CN109023013B - Preparation method of corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy - Google Patents
Preparation method of corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy Download PDFInfo
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Abstract
The invention discloses a preparation method of corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy, which is prepared by high-energy ball milling and liquid-phase auxiliary SPS sintering technology. The high-entropy alloy prepared by the invention has the advantages of simple structure, uniform element distribution, no segregation of Cu element, a nano-precipitation/coupling organization structure, excellent corrosion resistance, high strength and toughness and wide industrial application prospect.
Description
Technical Field
The invention relates to a preparation method of corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy, in particular to a method for eliminating Cu macrosegregation in the high-entropy alloy by coupling high-energy ball milling and liquid-phase auxiliary SPS (spark plasma sintering).
Background
In recent years, an alloy breaking the traditional design concept, namely a high-entropy alloy, has attracted extensive attention in the material field, the traditional alloy generally contains one or two main elements to determine the basic performance of the alloy, the basic performance is optimized to a certain degree by adding a small amount of other elements, such as solid solution materials of steel and the like with higher toughness and intermetallic compound materials of titanium-aluminum alloy and the like with higher strength, the high-entropy alloy contains a plurality of main elements, the alloy can still meet the stable state of low free energy at relatively low high temperature by ensuring the lower atomic size difference, valence electron concentration and mixed enthalpy among the main elements and the lower mixed entropy of a system, namely the solid solution state of a plurality of main elements is maintained, when the temperature is as low as T △ S (temperature × entropy change) is difficult to offset △ H (enthalpy change), the alloy has the tendency of phase change, but because the temperature is lower, the certain size difference among the plurality of main elements and the element diffusion are slow, the alloy has the defects of high-dimensional deformation, such as unstable solid solution state or the formation of fine structure precipitation/coupling in the field according to the size of △ H, the alloy is easy to generate the large-induced and has the high-dimensional deformation, the strong-strengthening property of the high-induced crystal lattice, the corrosion-resistant property, the high-induced.
In order to ensure low mixing enthalpy and valence electron concentration difference of the high-entropy alloy, main elements of the high-entropy alloy are concentrated in transition group metals with approximate outermost layer electronic structure characteristics, such as Co, Cr, Fe, Ni, Mo and the like. Elements such as Cu and Ag, which have close atomic sizes to the relevant transition group elements and positive enthalpy of mixing, are added to effectively adsorb elements (such as Al) in the alloy that tend to undergo phase transition. Elements such as Cu and Ag are introduced, so that the stability of an alloy system can be improved, and the obtaining of the controllable high-entropy alloy with a simple structure is promoted; the alloy types of the high-entropy alloy can be increased, and a novel alloy structure is obtained. In the first report of 2004 high-entropy alloy, AlCoCrFeNiCu was the first high-entropy alloy developed by the professor of Yu Yi.
However, because the bonding enthalpy of Cu, Ag and other elements is relatively high (the bonding enthalpy between transition group elements is generally less than 5 kJ/mol, and the bonding enthalpy between Cu, Ag and such elements is generally higher than 10 kJ/mol), Cu element segregation exists in Cu-containing high-entropy alloys obtained by the existing preparation methods (smelting, spraying, hot-pressing and sintering), and the Cu element segregation deteriorates the corrosion resistance and mechanical properties of such high-entropy alloys. The segregation of Cu element can cause large potential difference between tissues, and under a corrosive environment, the Cu-rich area is easy to corrode, thus deteriorating the corrosion resistance of the alloy (D.H. Xiao, P.F. Zhou, W.Q. Wu, et al. Microstructure, mechanical and corrosion bearings of AlCoCuFeNi- (Cr, Ti) high-level corrosion alloys, Materials and Design 116 (2017) 438-447); cu element segregates to form FCC (face centered cubic) phase, which has low strength and reduces the strength of the material (J.M. Zhu, J.L. Meng and J.L.Liang. Microstructure and mechanical properties of Multi-principal component AlCoCrFeNiCux alloy, Rare Metals 35, 5 (2016) 385 389). Therefore, the Cu-containing high-entropy alloy without segregation is developed, the negative effects of the macrosegregation on the corrosion resistance and the mechanical property are inhibited while the positive effect of Cu on the low free energy of an alloy system is ensured, and the Cu-containing high-entropy alloy has very important values on the development of the high-entropy alloy field and the development of the high-performance high-entropy alloy.
