CN111763843B - Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy - Google Patents

Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy Download PDF

Info

Publication number
CN111763843B
CN111763843B CN202010859642.2A CN202010859642A CN111763843B CN 111763843 B CN111763843 B CN 111763843B CN 202010859642 A CN202010859642 A CN 202010859642A CN 111763843 B CN111763843 B CN 111763843B
Authority
CN
China
Prior art keywords
powder
copper
specific gravity
tungsten
nickel alloy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010859642.2A
Other languages
Chinese (zh)
Other versions
CN111763843A (en
Inventor
刘东光
张力
罗来马
吴玉程
阮崇飞
朱晓勇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hefei University of Technology
Original Assignee
Hefei University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hefei University of Technology filed Critical Hefei University of Technology
Priority to CN202010859642.2A priority Critical patent/CN111763843B/en
Publication of CN111763843A publication Critical patent/CN111763843A/en
Application granted granted Critical
Publication of CN111763843B publication Critical patent/CN111763843B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum

Abstract

The invention disclosesA preparation method of a multi-element doped high-specific gravity tungsten copper nickel alloy relates to the field of high-specific gravity alloy materials and is provided based on the problems of lower compactness and poor mechanical property of the existing tungsten-based high-specific gravity alloy. The invention comprises the following steps: (1) weighing raw materials of pure tungsten powder, copper powder, nickel powder, yttrium oxide powder, zirconium hydride powder and titanium powder; (2) ball milling raw materials for 18-24 h; (3) and (4) high-temperature calcination. The invention also provides the high-specific gravity tungsten-copper-nickel alloy prepared by the preparation method of the multi-element doped high-specific gravity tungsten-copper-nickel alloy. According to the invention, trace yttrium oxide, zirconium and titanium alloy elements are doped in the alloy to generate solid solution strengthening and promote sintering densification, so that the sintered tungsten-copper-nickel alloy is completely densified, and the density can reach 16.5g/cm at most3Even more than 16.31g/cm3The theoretical density of (a); meanwhile, the microhardness of the alloy can reach 695.93HV to exceed that of common high-specific-gravity tungsten-copper-nickel alloy.

