CN115948667A - Tungsten nanoparticle reinforced CuCr alloy and preparation method thereof - Google Patents
Tungsten nanoparticle reinforced CuCr alloy and preparation method thereof Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the technical field of metallurgy, and particularly relates to a tungsten nanoparticle reinforced CuCr alloy and a preparation method thereof 2 O 3 Raw materials, al powder as a reducing agent, caO as a slagging agent and KClO 3 The alloy is taken as a heating agent, and CuCr alloy melt and aluminum oxide-based reduction smelting slag which are mutually soluble at high temperature are obtained through aluminothermic self-propagating; in the process of quenching and tempering refining of alloy melt under the protection of molten slag of high-temperature melt under electromagnetic induction, high-energy ball milling activation pretreatment Mg powder and WO are injected into the high-temperature melt in a stirring and injecting mode 3 The mixture of (2) realizes the dispersion addition of nano W particles through in-situ reduction, and strengthens the performance of the CuCr alloy, wherein the addition amount of the nano W particles is less than 5 percent.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a tungsten nanoparticle reinforced CuCr alloy and a preparation method thereof.
Background
The contact is a part for generating and extinguishing electric arcs in the vacuum arc-extinguishing chamber, and has higher requirements on materials and structures. The following requirements are imposed on the properties of the contact material: 1. high breaking capacity. The material itself is required to have large electrical conductivity, small thermal conductivity, large thermal capacity and low thermionic emission capability. 2. High breakdown voltage. The breakdown voltage is high, the dielectric recovery strength is high, and the arc extinction is facilitated. 3. High resistance to erosion. I.e., withstand the arc ablation and have a low metal evaporation. 4. Resistance to fusion welding. 5. Low cutoff current value. 6. Low gas content. W-Cu electrical contact materials have previously been widely used, but the breaking performance of such materials is poor. Tungsten has a strong electron emission property, so the W-Cu material is generally used only as a vacuum switch with a current less than 10 kA. The CuCr alloy has good electrical and thermal conductivity and is durable, so it is widely used in industrial production. The Cu-Cr alloy has higher strength and hardness after heat treatment, and the electric conduction and fusing resistance are better than those of W-Cu, so that the proportion of the Cu-Cr alloy applied to an electric contact material is gradually increased, but the erosion resistance of the CuCr alloy is inferior to that of the CuW alloy, and the CuCrW contact can combine the advantages of two contact materials of a CuCr contact and a CuW contact.
The preparation process of the CuCrW contact comprises a solid-phase sintering and infiltration method. The solid-phase sintering has the defects of low density, more pores and difficulty in meeting the requirements on hardness; the patent application No. 200910219253.7 is to melt Cr blocks and W blocks in a vacuum furnace; the method comprises the steps of preparing CrW alloy powder through low-temperature powder preparation, preparing a CrW framework through compression molding and sintering, and then infiltrating Cu to prepare a CuCrW composite material. Patent 201410345138.0 discloses a method for preparing immiscible alloy ingots by aluminothermic reduction-slag refining, and provides a method for preparing immiscible alloy ingots by aluminothermic reduction by taking metal oxide powder as a raw material, refining and impurity removal are carried out on the high-temperature melt under the action of an electromagnetic field, a deoxidizer is blown into the melted high-temperature melt, and finally, the homogeneous alloy ingots are obtained by forced water cooling. However, how to realize the preparation of the homogenized ternary CuCrW alloy cast ingot is always a difficulty in the preparation of the copper-based immiscible alloy, and particularly the in-situ addition technology of the nanoparticles of the third component is a bottleneck restricting the preparation and application of the high-homogenization CuCrW alloy.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing a tungsten nanoparticle reinforced CuCr alloy, comprising the steps of:
a. according to the mass ratio of 1:0.58 to 1.75: 0.38-0.81: 0.03 to 0.37:0.08 to 0.17, weighing CuO and Cr 2 O 3 Al powder, KClO 3 Placing the CaO raw material mixture into a mixing tank, placing Mg powder on the surface layer of the mixture, directly igniting the Mg powder by open fire, and initiating an aluminothermic reduction reaction to obtain a high-temperature mutually soluble CuCr alloy melt through aluminothermic self-propagation;
b. quenching and tempering and refining the CuCr alloy melt at the smelting temperature of 1800-1900 ℃ for 5-30 min;
c. blowing Mg powder and WO into high-temperature solution by carrying inert gas 3 The mixed material is subjected to reduction reaction in a high-temperature melt environment; under the stirring action of an electromagnetic field, nano W particles obtained by reduction are dispersed in a copper-chromium alloy melt in situ;
d. and then adding the obtained nano W particles into the copper-chromium alloy melt of the nano tungsten particles in situ, and rapidly solidifying under the water cooling effect to obtain the nano tungsten particle reinforced CuCrW ternary composite material.