Disclosure of Invention
The invention aims to provide a preparation method of corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy.
The method selects AlCoCrFeNi high-entropy alloy powder and Cu powder, promotes the diffusion of the high-entropy alloy and Cu by coupling high-energy ball milling and liquid-phase auxiliary SPS (spark plasma sintering), eliminates the macro segregation of Cu element, and obtains the corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy.
A preparation method of corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy is characterized by comprising the following process steps:
1) high-energy ball milling: respectively weighing Cu powder and AlCoCrFeNi high-entropy alloy powder, and putting the Cu powder and the AlCoCrFeNi high-entropy alloy powder into a WC (tungsten carbide) ball milling tank for ball milling to obtain an original powder product which is uniformly mixed;
2) liquid phase auxiliary SPS sintering, namely, putting the product obtained in the step 1) into a graphite mould, and then putting the graphite mould into an SPS discharge plasma sintering furnace for sintering, wherein the sintering parameter is that the vacuum degree is lower than 5 × 10-3Pa, liquid-phase auxiliary sintering temperature of 1120-1220 ℃, applied pressure of 30-40 MPa, and heat preservation time of 4-8 min, and after sintering, cooling the material to room temperature along with a furnace to obtain the corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy.
The mass percentages of the Cu powder and the AlCoCrFeNi high-entropy alloy powder in the Cu powder and the AlCoCrFeNi high-entropy alloy powder are 10-20% and 80-90% in sequence.
The AlCoCrFeNi high-entropy alloy powder is atomized alloy powder, is spherical and has the granularity of 20-50 mu m; the Cu powder is electrolytic powder and is dendritic, and the granularity is 20-50 mu m.
The ball milling conditions are as follows: and (3) taking WC balls as grinding balls, mixing the balls and the materials at a ball-to-material ratio of 5-10: 1 at a speed of 300-500 r/min for 15-30 h under the protection of argon.
The heating process of the liquid phase auxiliary SPS sintering comprises the following steps: 100oThe temperature of C/min is increased from room temperature to 1050 ℃,30othe C/min is increased from 1050 ℃ to 1120-1220 ℃.
The pressurizing process of the liquid-phase auxiliary SPS sintering comprises the following steps: pressurizing to 10MPa at room temperature, pressurizing to 20MPa at 600 ℃, and pressurizing to 30-40 MPa at 1050 ℃.
The phase composition of the high-entropy alloy is analyzed by X-ray diffraction (XRD), the tissue morphology characteristic of the material is characterized by a Scanning Electron Microscope (SEM), the sample size of a compression strength test is phi 3 mm × 6 mm, the downward moving speed of a pressure head is 0.5 mm/min, the corrosion resistance of the high-entropy alloy is evaluated by an AUTOLAB PGSTAT 302 electrochemical workstation, the corrosion solution is 3.5% NaCl solution, the auxiliary electrode is platinum alloy, and the reference electrode is a calomel electrode of saturated potassium chloride solution.
The corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy prepared by adopting the material composition and the process parameters has the following advantages:
the invention has the characteristics of simple alloy structure, uniform element distribution and elimination of macrosegregation of Cu element.
The invention is characterized in that the alloy keeps the nanometer precipitation/coupling structure of AlCoCrFeNi high-entropy alloy.
The alloy has excellent corrosion resistance, Rt in 3.5% NaCl solution is more than 3 times of that of the as-cast AlCoCrFeNi-Cu high-entropy alloy, and the corrosion resistance is superior to that of 304 stainless steel.
The invention is characterized in that the alloy has higher strength, the room temperature yield strength is not lower than 1150MPa, the fracture strength is not lower than 2400MPa, and the toughness is not lower than 22%.
Drawings
FIG. 1 is the XRD diffraction pattern (a), low power (b) and high power (c) scanning electron microscope structure photographs of the sintered block of the AlCoCrFeNi-Cu (11.18 wt%) high entropy alloy provided in example 1.
FIG. 2 is a scanning image of the Al, Co, Cr, Fe, Ni, Cu composition of the sintered block of AlCoCrFeNi-Cu (11.18 wt%) high entropy alloy provided in example 1.
FIG. 3 is a scanning image of the Al, Co, Cr, Fe, Ni, Cu composition of the sintered block of AlCoCrFeNi-Cu (10 wt%) high entropy alloy provided in example 2.