Description

Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy
Technical Field
The invention relates to the field of high-specific gravity alloy materials, in particular to a preparation method of a multi-element doped high-specific gravity tungsten copper nickel alloy and the prepared high-specific gravity tungsten copper nickel alloy.
Background
The high specific gravity tungsten alloy is also called high density tungsten alloy. The alloy is formed by taking tungsten as a matrix (the content is more than 85 percent), adding elements such as copper, nickel, iron and the like as a main binding phase, and adding a small amount of strengthening elements (such as molybdenum, titanium and the like). Tungsten particles whose microstructure is simple substance are bonded by a liquid phase formed by melting of alloy elements. The tungsten particles are a hard and brittle phase, the binding phase is a tough phase, and the high specific gravity tungsten alloy has such components and structure as to determine the excellent comprehensive mechanical properties. Compared with other high-specific gravity materials, the high-specific gravity tungsten alloy has the excellent performances of high strength, high density, small thermal expansion coefficient, good corrosion resistance and oxidation resistance, good electric conduction and heat conduction performance, good ductility and the like. The high-strength high.
However, because tungsten and copper are not mutually soluble, it is difficult to obtain a fully dense and uniform-structure high-specific-gravity tungsten-copper alloy by conventional liquid phase sintering, and thus it is difficult to fully exert the performance advantages of the material. Particularly, the hardness of the material is difficult to improve due to lower sintering compactness and the agglomeration of copper phases. The traditional preparation of tungsten-based high specific gravity alloy is to mix all element powders and adopt liquid phase sintering to reach nearly full density, and the prepared tungsten alloy has large grains (about 30-40 μm) due to large powder particle size (2-4 μm), high sintering temperature and long sintering time. For example, a Mo-W-Ni-Cu alloy sintered in liquid phase can obtain the maximum tensile strength of 1100MPa, but has the highest hardness of 390HV only when the total content of copper and nickel does not exceed 6 percent. The high specific gravity ferrotungsten alloys commonly used in armor-piercing materials require higher hardness and strength, but only when the total amount of ferronickel is 2%, the highest hardness is 310 HV. With the technological progress and the technical development, the performance of the tungsten-copper alloy material with high specific gravity has higher requirements.
The application number is CN201510454364.1 discloses a preparation method of tungsten-copper-nickel alloy powder, carbonyl nickel powder is added into atomized copper powder and crystalline tungsten powder, the atomized copper powder and the crystalline tungsten powder are placed in a steel belt reduction furnace, high-temperature diffusion treatment is carried out in protective gas or reducing atmosphere, the atomized copper powder and the crystalline tungsten powder are enabled to realize alloy connection through diffusion of the carbonyl nickel powder in the atomized copper powder and the crystalline tungsten powder, and the tungsten-copper-nickel alloy powder is obtained through crushing and screening of a crusher. However, it is not easy to improve the material properties of the high specific gravity tungsten copper alloy while maintaining its high density. The mechanical properties of the material can be improved without reducing the higher density of the material only by doping a small amount of various trace elements and improving various processes such as powder making, sintering and the like.
The patent with the application number of CN201811105619.3 discloses a preparation method of a tungsten-based high-specific gravity alloy material, which comprises the following steps of firstly preparing a tungsten-based high-specific gravity alloy material by adopting an intermittent stirring ball mill, wherein the ratio of Co to Ni to Cu to Cr to Fe to 1:1: 1 (0.5-1.5) of a pentabasic amorphous binder phase powder; then mixing the five-membered amorphous bonding phase powder with the W powder; and finally, filling the powder into a die for SPS sintering, and crystallizing the amorphous binding phase by a process of rapid heating and short-time heat preservation to finally prepare the tungsten-based high-specific gravity alloy of which the binding phase is the face-centered cubic structure high-entropy alloy. The problems of the technology are as follows: the prepared tungsten-based high-specific gravity alloy has lower density and poor mechanical property.
Disclosure of Invention
The invention solves the technical problems of lower density and poor mechanical property of the existing tungsten-based high-specific gravity alloy.
The invention adopts the following technical scheme to solve the technical problems:
the invention provides a preparation method of a multi-element doped high-specific gravity tungsten copper nickel alloy, which comprises the following steps:
(1) respectively weighing 88.5-90.5% of pure tungsten powder, 5% of copper powder, 3% of nickel powder, 0.5% of yttrium oxide powder, 0.5-1.5% of zirconium hydride powder and 0.5-1.5% of titanium powder according to weight percentage;
(2) stirring and ball-milling the raw material powder weighed in the step (1), and stirring and ball-milling for 18-24 hours under the argon atmosphere condition according to the ball-to-material ratio of 5:1 to prepare mixed powder;