Further, in the step a, before the raw materials are weighed, cuO and Cr required by the reaction are added 2 O 3 、KClO 3 、CaO、WO 3 The materials are placed in an oven and dried for 24 hours at the temperature of 150 ℃.
Further, in step a, the mixing bowl is placed on a ball mill for mixing for 40min.
Further, in the step a, the content of Cr in the CuCr alloy is 25wt.% to 50wt.%.
And further, in the step b, carrying out quenching and tempering and refining on the CuCr alloy melt under the protection of molten slag under electromagnetic induction, wherein the electromagnetic induction parameter is 2000-5000HZ.
Furthermore, in the step c, on the basis of the existing CuCr alloy preparation, a nano W reinforced CuCr alloy is added, and the addition amount of nano W particles is less than 5%.
Further, in step c, the Mg powder and WO are mixed before blowing 3 The mixture is subjected to high-energy ball milling activation pretreatment and ball millingThe rotating speed is 250-300rpm, the ball milling time is 20-30min, and after blowing, the in-situ reduction addition and dispersion distribution of the nano W particles are realized under the action of electromagnetic stirring, wherein the W particles are 3-6nm.
Further, mg powder and WO 3 3:1 to 3.5.
On the other hand, the invention also provides a tungsten nanoparticle reinforced CuCr alloy prepared by any one of the methods.
The invention has the following advantages:
a. the cost is saved: the process utilizes the heat generated in the aluminothermic reduction process to obtain the mutually soluble CuCr alloy melt, reduces the energy consumption of the traditional heating melting process, and shortens the process flow.
b. Alloy purification: the uniform high-temperature melt obtained by aluminothermic reduction is directly refined and purified, and the defects of non-metallic inclusions, air holes and the like in the high-temperature melt can be effectively removed.
c. In-situ dispersion of nano W particles in a copper-chromium alloy melt: blowing Mg powder and WO under the stirring action of electromagnetic field 3 The mixed material can ensure that the W particles obtained by reduction are dispersed and distributed in the miscible CuCr alloy melt.
d. Obtaining the segregation-free homogeneous CuCrW ternary composite material: the rapid solidification under the action of electromagnetic field stirring and water cooling can ensure that the three phases of Cu, cr and W are uniformly distributed, thereby ensuring the uniformity, compactness and purity of the material.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the tungsten nanoparticle reinforced CuCr alloy.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, the present invention provides a method for preparing a tungsten nanoparticle reinforced CuCr alloy, comprising the following steps,
a. according to massThe ratio of 1:0.58 to 1.75: 0.38-0.81: 0.03 to 0.37:0.08 to 0.17, weighing CuO and Cr 2 O 3 Al powder, KClO 3 Placing the CaO raw material mixture into a mixing tank, placing Mg powder on the surface layer of the mixture, directly igniting the Mg powder by open fire, and initiating an aluminothermic reduction reaction to obtain a high-temperature mutually soluble CuCr alloy melt through aluminothermic self-propagation; reduces the energy consumption of the traditional heating melting process and shortens the process flow.
b. The CuCr alloy melt is subjected to quenching and tempering and refining of the alloy melt, the uniform high-temperature alloy melt obtained by aluminothermic reduction is directly refined and purified, and the defects of non-metallic inclusions, air holes and the like in the high-temperature alloy melt can be effectively removed. The smelting temperature is 1800-1900 ℃ and the time is 5-30 min; the method can effectively ensure the separation of slag and gold at the smelting temperature, better purify the alloy, and simultaneously ensure that the temperature of the CuCr alloy melt is higher than the melting point, so that the solidified CuCr alloy is homogeneous, thereby ensuring the superiority of the electrical property of the solidified CuCr alloy.
c. Blowing Mg powder and WO into high-temperature solution by carrying inert gas 3 The mixed material of (2) is subjected to a reduction reaction in a high-temperature melt environment; under the stirring action of an electromagnetic field, nano W particles obtained by reduction are dispersed in the copper-chromium alloy melt in situ. In-situ dispersion of nano W particles in a CuCr alloy melt: blowing Mg powder and WO under the stirring action of electromagnetic field 3 The mixed material can ensure that the W particles obtained by reduction are dispersed and distributed in the miscible CuCr alloy melt. The dispersed distribution of W can strengthen the mechanical property of the alloy and simultaneously improve the corrosion resistance and the breakdown property of the alloy as a contact material.
d. And then adding the obtained nano W particles into the copper-chromium alloy melt of the nano tungsten particles in situ, and rapidly solidifying under the water cooling effect to obtain the nano tungsten particle reinforced CuCrW ternary composite material. The rapid solidification under the action of electromagnetic field stirring and water cooling can make Cu, cr and W three phases uniformly distributed, and ensure the uniformity, compactness and purity of the material.
