloy with excellent plasticity, such as FeCoCrNi and the like as a matrix, and can ensure that the alloy still has better plasticity after laser melting forming in a selected area; meanwhile, a gap element C is introduced, so that the yield strength and the ultimate strength of the matrix are obviously improved through solid solution strengthening; the supercooling degree in the selective laser melting process is very high, the interstitial element C is uniformly dissolved in the matrix in a solid mode, no coarse carbide is segregated in a segregation mode, and therefore the plasticity of the material is guaranteed.
(2) In the preparation method, a high-density (more than 99%) product is obtained by adopting a selective laser melting mode, and the method is suitable for forming parts with complex shapes; the formed parts do not need to be machined, the material utilization rate is high, and the forming speed is high.
(3) The carbon-containing high-entropy alloy is different from other two-phase or multi-phase high-entropy alloys, and in the formed structure, a second phase has a certain initial size and cannot be reduced; the carbon-containing high-entropy alloy prepared by the selective laser melting method has the advantages that the carbon elements in the carbon-containing high-entropy alloy are uniformly distributed, and no carbide is precipitated. Therefore, the invention can effectively control the size of the intermetallic compound and precipitate the nano-scale carbon compound through precipitation strengthening heat treatment, effectively improve the strength of the material and hardly lose plasticity.
(4) Most metals can be combined with interstitial elements C to form a carbon compound strengthening phase, so that the method is a universal strengthening mode and can be widely applied to strengthening high-entropy alloys prepared by selective laser melting, and the method has great significance and value.
Drawings
FIG. 1 is a diagram of a high-entropy alloy composite material prepared in example 1 of the present invention.
FIG. 2 is a drawing experiment graph of the high-entropy alloy composite material prepared in example 1 of the present invention.
Fig. 3 is a picture of carbon element distribution analysis of the high-entropy alloy composite material prepared in example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention provides a preparation method of a carbon-containing high-entropy alloy composite material, which comprises the following steps:
(1) selecting Fe, Co, Cr and Ni metal simple substances and chromium carbide as raw materials, wherein the atomic ratio of Fe, Cr, Ni, Co and C in the composite material is 1: 1: 1: 1: 0.05, preparing high-entropy pre-alloy powder by adopting an air atomization method; wherein, the alloy element powder does not contain other impurities except a small amount of inevitable impurity oxygen element, and the raw materials do not contain other element components except Fe, Co, Cr, Ni and C; the particle size range of the high-entropy pre-alloy powder is 15-55 mu m, and D50 is controlled to be 45 mu m;
(2) establishing a three-dimensional model of the part on a computer, planning a scanning path of a component, and scanning layer by adopting a checkerboard mode; the deflection angle is 65 degrees when scanning layer by layer;
(3) forming by adopting a selective laser melting process: the scanning laser power is 400W, the scanning speed is 800mm/s, the spot diameter is 90 μm, the scanning interval is 120 μm, and the powder layer thickness is 50 μm;
(4) the adopted inert gas is argon, the equipment adopts a mode of directly introducing argon and combining gas circulation, the oxygen content in the cavity is reduced to 2000ppm, and the pressure in the cavity is 30 mbar;
(5) preheating a substrate at 100 ℃, and spreading a layer of high-entropy prealloy powder with the thickness of 40 mu m on the substrate by manually spreading powder after the substrate is preheated;
(6) after the part is formed, cooling the part in a furnace to room temperature, taking out the part, and performing stress relief annealing: heating to 400 deg.C within 1h, maintaining for 3h, and vacuum degree of 8 × 10
-3Pa, cooling to 100 ℃ along with the furnace, opening the furnace, taking out the parts, and cooling to room temperature in the air.
(7) Carrying out precipitation strengthening heat treatment: and (3) heating to 800 ℃, putting the part into a furnace at a high temperature, preserving the heat for 30min, opening the furnace, taking out the part, and cooling the part to room temperature by high-temperature air to obtain the carbon-containing high-entropy alloy, wherein a physical diagram is shown in figure 1.
The parts prepared by the selective laser melting method have no obvious warping phenomenon on the surface. The part of the embodiment is tested by a drainage method, and the density of the high-entropy alloy composite material is 99.5%; the tensile test engineering curve of the part is shown in FIG. 2, before heat treatment: the yield strength is 638MPa, the tensile strength is 797MPa, and the elongation reaches 13.5%; after heat treatment: the yield strength is 706MPa, the tensile strength is 903MPa, and the elongation is 12.8%.