FIG. 4 is a scanning electron microscope structural photograph (a) and a scanning photograph (b) of Al, Co, Cr, Fe, Ni, Cu composition surface of the sintered block of AlCoCrFeNi-Cu (20 wt%) provided in example 3.
FIG. 5 shows the impedance spectrum (a) and polarization curve (b) of the sintered blocks of AlCoCrFeNi-Cu (11.18 wt%) and AlCoCrFeNi-Cu (20 wt%) high entropy alloys provided in examples 1 and 3, and the high entropy alloys of 304 stainless steel and as-cast AlCoCrFeNi-Cu (11.18 wt%) in 3.5% NaCl solution.
FIG. 6 is a room temperature compressive true stress-strain curve for sintered blocks of AlCoCrFeNi-Cu (11.18 wt%) and AlCoCrFeNi-Cu (20 wt%) high entropy alloys provided in examples 1 and 3.
Detailed Description
Example 1
The AlCoCrFeNi alloy is atomized alloy powder which is spherical and has the granularity less than 30 mu m; the copper is electrolytic powder and is dendritic, and the granularity is 20-50 mu m.
High-energy ball milling: respectively weighing copper powder and AlCoCrFeNi high-entropy alloy powder according to the mass percent of Cu of 11.18% and the balance AlCoCrFeNi high-entropy alloy, putting the copper powder and the AlCoCrFeNi high-entropy alloy powder into a WC ball milling tank, taking a WC ball as a grinding ball with the ball-to-material ratio of 5:1, and then mixing for 15 hours at the speed of 300 r/min under the protection of argon to obtain an original powder product which is uniformly mixed.
Liquid phase auxiliary SPS sintering, the mixed powder is filled into a graphite die and then is placed into an SPS discharge plasma sintering furnace for sintering, the sintering parameter is that the vacuum degree is lower than 5 × 10-3Pa, liquid-phase auxiliary sintering temperature of 1150 ℃, applied pressure of 30MPa, and heat preservation time of 5 min, after sintering, furnace-cooling the material to room temperature to obtain the corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy.
The heating process of the liquid phase auxiliary SPS sintering is 100oC/min is increased from room temperature to 1050 ℃, 30 DEG CoThe C/min is increased from 1050 ℃ to 1150 ℃. The pressurization process of the liquid phase auxiliary SPS sintering is that the SPS sintering is pressurized to 10MPa at room temperature, to 20MPa at 600 ℃ and to 30MPa at 1050 ℃.
The structure of the material is simple BCC (body core)Cubic) phase and a small amount of FCC (face centered cubic) phase, the structure is equiaxial crystal structure, the equiaxial crystal is reticular nanometer precipitation/coupling, all elements are uniformly distributed, and Rt is 27 k omega cm in 3.5 percent NaCl solution2The corrosion current is 1.77 × 10-3mA/cm2The corrosion point is-0.30V, the compressive fracture strength is 2447MPa, and the plasticity is 26.37%.
Example 2
The AlCoCrFeNi alloy is atomized alloy powder which is spherical and has the granularity less than 30 mu m; the copper is electrolytic powder and is dendritic, and the granularity is 20-50 mu m.
High-energy ball milling: respectively weighing copper powder and AlCoCrFeNi high-entropy alloy powder according to the mass percent of Cu of 10% and the balance AlCoCrFeNi high-entropy alloy, putting the copper powder and the AlCoCrFeNi high-entropy alloy powder into a WC ball mill tank, taking WC balls as grinding balls, and mixing for 30 hours under the protection of argon at the speed of 500 r/min to obtain an original powder product which is uniformly mixed.
Liquid phase auxiliary SPS sintering, the mixed powder is filled into a graphite die and then is placed into an SPS discharge plasma sintering furnace for sintering, the sintering parameter is that the vacuum degree is lower than 5 × 10-3Pa, the liquid-phase auxiliary sintering temperature is 1220 ℃, the applied pressure is 40MPa, the heat preservation time is 8 min, and after the sintering is finished, the material is cooled to room temperature along with the furnace to obtain the corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy.
The heating process of the liquid phase auxiliary SPS sintering is 100oC/min is increased from room temperature to 1050 ℃, 30 DEG CoThe C/min is increased from 1050 ℃ to 1220 ℃. The pressurization process of the liquid phase auxiliary SPS sintering is that the SPS sintering is pressurized to 10MPa at room temperature, to 20MPa at 600 ℃ and to 40MPa at 1050 ℃.