(3) and (3) high-temperature sintering: putting the mixed powder subjected to ball milling in the step (2) into a graphite mould, putting the mould into a discharge plasma sintering furnace, introducing hydrogen into the furnace chamber, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at a heating rate of 100 ℃/min for 6min, preserving heat for 5min, and pressurizing to 20Mpa during heat preservation; then heating to 1050 ℃ at a heating rate of 100 ℃/min for 4.5min, pressurizing to 70MPa when heating, and keeping the temperature for 10 min; and then the temperature is reduced to room temperature at the cooling rate of 100 ℃/min, and the multielement doped high specific gravity tungsten-copper-nickel alloy is obtained.
According to the invention, trace yttrium oxide, zirconium and titanium alloy elements are doped in the alloy to generate solid solution strengthening and promote sintering densification, so that the sintered tungsten-copper-nickel alloy is completely densified, and the density can reach 16.5g/cm at most3Even more than 16.31g/cm3The theoretical density of (a); meanwhile, zirconium, titanium, copper and nickel have strong formation quaternionThe ability of the alloy glass to undergo martensitic transformation under rapid cooling conditions serves as a second phase reinforcement, which can further increase hardness.
The invention simultaneously applies long-time high-energy ball milling to break the powder and refine the powder particles, thereby ensuring that the particle size of the powder particles is uniform.
Preferably, the purity of the pure tungsten powder is 99.8%, and the particle size is 1.8-2.2 μm.
Preferably, the copper powder has a purity of 99.9% and a particle size of 35 μm.
Preferably, the nickel powder has a purity of 99.9% and a particle size of 30 μm.
Preferably, the yttrium oxide powder has a purity of 99.8% and a particle size of 30 μm.
Preferably, the zirconium hydride powder has a purity of 99.9% and a particle size of 1 μm.
Preferably, the titanium powder has a purity of 99.7% and a particle size of 32.5 μm.
Preferably, the ball milling speed in the step (2) is 500 r/min.
Preferably, the flow rate of hydrogen in the step (3) is 0.15L/min.
The invention also provides the multielement-doped high-specific gravity tungsten-copper-nickel alloy prepared by the preparation method of the multielement-doped high-specific gravity tungsten-copper-nickel alloy.
The invention has the beneficial effects that:
(1) according to the invention, trace yttrium oxide, zirconium and titanium alloy elements are doped in the alloy to generate solid solution strengthening and promote sintering densification, so that the sintered tungsten-copper-nickel alloy is completely densified, and the density can reach 16.5g/cm at most3Even more than 16.31g/cm3The theoretical density of (1) is calculated on the premise that the element components are not dissolved mutually, but the nickel is dissolved in the tungsten phase and the copper phase in the invention, so the real theoretical density is a bit higher than the calculated theoretical density, and the false impression that the density exceeds 1 is caused; meanwhile, zirconium, titanium, copper and nickel have strong capability of forming quaternary alloy glass, and martensite phase transformation occurs under the condition of rapid cooling, and the zirconium, titanium, copper and nickel serve as second phase strengthening, so that the hardness can be further improved.
(2) The multi-element doping does not obviously reduce the density of the tungsten-copper-nickel alloy under the condition of greatly improving the hardness of the alloy, and the aim of improving the mechanical property of the tungsten-copper alloy material on the premise of maintaining higher density is fulfilled.
(3) The invention simultaneously applies long-time high-energy ball milling to break the powder and refine the powder particles, thereby ensuring that the particle size of the powder particles is uniform.
Drawings
FIG. 1 is a powder morphology graph after ball milling.
FIG. 2 is a surface scan of the powder after ball milling;
FIG. 3 is a microscopic surface topography of a multi-element doped high specific gravity tungsten copper nickel alloy under different magnifications;
FIG. 4 is a microscopic view of a multi-element doped high specific gravity tungsten copper nickel alloy fracture at different magnifications;
FIG. 5 is a cross-sectional view of the microstructure of a multi-element doped high specific gravity tungsten copper nickel alloy.
Detailed Description
The invention will be described in further detail below with reference to the drawings and examples of the specification.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
A preparation method of a multi-element doped high-specific gravity tungsten copper nickel alloy comprises the following steps:
(1) according to the weight percentage, 90.5 percent of pure tungsten powder with the purity of 99.8 percent, the granularity of 1.8-2.2 mu m, 5 percent of pure tungsten powder with the purity of 99.9 percent, the granularity of 35 mu m, 3 percent of copper powder with the purity of 99.9 percent, 30 mu m nickel powder, 0.5 percent of purity of 99.8 percent, 30 mu m yttrium oxide powder, 0.5 percent of purity of 99.9 percent, 1 mu m zirconium hydride powder and 0.5 percent of purity of 99.7 percent are respectively weighed, and the granularity of 32.5 mu m titanium powder is respectively weighed;
(2) stirring and ball-milling the raw material powder weighed in the step (1), and ball-milling for 24 hours under the conditions of a ball-material ratio of 5:1 and a rotating speed of 500r/min in an argon atmosphere to prepare mixed powder, wherein the particle size distribution of the powder subjected to high-energy ball milling is uniform, and the powder particles are mellow and easy to sinter and densify as can be seen from figure 1; as can be seen from fig. 2, the distribution of the alloy elements including copper, nickel, zirconium and titanium is such that large particles of each element, which are not agglomerated, are uniformly coated on the surface of the tungsten particles;