As an improvement of the scheme, in the step a, before the raw materials are weighed, cuO and Cr required by the reaction are added 2 O 3 、KClO 3 、CaO、WO 3 Placing the materials in an oven at 150 deg.CAnd (5) drying the workpiece for 24 hours, so that the moisture in the material is effectively removed, and the safety of the experiment is ensured.
As an improvement of the scheme, in the step a, the mixing tank is placed on the mixing tank to be mixed for 40min, so that all materials are uniformly mixed, and the melt obtained in the reaction process is ensured to be homogeneous, thereby ensuring the stability of the performance of the CuCr alloy.
As an improvement of the scheme, in the step a, the content of Cr in the CuCr alloy is 25wt.% to 50wt.%, and the CuCr alloy with high content of Cr (20-50 wt.%) has become a main contact material of medium-voltage and high-current vacuum arc-extinguishing chambers due to its excellent electrical conductivity, thermal conductivity, high voltage-bearing capacity, low off-current and good arc-erosion resistance.
In the step b, under the protection of slag under electromagnetic induction, the CuCr alloy melt is subjected to quenching and tempering and refining, wherein the electromagnetic induction parameter is 2000-5000HZ. The electromagnetic induction parameters are used for ensuring the stirring strength of the CuCr alloy in the solidification process, inhibiting the segregation phenomenon, refining Cr phase grains and improving the electrical property of the CuCr alloy.
As an improvement of the scheme, in the step c, on the basis of the existing CuCr alloy preparation, the nano W reinforced CuCr alloy is added, the addition amount of nano W particles is less than 5%, W is used as a high-melting-point metal, and the W content exceeding the proportion can aggravate the nucleation and growth of the W particles and worsen the reinforcing effect of the nano W particles.
As a modification of the protocol, in step c, the Mg powder and WO are mixed prior to blowing 3 Subjecting the mixture to high-energy ball milling activation pretreatment to enable WO 3 The particles are fully reduced into nano W particles which are dispersed and distributed in the CuCr alloy melt, the ball milling rotating speed is 250-300rpm, the ball milling time is 20-30min, after the blowing, the in-situ reduction addition and the dispersion distribution of the nano W particles are realized under the action of electromagnetic stirring, and the W particles are 3-6nm.
As an improvement of the protocol, mg powder and WO 3 3:1-3.5, ensuring that WO 3 The byproduct MgO generated while the nano W particles are completely reduced to be nano W particles participates in slagging, and the effect of separating slag from gold is improved.
On the other hand, the invention also provides a tungsten nanoparticle reinforced CuCr alloy prepared by any one of the methods.
The raw materials adopted by the patent are as follows: the purity of the CuO powder is more than or equal to 99.7 percent, and the granularity is as follows: 25 μm, cr 2 O 3 Powder is more than or equal to 99.7%, and granularity is as follows: 24.5 mu m, more than or equal to 99.5 percent of Al powder, the granularity of 0.1-2.5mm, more than or equal to 99.0 percent of Mg powder, the granularity: 85 μm, KClO 3 Not less than 99.6%, particle size: 85 μm, caO powder is more than or equal to 98.0 percent; the purity of the argon is more than or equal to 9.5 percent, and the electromagnetic induction parameter is 2000-5000HZ.
Example 1:
preparing CuO powder and Cr according to the composition of CuCr25W2 alloy ingot to be prepared 2 O 3 Powder, mixing the metal oxide powder and the A1 powder, and then respectively adding a slagging agent CaO and a heating agent KClO 3 CuO and Cr required for reaction 2 O 3 、KClO 3 、CaO、WO 3 And (3) placing the oxidized materials (except Al and Mg) in an oven for 24 hours at 150 ℃.