In this example, the high-entropy alloy composite material prepared by selective laser melting is subjected to atom probe analysis (EPMA), and the photograph is shown in fig. 3 (the left image is the distribution of carbon element, and the right image is the microstructure of the corresponding region). As can be seen from FIG. 3, the high-entropy alloy composite material prepared by the embodiment has the advantages that the carbon element is uniformly dissolved in the matrix in a solid manner, and no obvious carbide segregation exists.
Example 2:
the invention provides a preparation method of a carbon-containing high-entropy alloy composite material, which comprises the following steps:
(1) selecting Fe, Co, Cr and Ni metal simple substances and chromium carbide as raw materials, wherein the atomic ratio of Fe, Cr, Ni, Co and C in the composite material is 1: 1: 1: 1: 0.1, preparing high-entropy pre-alloy powder by adopting an air atomization method; wherein, the alloy element powder does not contain other impurities except a small amount of inevitable impurity oxygen element, and the raw materials do not contain other element components except Fe, Co, Cr, Ni and C; the particle size range of the high-entropy pre-alloy powder is 15-45 mu m, wherein d50 is controlled to be 40 mu m;
(2) establishing a three-dimensional model of the part on a computer, planning a scanning path of a component, and scanning layer by adopting a checkerboard mode; the deflection angle is 70 degrees when scanning layer by layer;
(3) the adopted selective laser melting process comprises the following steps: the scanning laser power is 400W, the scanning speed is 1000mm/s, the spot diameter is 80 μm, the scanning interval is 110 μm, and the powder layer thickness is 40 μm.
(4) The adopted inert gas is argon, the equipment adopts a mode of directly introducing argon and combining gas circulation, the oxygen content in the cavity is reduced to 2000ppm, and the pressure in the cavity is 30 mbar;
(5) preheating a substrate at 100 ℃, and spreading a layer of high-entropy prealloy powder with the thickness of 35 mu m on the substrate by manually spreading powder after the substrate is preheated;
(6) after the part is formed, cooling the part in a furnace to room temperature, taking out the part, and performing stress relief annealing: heating to 450 ℃ within 1h, keeping the temperature for 4h, keeping the vacuum degree at 8 multiplied by 10 < -3 > Pa, cooling to 100 ℃ along with the furnace, opening the furnace, taking out the parts, and cooling to room temperature in the air.
(7) Carrying out precipitation strengthening heat treatment: and (3) heating to 760 ℃, putting the part into a furnace at a high temperature, preserving the heat for 20min, opening the furnace, taking out the part, and cooling the part to room temperature through high-temperature air to obtain the carbon-containing high-entropy alloy.
The parts prepared by the selective laser melting method have no obvious warping phenomenon on the surface. The part of the embodiment is tested by a drainage method, and the density of the high-entropy alloy composite material is 99.3%; before heat treatment: the yield strength is 674MPa, the tensile strength is 832MPa, and the elongation reaches 9.9 percent; after heat treatment: the yield strength was 743MPa, the tensile strength was 916MPa, and the elongation was 9.3%.
Example 3:
the invention provides a preparation method of a carbon-containing high-entropy alloy composite material, which comprises the following steps:
(1) selecting Fe, Co, Cr, Ni and Mn elementary metals and chromium carbide as raw materials, wherein the atomic ratio of Fe, Cr, Ni, Co, Mn and C in the composite material is 1: 1: 1: 1: 1: 0.07, preparing high-entropy pre-alloy powder by adopting an air atomization method; wherein, the alloy element powder does not contain other impurities except a small amount of inevitable impurity oxygen element, and the raw materials do not contain other element components except Fe, Co, Cr, Ni, Mn and C; the particle size range of the high-entropy pre-alloy powder is 15-45 mu m, wherein d50 is controlled to be 35 mu m;
(2) establishing a three-dimensional model of the part on a computer, planning a scanning path of a component, and scanning layer by adopting a checkerboard mode; the deflection angle is 63 degrees when scanning layer by layer;
(3) the adopted selective laser melting process comprises the following steps: the scanning laser power is 350W, the scanning speed is 1200mm/s, the spot diameter is 90 μm, the scanning interval is 100 μm, and the powder layer thickness is 35 μm;
(4) the adopted inert gas is argon, the equipment adopts a mode of directly introducing argon and combining gas circulation, the oxygen content in the cavity is reduced to 2000ppm, and the pressure in the cavity is 30 mbar;
(5) preheating a substrate at 100 ℃, and spreading a layer of high-entropy prealloy powder with the thickness of 35 mu m on the substrate by manually spreading powder after the substrate is preheated;
(6) after the part is formed, cooling the part in a furnace to room temperature, taking out the part, and performing stress relief annealing: heating to 500 ℃ within 1h, keeping the temperature for 3h, keeping the vacuum degree at 9 x 10 < -3 > Pa, cooling to 100 ℃ along with the furnace, opening the furnace, taking out the parts, and cooling to room temperature in the air.