(3) and (3) high-temperature sintering: putting the mixed powder subjected to ball milling in the step (2) into a graphite mould, putting the mould into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at a heating rate of 100 ℃/min for 6min, preserving heat for 5min, and pressurizing to 20Mpa during heat preservation; then heating to 1050 ℃ at a heating rate of 100 ℃/min for 4.5min, pressurizing to 70MPa when heating, and keeping the temperature for 10 min; and then the temperature is reduced to room temperature at the cooling rate of 100 ℃/min, and the multielement doped high specific gravity tungsten-copper-nickel alloy is obtained.
(4) Density detection and mechanical property detection: the sintered high specific gravity tungsten copper nickel alloy has consistent grain size, uniform copper phase distribution and 16.74g/cm density3The compactness is 98.04%, the microhardness reaches 447.31HV and exceeds that of the common high-specific gravity tungsten copper nickel alloy, the tensile strength is 338Mpa, and the alloy is not reduced compared with the common high-specific gravity tungsten copper nickel alloy.
Example 2
A preparation method of a multi-element doped high-specific gravity tungsten copper nickel alloy comprises the following steps:
(1) 89.5 percent of pure tungsten powder with the granularity of 1.8-2.2 mu m, 5 percent of pure tungsten powder with the granularity of 99.9 percent, 35 mu m of copper powder, 3 percent of pure nickel powder with the granularity of 99.9 percent, 30 mu m of nickel powder, 0.5 percent of pure yttrium oxide powder with the granularity of 30 mu m, 1.0 percent of pure zirconium hydride powder with the granularity of 1 mu m and 1.0 percent of pure titanium powder with the granularity of 32.5 mu m are respectively weighed according to the weight percentage;
(2) stirring and ball-milling the raw material powder weighed in the step (1), and ball-milling for 20 hours at a ball-to-material ratio of 5:1 and a rotation speed of 500r/min under an argon atmosphere to obtain mixed powder;
(3) and (3) high-temperature sintering: putting the mixed powder subjected to ball milling in the step (2) into a graphite mould, putting the mould into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at a heating rate of 100 ℃/min for 6min, preserving heat for 5min, and pressurizing to 20Mpa during heat preservation; then heating to 1050 ℃ at a heating rate of 100 ℃/min for 4.5min, pressurizing to 70MPa when heating, and keeping the temperature for 10 min; and then the temperature is reduced to room temperature at the cooling rate of 100 ℃/min, and the multielement doped high specific gravity tungsten-copper-nickel alloy is obtained.
(4) Density detection and mechanical property detection: the sintered high specific gravity tungsten copper nickel alloy has consistent grain size and uniform copper phase distribution, and the density reaches 16.21g/cm3The compactness is 97.15 percent, the microhardness reaches 571.4HV and exceeds that of the common high-specific gravity tungsten copper nickel alloy, the tensile strength is 312.5Mpa, and the reduction is not obvious compared with that of the common high-specific gravity tungsten copper nickel alloy; from fig. 3, it can be seen that the microstructure of the multi-element doped high specific gravity tungsten copper nickel alloy is uniform, no larger copper phase agglomeration exists, and the tungsten phase grains are finer and have no larger holes; it can be seen from FIG. 4 that the fracture is along the grain boundary, the grains of the multi-doped high specific gravity W-Cu-Ni alloy are fine and uniform in size, the grains are mostly spherical, and a small amount of Cu is present between the grains as the bonding phase.
Example 3
A preparation method of a multi-element doped high-specific gravity tungsten copper nickel alloy comprises the following steps:
(1) respectively weighing 88.5 percent of pure tungsten powder with the purity of 99.8 percent, the granularity of 1.8-2.2 mu m, 5 percent of pure tungsten powder with the purity of 99.9 percent, the granularity of 35 mu m, 3 percent of copper powder with the purity of 99.9 percent, 30 mu m of nickel powder, 0.5 percent of purity of 99.8 percent, 30 mu m of yttrium oxide powder, 1.5 percent of purity of 99.9 percent, 1 mu m of zirconium hydride powder and 1.5 percent of purity of 99.7 percent, and 32.5 mu m of titanium powder according to weight percentage;
(2) stirring and ball-milling the raw material powder weighed in the step (1), and ball-milling for 18 hours at a ball-to-material ratio of 5:1 and a rotation speed of 500r/min under an argon atmosphere to obtain mixed powder;
(3) and (3) high-temperature sintering: putting the mixed powder subjected to ball milling in the step (2) into a graphite mould, putting the mould into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at a heating rate of 100 ℃/min for 6min, preserving heat for 5min, and pressurizing to 20Mpa during heat preservation; then heating to 1050 ℃ at a heating rate of 100 ℃/min for 4.5min, pressurizing to 70MPa when heating, and keeping the temperature for 10 min; and then the temperature is reduced to room temperature at the cooling rate of 100 ℃/min, and the multielement doped high specific gravity tungsten-copper-nickel alloy is obtained.
(4) Density detection and mechanical property detection: the sintered high specific gravity tungsten copper nickel alloy has consistent grain size and uniform copper phase distribution, and the density reaches 16.50g/cm3The compactness reaches 101.13%, the microhardness reaches 695.93HV far exceeding that of a common high-specific gravity tungsten-copper-nickel alloy, and as can be seen from figure 5, more nickel and titanium are dissolved in the copper phase, so that the hardness of the copper phase is improved, while zirconium is uniformly distributed in the tungsten phase and the copper phase to play a role in solid solution strengthening, so that the overall hardness of the material is finally improved; meanwhile, the tensile strength is 305.7MPa, and compared with the common high-specific gravity tungsten-copper-nickel alloy, the hardness is greatly improved, and the tensile strength is only slightly reduced.