Mixing the materials with CuO powder and Cr 2 O 3 Powder, A1 powder, KClO 3 And CaO in a mixing ratio of 1:0.58:0.38:0.03:0.08 into a mixing tank, and mixing for 40min on a ball mill. Mixing, putting Mg powder on the surface layer of the material to be reduced in a reactor, directly igniting the Mg powder by open fire to initiate aluminothermic reduction reaction, and respectively obtaining high-temperature melt consisting of alloy melt and alumina-based reduction slag. Smelting alloy slag of the high-temperature melt under the action of an electromagnetic field, wherein the electromagnetic induction parameters are as follows: 2000HZ, the smelting temperature is 1800 ℃, the smelting time is 10min, the upper layer forms reduction slag, and the lower layer forms alloy melt; blowing Mg and WO 3 Reducing the mixture to obtain W accounting for 2% of the total weight of the material, blowing Mg and WO subjected to high-energy ball milling activation pretreatment into melting high Wen Rongti in a bottom blowing mode through argon carrying 3 The ball milling rotation speed of the mixture in the high-energy ball milling activation pretreatment process is 250rpm, and the ball milling time is 20min; the flow of argon is 5L/min when bottom blowing is carried out for powder spraying, after refining and deslagging, the nano tungsten particle reinforced CuCr25W2 ternary composite material with the size is obtained by rapid solidification under the water cooling effect
Based on the technical conditions of GB/T26867-2011 copper-chromium electrical contact, the content of Cr in CuCr25 is 23-27%, and the density is more than or equal to 8.25g/cm 3 The hardness is more than or equal to 70HB, the conductivity is more than or equal to 28MS/m, the Cr content of different parts of the composite material prepared by the process along the radial direction and the longitudinal direction is between 24 and 25 percent, the W particles are uniformly distributed in the CuCr alloy material according to the size of 5 to 6nm, the content is between 1.85 and 2.15 percent, and the density of the composite material is 8.42g/cm 3 The hardness is 91.3HB, the conductivity is 30MS/m, and the homogeneity and the performance of the composite material are superior to those of the national standard.
Example 2: preparing CuO powder and Cr according to the components of CuCr50W1 alloy ingot to be prepared 2 O 3 Powder, WO 3 Powder, al powder, mg powder, caO powder, KClO 3 Powder, cuO by mass: cr (chromium) component 2 O 3 ：Al：KClO 3 : caO =1:1.75:0.81:0.37:0.17, uniformly mixing the raw materials in proportion, and preheating the mixed material for 1 hour at 373K; taking a proper amount of preheated mixture, putting the mixture into a graphite reactor, putting Mg powder on the surface layer of a material to be reduced, directly igniting the Mg powder by open fire to initiate aluminothermic reduction reaction, and respectively obtaining high-temperature melts consisting of an alloy melt and alumina-based reduction slag; carrying out gold slag smelting on the high-temperature melt under the action of an electromagnetic field, wherein the magnetic induction parameters in the smelting process are as follows: 5000HZ, the smelting temperature of 1900 ℃, the smelting time of 15min, the upper layer forming reducing slag and the lower layer forming alloy melt; blowing Mg and WO subjected to high-energy ball milling activation pretreatment into smelted high Wen Rongti in a bottom blowing mode through argon carrying 3 The ball milling speed of the mixture is 300rpm, and the ball milling time is 30min; when powder is sprayed by bottom blowing, the flow of argon is 10L/min, after refining and deslagging, the electromagnetic field is stopped to be applied, and rapid solidification is carried out under the water cooling effect to obtain the size of the CuCr50W1 ternary composite material strengthened by the nano tungsten particles
Based on the technical conditions of GB/T26867-2011 copper-chromium electrical contact, the content of Cr in CuCr50 is 47-52%, and the density is more than or equal to 7.9g/cm 3 The hardness is more than or equal to 80HB, the conductivity is more than or equal to 16MS/m, and the composite material prepared by the process has different parts along the radial direction and the longitudinal directionThe Cr content of the CuCr alloy is 48-50 percent, the W particles are uniformly distributed in the CuCr alloy material with the size of 3-4nm, the content of the CuCr alloy material is 0.95-1.05 percent, and the density is 7.96g/cm 3 Hardness of 105HB and conductivity of 20.1MS/m, and the homogeneity and performance of the material are all superior to the national standard. .