(7) Carrying out precipitation strengthening heat treatment: and (3) heating to 830 ℃, putting the part into a furnace at a high temperature, keeping the temperature for 25min, opening the furnace, taking out the part, and cooling the part to room temperature by air at the high temperature.
The parts prepared by the selective laser melting method have no obvious warping phenomenon on the surface. The density of the high-entropy alloy composite material is 99.6% by testing the parts of the embodiment through a drainage method; the tensile test engineering curve of the part is shown in FIG. 2, before heat treatment: the yield strength is 625MPa, the tensile strength is 786MPa, and the elongation reaches 16.3 percent; after heat treatment: the yield strength is 689MPa, the tensile strength is 891MPa, and the elongation is 16.1%.
Claims (8)
1. The preparation method of the carbon-containing high-entropy alloy composite material is characterized by comprising the following steps of:
(1) preparing high-entropy pre-alloy powder; the high-entropy pre-alloy powder consists of at least four metal elements of Fe, Co, Cr, Ni and Mn and C element; the mol percentage content of carbon atoms in the high-entropy pre-alloy powder is 1-4%;
(2) and carrying out selective laser melting molding on the high-entropy pre-alloy powder, and carrying out subsequent heat treatment on the molded part to obtain the carbon-containing high-entropy alloy.
2. The method according to claim 1, wherein the high-entropy pre-alloyed powder is prepared from elemental metal and metal carbide as raw materials.
3. The method according to claim 2, wherein the metal element is selected from at least four of the elements Fe, Co, Cr, Ni, Mn; the metal carbide is one of chromium carbide, cementite and nickel carbide.
4. The method of claim 1, wherein the heat treatment comprises annealing followed by precipitation strengthening.
5. The method of claim 4, wherein the annealing is performed under conditions of: heating the part to 350-450 ℃ within 1-2 h, preserving the heat for 2-5 h, and keeping the vacuum degree higher than 9 multiplied by 10
-3And cooling to below 100 ℃ along with the furnace under the condition of Pa.
6. The production method according to claim 4, wherein the precipitation hardening conditions are: and heating the part to 800-1000 ℃, preserving the heat for 15-50 min, taking out the part, and cooling the part to room temperature in air.
7. The method of claim 1, wherein the selective laser melting process conditions are: the scanning laser power is 300-400W, the scanning speed is 600-2000 mm/s, the spot diameter is 70-100 μm, the scanning distance is 90-130 μm, and the powder spreading layer thickness is 30-50 μm.
8. The preparation method according to claim 1, comprising the following steps:
(1) taking metal carbide and metal simple substance as raw materials to prepare high-entropy pre-alloy powder;
(2) establishing a three-dimensional model of a part to be prepared on a computer, guiding the three-dimensional model into selective laser melting molding equipment, and setting molding process parameters;
(3) placing the high-entropy pre-alloy powder prepared in the step (1) into a powder supply cylinder in selective laser melting forming equipment, and introducing inert gas into a working cavity to preheat a metal substrate;
(4) and carrying out selective laser melting forming, and annealing and precipitation strengthening on the formed part.
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| CN115533116A (en) * | 2022-09-19 | 2022-12-30 | 华东理工大学 | Multicomponent alloy composite material and preparation method thereof |
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| CN101418394A (en) * | 2007-10-23 | 2009-04-29 | 财团法人工业技术研究院 | Superhard composite material and method for preparation thereof |
| CN103255415A (en) * | 2013-05-08 | 2013-08-21 | 北京工业大学 | TiC-enhanced high-entropy alloy coating and preparation method thereof |
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| CN104308153B (en) * | 2014-10-27 | 2016-08-03 | 西安交通大学 | A kind of manufacture method of high-entropy alloy turbogenerator hot-end component based on precinct laser fusion |
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