Comparative example 1
The high-hardness multi-element doped high-specific gravity tungsten copper nickel alloy in the comparative example is prepared from tungsten powder, copper powder, nickel powder, yttrium oxide powder, zirconium hydride powder and titanium powder in percentage by weight: 88.5: 5: 3: 0.5: 1.5: and 1.5, ball-milling by a high-energy ball mill, pressurizing and molding the prepared powder, and then putting the powder into a tube furnace for sintering.
The preparation method of the multi-element doped high-specific gravity tungsten copper nickel alloy in the embodiment comprises the following steps:
(1) ball-milling the weighed raw material powder for 18 hours at a ball-to-material ratio of 5:1 and a rotating speed of 500r/min under the argon atmosphere condition to prepare mixed powder;
(2) preparing a sample: putting the mixed powder after ball milling into an alloy steel die, pressurizing to 280Mpa, and maintaining the pressure for 45s to prepare a sample blank;
(3) and (3) sintering: putting the sample blank into a tube furnace, introducing hydrogen into the furnace chamber at a flow rate of 0.15L/min, heating to 1050 ℃ at a heating rate of 10 ℃/min for 103min, and preserving heat for 15 min. Then the temperature is reduced to 500 ℃ at the temperature reduction rate of 5 ℃/min for 110min, and then the temperature is cooled to the room temperature along with the furnace. And obtaining the solid-phase sintered multi-element doped high-specific gravity tungsten-copper-nickel alloy.
(4) Density detection and mechanical property detection: the density of the sintered high-specific gravity tungsten-copper-nickel alloy of the comparative example is 11.4205g/cm3The compactness is 70%, the holes of the microstructure are serious, the copper phase is seriously gathered, the tungsten and the copper are connected unevenly, the microhardness is 147.2HV, and the tensile strength is 122 Mpa.
Comparative example 2
The multi-element doped high-specific gravity tungsten-copper-nickel alloy with high hardness in the comparative example is prepared from tungsten powder, copper powder and nickel powder in percentage by weight of 92: 5: 3, ball milling by a high-energy ball mill, and then sintering by discharge plasma.
The preparation method of the multi-element doped high-specific gravity tungsten copper nickel alloy with high hardness in the embodiment comprises the following steps:
(1) ball-milling the raw materials for 18-24 hours at a ball-to-material ratio of 5:1 and a rotation speed of 500r/min under the condition of argon atmosphere;
(2) and (3) sintering: putting the mixed powder after ball milling into a graphite mould, putting the mould into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at a heating rate of 100 ℃/min for 6min, preserving heat for 5min, and pressurizing to 20Mpa during heat preservation; heating to 1050 deg.C at a heating rate of 100 deg.C/min for 4.5min, slowly pressurizing to 70Mpa, and keeping the temperature for 5-10 min; cooling to room temperature at a cooling rate of 100 ℃/min to obtain the high-hardness multi-element doped high-specific gravity tungsten-copper-nickel alloy;
(4) density detection and mechanical property detection: the sintered high-specific gravity tungsten-copper-nickel alloy of the comparative example has consistent grain size, uniform copper phase distribution and 16.96g/cm density3The compactness is 97.01%, the microhardness reaches 368HV, the tensile strength is 354Mpa, and all data are better than those of solid-phase sintered high-specific-weight tungsten-copper-nickel alloy.
The invention according to example 1-3 compared with the comparative examples 1-2, the invention can be seen in the results that the invention produces solid solution strengthening and promotes sintering densification by doping trace yttrium oxide, zirconium and titanium alloy elements in the alloy, so that the sintered tungsten-copper-nickel alloy is completely densified, and the density can reach 16.5g/cm at most3Even more than 16.31g/cm3The theoretical density of (1) is calculated on the premise that the element components are not dissolved mutually, but the nickel is dissolved in the tungsten phase and the copper phase in the invention, so the real theoretical density is a bit higher than the calculated theoretical density, and the false impression that the density exceeds 1 is caused; meanwhile, zirconium, titanium, copper and nickel have strong capability of forming quaternary alloy glass, martensite phase transformation occurs under the condition of rapid cooling, and the zirconium, titanium, copper and nickel are used as second phase reinforcement to further improve the hardness, and the microhardness can reach 695.93HV to far exceed that of a common high-specific-gravity tungsten-copper-nickel alloy; the density and hardness of the sintered high-specific-gravity tungsten-copper-nickel alloy prepared in the comparative example 1 are poor; the sintered high-specific gravity tungsten-copper-nickel alloy prepared in the comparative example 2 has good density but poor hardness, and the multi-element doping of the invention does not obviously reduce the density of the tungsten-copper-nickel alloy under the condition of greatly improving the hardness of the alloy, thereby completing the purpose of improving the mechanical property of the tungsten-copper alloy material on the premise of maintaining higher density.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and various process schemes having no substantial difference from the concept of the present invention are within the protection scope of the present invention.