Example 3: preparing CuO powder and Cr according to the components of CuCr35W1 alloy ingot to be prepared 2 O 3 Powder, WO 3 Powder, al powder, mg powder, caO powder, KClO 3 Powder, cuO by mass: cr 2 O 3 ：Al：KClO 3 : caO =1:0.94:0.52:0.15:0.11, uniformly mixing the raw materials in proportion, and preheating the mixed material for 1h at 373K; putting a proper amount of preheated mixture into a graphite reactor, putting Mg powder on the surface layer of a material to be reduced, directly igniting the Mg powder by open fire to initiate aluminothermic reduction reaction, and respectively obtaining high-temperature melts consisting of an alloy melt and alumina-based reduction slag; carrying out gold slag smelting on the high-temperature melt under the action of an electromagnetic field, wherein the magnetic induction parameters in the smelting process are as follows: 4000HZ, the smelting temperature is 1850 ℃, the smelting time is 12min, the upper layer forms reduction slag, and the lower layer forms alloy melt; adopting a bottom blowing mode, blowing Mg and WO subjected to high-energy ball milling activation pretreatment into high-smelting Wen Rongti carried by argon 3 The ball milling speed of the mixture is 270rpm, and the ball milling time is 25min; when powder spraying is carried out by bottom blowing, the flow of argon is 7L/min, refining and deslagging are carried out, the electromagnetic field is stopped to be applied, and rapid solidification is carried out under the water cooling effect to obtain the size of the CuCr35W1 ternary composite material reinforced by the nano tungsten particles
Based on the technical conditions of GB/T26867-2011 copper-chromium electrical contact, the content of Cr in CuCr35 is between 32 and 37 percent, and the density is more than or equal to 8.06g/cm 3 The hardness is more than or equal to 75HB, the conductivity is more than or equal to 22MS/m, the Cr content of different parts of the composite material prepared by the process along the radial direction and the longitudinal direction is 34-36 percent, the W particles are uniformly distributed in the CuCr alloy material with the size of 4-5nm, the content is 0.98-1.02 percent, and the density is 8.26g/cm 3 Hardness is 95HB, conductivity is 25MS/m, and homogeneity and performance of the material are superior to national standards. .
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of tungsten nanoparticle reinforced CuCr alloy is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
a. according to the mass ratio of 1:0.58 to 1.75:0.38 to 0.81:0.03 to 0.37:0.08 to 0.17, weighing CuO and Cr 2 O 3 Al powder, KClO 3 Placing the CaO raw material mixture into a mixing tank, placing Mg powder on the surface layer of the mixture, and igniting the Mg powder to obtain a CuCr alloy melt with high temperature intersolubility;
b. quenching and tempering and refining the CuCr alloy melt at the smelting temperature of 1800-1900 ℃ for 5-30 min;
c. blowing Mg powder and WO into high-temperature solution by carrying inert gas 3 The mixed materials of (1); under the stirring action of an electromagnetic field, nano W particles obtained by reduction are dispersed in a copper-chromium alloy melt in situ;
d. and then adding the obtained nano W particles into a copper-chromium alloy melt of the nano tungsten particles in situ, and rapidly solidifying under the water cooling effect to obtain the nano tungsten particle reinforced CuCrW ternary composite material.
2. The method of claim 1, wherein the tungsten nanoparticle reinforced CuCr alloy comprises: in the step a, before raw materials are weighed, cuO and Cr required by the reaction are added 2 O 3 、KClO 3 、CaO、WO 3 The materials are placed in an oven and dried for 24 hours at the temperature of 150 ℃.
3. The method of claim 1, wherein the tungsten nanoparticle reinforced CuCr alloy comprises: in step a, the mixing tank is placed on a ball mill for mixing for 40min.
4. The method of claim 1, wherein the tungsten nanoparticle reinforced CuCr alloy comprises: in the step a, the content of Cr in the CuCr alloy is 25-50 wt.%.
5. The method of claim 1, wherein the tungsten nanoparticle reinforced CuCr alloy comprises: and b, carrying out quenching and tempering and refining on the CuCr alloy melt under the protection of molten slag under electromagnetic induction, wherein the electromagnetic induction parameter is 2000-5000HZ.
6. The method of claim 1, wherein the tungsten nanoparticle reinforced CuCr alloy comprises: in the step c, on the basis of the existing CuCr alloy preparation, a nano W reinforced CuCr alloy is added, and the addition amount of nano W particles is less than 5%.
7. The method of claim 1, wherein the tungsten nanoparticle reinforced CuCr alloy comprises: in step c, the Mg powder and WO are mixed before blowing 3 The mixture is subjected to high-energy ball milling activation pretreatment, the ball milling rotation speed is 250-300rpm, the ball milling time is 20-30min, and after blowing, in-situ reduction addition and dispersion distribution of nano W particles are realized under the action of electromagnetic stirring, wherein the W particles are 3-6nm.
8. The method of claim 1, wherein the tungsten nanoparticle reinforced CuCr alloy comprises: mg powder and WO 3 3:1 to 3.5 in terms of the molar ratio of (1).
9. A tungsten nanoparticle reinforced CuCr alloy is characterized in that: prepared by the method of any one of the above claims 1-8.
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