The structure of the material is equiaxed crystal structure, the equiaxed crystal is netty nano-precipitation/coupling, and all elements are uniformly distributed.
Example 3
The AlCoCrFeNi alloy is atomized alloy powder which is spherical and has the granularity less than 30 mu m; the copper is electrolytic powder and is dendritic, and the granularity is 20-50 mu m.
High-energy ball milling: respectively weighing Cu powder and AlCoCrFeNi high-entropy alloy powder according to the mass percent of Cu of 20% and the balance AlCoCrFeNi high-entropy alloy, putting the Cu powder and the AlCoCrFeNi high-entropy alloy powder into a WC ball mill tank, taking WC balls as grinding balls with the ball-to-material ratio of 6:1, and then mixing for 20 hours at the speed of 400 r/min under the protection of argon to obtain an original powder product which is uniformly mixed.
Liquid phase auxiliary SPS sintering, the mixed powder is filled into a graphite die and then is placed into an SPS discharge plasma sintering furnace for sintering, the sintering parameter is that the vacuum degree is lower than 5 × 10-3Pa, liquid-phase auxiliary sintering temperature of 1120 ℃, applied pressure of 30MPa, heat preservation time of 4 min, and after sintering, furnace-cooling the material to room temperature to obtain the corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy.
The heating process of the liquid phase auxiliary SPS sintering is 100oC/min is increased from room temperature to 1050 ℃, 30 DEG CoThe temperature of C/min is increased from 1050 ℃ to 1120 ℃. The pressurization process of the liquid phase auxiliary SPS sintering is to pressurize to 10MPa at room temperature, to pressurize to 20MPa at 600 ℃ and to pressurize to 30MPa at 1050 ℃.
The structure of the material is equiaxed crystal structure, the equiaxed crystal is netty nano-precipitation/coupling, all elements are uniformly distributed, and Rt is 25 k omega cm in 3.5 percent NaCl solution2The corrosion current is 2.26 × 10-3mA/cm2The corrosion point is-0.314V, the compressive fracture strength is 2426MPa, and the plasticity is 22.61%.
Claims (4)
1. A preparation method of corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy is characterized by comprising the following process steps:
1) high-energy ball milling: respectively weighing Cu powder and AlCoCrFeNi high-entropy alloy powder, and filling the Cu powder and the AlCoCrFeNi high-entropy alloy powder into a WC ball-milling tank for ball-milling to obtain an original powder product which is uniformly mixed;
2) liquid phase auxiliary SPS sintering, namely, putting the product obtained in the step 1) into a graphite mould, and then putting the graphite mould into an SPS discharge plasma sintering furnace for sintering, wherein the sintering parameter is that the vacuum degree is lower than 5 × 10-3Pa, liquid-phase auxiliary sintering temperature is 1120-1220 ℃, applied pressure is 30-40 MPa, heat preservation time is 4-8 min, and after sintering is finished, the material is cooled to room temperature along with a furnace to obtain corrosion-resistant high-strength AlCoCrFeNi-Cu high-entropy alloy;
conditions of high-energy ball milling: using WC balls as grinding balls, mixing the ball materials at a ball material ratio of 5-10: 1 at a speed of 300-500 r/min for 15-30 h under the protection of argon;
the mass percentages of the Cu powder and the AlCoCrFeNi high-entropy alloy powder in the Cu powder and the AlCoCrFeNi high-entropy alloy powder are 10-20% and 80-90% in sequence.
2. The preparation method according to claim 1, wherein the AlCoCrFeNi high-entropy alloy powder is atomized alloy powder, is spherical, and has a particle size of 20-50 μm; the Cu powder is electrolytic powder and is dendritic, and the granularity is 20-50 mu m.
3. The method of claim 1, wherein the liquid-assisted SPS sintering is performed by a heating process comprising: the temperature is increased from room temperature to 1050 ℃ at a speed of 100 ℃/min, and the temperature is increased from 1050 ℃ to 1120-1220 ℃ at a speed of 30 ℃/min.
4. The method of claim 1, wherein the liquid-assisted SPS sintering is performed by a pressurization process comprising: pressurizing to 10MPa at room temperature, pressurizing to 20MPa at 600 ℃, and pressurizing to 30-40 MPa at 1050 ℃.
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| CN111085685B (en) * | 2019-12-26 | 2021-01-29 | 中国科学院兰州化学物理研究所 | Porous high-entropy alloy material and preparation method and application thereof |
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