Claims (2)

1. The preparation method of the multi-element doped high-specific gravity tungsten copper nickel alloy is characterized by comprising the following steps of:
(1) respectively weighing 89.5% of pure tungsten powder, 5% of copper powder, 3% of nickel powder, 0.5% of yttrium oxide powder, 0.5-1.5% of zirconium hydride powder and 1% of titanium powder according to the weight percentage, wherein the purity of the pure tungsten powder is 99.8%, the granularity is 1.8-2.2 mu m, the purity of the copper powder is 99.9%, the granularity is 35 mu m, the purity of the nickel powder is 99.9%, the granularity is 30 mu m, the purity of the yttrium oxide powder is 99.8%, the granularity is 30 mu m, the purity of the zirconium hydride powder is 99.9%, the granularity is 1 mu m, the purity of the titanium powder is 99.7%, and the granularity is 32.5 mu m;
(2) stirring and ball-milling the raw material powder weighed in the step (1), and stirring and ball-milling for 20 hours under the argon atmosphere condition according to the ball-material ratio of 5:1 and the ball-milling rotation speed of 500r/min to prepare mixed powder;
(3) and (3) high-temperature sintering: putting the mixed powder subjected to ball milling in the step (2) into a graphite mould, putting the mould into a discharge plasma sintering furnace, introducing hydrogen into a furnace chamber, wherein the flow rate of the hydrogen is 0.15L/min, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ at the heating rate of 100 ℃/min for 6min, preserving heat for 5min, and pressurizing to 20MP a during heat preservation; then heating to 1050 ℃ at a heating rate of 100 ℃/min for 4.5min, pressurizing to 70MP a during heating, and keeping the temperature for 10 min; and then the temperature is reduced to room temperature at the cooling rate of 100 ℃/min, and the multielement doped high specific gravity tungsten-copper-nickel alloy is obtained.
2. The multi-element doped high specific gravity tungsten copper nickel alloy prepared by the preparation method of the multi-element doped high specific gravity tungsten copper nickel alloy of claim 1.
CN202010859642.2A 2020-08-24 2020-08-24 Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy Active CN111763843B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010859642.2A CN111763843B (en) 2020-08-24 2020-08-24 Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010859642.2A CN111763843B (en) 2020-08-24 2020-08-24 Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy

Publications (2)

Publication Number Publication Date
CN111763843A CN111763843A (en) 2020-10-13
CN111763843B true CN111763843B (en) 2021-10-26

Family

ID=72729152

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010859642.2A Active CN111763843B (en) 2020-08-24 2020-08-24 Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy

Country Status (1)

Country Link
CN (1) CN111763843B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114635052B (en) * 2020-12-16 2023-08-29 福建工程学院 TiCN-doped wear-resistant tungsten copper composite material and preparation method thereof
CN113718127A (en) * 2021-08-16 2021-11-30 安泰科技股份有限公司 High-performance copper-based solid self-lubricating composite material and preparation method thereof

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RO101337B1 (en) * 1988-01-14 1992-10-20 Electric contacts and production method
JP4249356B2 (en) * 1999-12-28 2009-04-02 株式会社東芝 Electrical contact material
CN103526096B (en) * 2013-10-25 2015-11-18 中国科学院合肥物质科学研究院 Tungsten-zirconium-yttrium oxide Alloy And Preparation Method
CN105177346B (en) * 2015-09-01 2018-02-13 河南科技大学 A kind of tungsten copper contact material and preparation method thereof
CN105238983B (en) * 2015-09-29 2018-04-20 河南科技大学 A kind of rare earth oxide Doped Tungsten copper alloy composite material and preparation method thereof
CN107217995A (en) * 2017-05-05 2017-09-29 胜利油田胜鑫防腐有限责任公司 A kind of tungsten-plated alloy anti-corrosion tubing and casing
CN107513653A (en) * 2017-08-10 2017-12-26 河池桂嘉知识产权服务有限公司 High-specific gravity tungsten alloy ultra thin plate and preparation method thereof
CN108913973B (en) * 2018-08-01 2020-06-26 西安华山钨制品有限公司 Preparation method of tungsten-nickel-copper alloy foil
CN109182871B (en) * 2018-10-24 2020-08-11 中国工程物理研究院材料研究所 Preparation method of fine-grain high-specific-gravity tungsten alloy
CN109852861B (en) * 2019-02-28 2020-07-03 北京工业大学 Low-temperature rapid preparation method of high-density nanocrystalline tungsten-copper-based bulk composite material
CN110315076B (en) * 2019-07-23 2020-06-12 西北有色金属研究院 Forming method of high-specific-gravity tungsten-based alloy based on pre-alloyed powder
CN111057926B (en) * 2019-12-25 2021-10-26 自贡硬质合金有限责任公司 Tungsten alloy and preparation method thereof
CN111230098B (en) * 2020-03-18 2021-07-13 北京大学 Metal-based nano composite powder material, preparation method and application thereof

Also Published As

Publication number Publication date
CN111763843A (en) 2020-10-13

Similar Documents

Publication Publication Date Title
CN108103381B (en) High-strength FeCoNiCrMn high-entropy alloy and preparation method thereof
CN108421985B (en) Method for preparing oxide dispersion strengthening medium-entropy alloy
CN108251695B (en) Preparation method of titanium-aluminum-niobium-zirconium-molybdenum alloy
CN110093548B (en) Ultrafine-grained high-toughness high-entropy alloy containing rare earth Gd and preparation method thereof
CN111763843B (en) Preparation method of multi-element doped high-specific gravity tungsten copper nickel alloy and prepared high-specific gravity tungsten copper nickel alloy
CN111118325B (en) Preparation method of fine-grain niobium-titanium alloy
CN109778042B (en) High-strength tungsten-based alloy and preparation method thereof
CN112680646B (en) Preparation method of TiC-based metal ceramic with high-entropy alloy binder phase
CN111349839B (en) Whisker toughened FCC (fluid catalytic cracking) high-entropy alloy composite material and preparation method thereof
CN111961906B (en) Preparation method of high-strength high-toughness corrosion-resistant nickel-based composite material and obtained product
CN113337746B (en) Preparation method of carbide-reinforced high-entropy alloy composite material
CN101942591A (en) Method for fast preparing molybdenum-copper alloy
CN113122747B (en) Cu- (WC-Y) with excellent mechanical property2O3) Method for preparing composite material
CN110079722A (en) A kind of infusibility high-entropy alloy TiZrNbMoTa and its method for preparing powder metallurgy containing B
CN112647006B (en) Tungsten carbide-based hard alloy and preparation method thereof
CN113549801A (en) Second-phase reinforced high-entropy binder hard alloy and preparation method thereof
CN108277412A (en) A kind of nanometer tungsten based alloy material and preparation method thereof
CN111118379B (en) Co-bonded TiZrNbMoTa refractory high-entropy alloy and preparation method thereof
CN113073274A (en) Novel method for preparing double-phase ultra-fine grain high-entropy alloy
CN110438384B (en) Iron-nickel-based ultrafine-grained hard alloy and preparation method thereof
CN110183231B (en) Preparation method of high-strength high-toughness boron carbide-based ceramic material and ceramic material thereof
CN116555653A (en) K-bubble and nano-oxide composite reinforced W-based material and preparation method thereof
CN113816747A (en) TiC enhanced MAX phase high-entropy ceramic matrix composite material and preparation method thereof
CN110449580B (en) High-strength and high-toughness boron-containing high-entropy alloy material for powder metallurgy and preparation method and application thereof
CN110560697A (en) preparation process for producing cobalt-base alloy powder metallurgy by simple substance ball milling method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant