CN114540659A - Weak current rare earth modified silver copper-oxide electric contact material and preparation method thereof - Google Patents
Weak current rare earth modified silver copper-oxide electric contact material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a weak current rare earth modified silver copper-oxide electric contact material and a preparation method thereof, the method combines solid solution strengthening and dispersion strengthening technologies, firstly, smelting and atomization are carried out to obtain AgCu rare earth-Me powder, then, oxidation is carried out to obtain silver copper oxide powder, then, hydrogen reduction is carried out to obtain silver copper oxide powder, then, molding, sintering and extrusion are carried out to obtain the silver copper oxide electric contact material generated in situ by oxides, and finally, the silver copper oxide electric contact material with good wear resistance, good arc erosion resistance and good fusion welding resistance is obtained. The material microstructure oxide dispersion part prepared by the invention has combined action with rare earth modification and reinforcement, has better material breaking capacity and stable contact resistance, can improve the quality stability of weak current electric appliances or electronic products, and prolongs the service life of the weak current electric appliances or electronic products.
Description
Technical Field
The invention relates to the technical field of in-situ metal oxide dispersion reinforced electric contact materials, in particular to a weak current rare earth modified silver copper-oxide electric contact material and a preparation method thereof.
Background
Compared with pure Ag metal, the Ag-Cu alloy electric contact material has good wear resistance and arc erosion resistance, is widely applied to electrical and electronic products such as micro switches, relays, automobile commutators, brush pieces, motor rotors and the like, but has the defects that fusion welding is easy to occur when the motor is instantly started, and the reliability and the service life of the electrical and electronic products such as the relays, the automobile commutators, unmanned aerial vehicles and the like are seriously influenced. The addition of metal oxide and rare earth element in Ag-Cu alloy can retain the advantages of good wear resistance and strong arc erosion resistance of Ag-Cu alloy, and can raise the fusion welding resistance of Ag-Cu alloy. Therefore, there is an urgent need for a silver-copper rare earth-oxide electrical contact material having excellent wear resistance, arc erosion resistance, and good fusion welding resistance to meet the increasing demand for high-quality and long-life electronic and electrical products.
Through search, the following results are found:
the invention discloses a Chinese patent with application publication number CN101217226A, which is characterized in that a silver-copper-nickel-magnesium weak current sliding contact material is prepared by adding metal elements such as Ni, Mg, Pd, Zn and the like into AgCu to perform smelting, ingot casting, rolling and annealing, and the contact material is silver alloy, so that fusion welding is easy to occur to a product, and particularly, the starting current is large at the moment of starting a motor, and the failure is easy to occur. Compared with oxides with the same mass fraction, the metal solid solution is strengthened, and the fusion welding resistance of the product is improved.
The invention patent of China with application publication number CN102290261A adopts the modes of atomizing silver-copper alloy, oxidizing, mixing powder, ball milling, molding, sintering, extruding and rolling to prepare the silver-copper-based metal oxide electrical contact material, but in the patent, a high-energy ball milling mode is adopted to mix various powders of silver, copper and oxide. The oxides are added and mixed, the oxides can only be distributed around the powder particles, the alloy particles have no oxides, when the particle size of the oxide powder is less than 1um, the powder mixing ball-milling process is difficult to achieve uniform dispersion, the stability of the performance of the contact product is seriously influenced, and the service life of the electric and electronic product is influenced.
Therefore, it is required to develop a method for preparing an electrical contact material with higher performance to solve the above technical problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a weak current rare earth modified silver copper-oxide electric contact material and a preparation method thereof.
According to one aspect of the invention, a preparation method of a weak current rare earth modified silver copper-oxide electrical contact material is provided, which comprises the following steps: the method comprises the following steps:
putting silver, copper, rare earth elements and additive metal Me into a smelting furnace according to a preset proportion for smelting to obtain molten metal;
atomizing the molten metal to prepare powder to obtain AgCu rare earth-Me alloy powder;
oxidizing the AgCu rare earth-Me alloy powder under high pressure to generate AgCuO-rare earth oxide-MeO powder in situ;
reducing the AgCuO-rare earth oxide-MeO powder to obtain AgCu rare earth-MeO powder;
carrying out cold isostatic pressing treatment on the AgCu rare earth-MeO powder to obtain an AgCu rare earth-MeO spindle;
sintering the AgCu rare earth-MeO spindle to obtain a blank;
and carrying out hot extrusion treatment on the blank to obtain the weak current rare earth modified silver copper-oxide electrical contact material.
Further, in the smelting process of putting the silver, the copper, the rare earth elements and the additive metal Me into a smelting furnace according to a preset proportion, the weight parts of the substances are as follows: 1-5 parts of copper, 0.1-1 part of rare earth element, 0.5-2 parts of additive metal Me0.5, and the balance of silver.
Further, the step of smelting the silver, the copper, the rare earth elements and the additive metal Me in a smelting furnace according to a preset proportion comprises the following steps: the rare earth element is a rare earth element capable of modifying the silver-copper alloy, and the additive metal Me is any one or more of non-rare earth metals of which oxides can be reduced by hydrogen.
Further, the step of smelting the silver, the copper, the rare earth elements and the additive metal Me in a smelting furnace according to a preset proportion comprises the following steps: the smelting temperature is 900-1200 ℃, the smelting time is 15-60 min, and the smelting atmosphere is a vacuum environment or a non-oxygen protective atmosphere.
Further, the atomizing the molten metal into powder comprises: and carrying out high-pressure water atomization on the molten metal to prepare AgCu rare earth-Me alloy powder, drying, and sieving with a 100-mesh and 600-mesh sieve to obtain the AgCu rare earth-Me alloy powder.
Further, the high-pressure oxidation of the AgCu rare earth-Me alloy powder includes: the pressure of oxygen is 0.3-5 Mpa, the temperature is 400-800 ℃, and the time is 1.5-60 h.
Further, the reduction treatment of the AgCuO-rare earth oxide-MeO powder includes: introducing hydrogen to reduce the CuO in the AgCuO-rare earth oxide-MeO powder; wherein the gas of hydrogenThe volume flow rate is 0.3-5 m3The reaction time is 12-60 h, and the temperature is 500-800 ℃.
Further, the sintering the AgCu rare earth-MeO spindle comprises: filling the AgCu rare earth-MeO spindle into a sintering furnace, and filling H2Under the protection of gas, the sintering temperature is 750-950 ℃, the time is 4-60 h, and the gas flow is 0.3-1.5 m3And h, cooling the mixture to room temperature along with the furnace, and discharging the mixture.
Further, the hot extrusion treatment of the blank body comprises the following steps: the heating temperature of hot extrusion is 600-850 ℃, the extrusion ratio is 30-450, the extrusion speed is 1-15 cm/min, and the wire material or the plate material is extruded.
According to another aspect of the invention, the weak current rare earth modified silver copper-oxide electrical contact material is obtained by the preparation method of the weak current rare earth modified silver copper-oxide electrical contact material, the rare earth modified silver copper-oxide electrical contact material has a microstructure that oxide MeO is uniformly dispersed and distributed in a single silver copper alloy particle, and the particle size of the oxide MeO is 1-10 μm.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the weak current rare earth modified silver copper-oxide electric contact material and the preparation method thereof, the combined action of metal solid solution strengthening, oxide dispersion distribution strengthening and rare earth modification is realized by combining an oxidation-reduction process with high-temperature sintering diffusion solid solution treatment, and the complementary advantages of the material can be fully realized by generating a small amount of oxide with high fusion welding resistance in situ, so that the electric contact material has good wear resistance and arc erosion resistance of a silver copper rare earth solution, and the rare earth modified silver copper-oxide electric contact material has better wear resistance, better fusion welding resistance, more stable contact resistance and longer service life, and therefore, the stability of a contact prepared by adopting the process and the service life of a product can be obviously improved.
2. Compared with the powder mixing/grinding direct addition process in the prior art, the process has more uniform tissue, less pollution and more fine and uniform oxide particles, and meanwhile, the more fine and uniform the oxide powder is, the more uniform the distribution is, the better the fusion welding resistance of the material is, and the longer the service life of the final product is reflected.
3. The rare earth modified silver copper-oxide electric contact material prepared by the invention has the advantages of simple processing method, easy mass production, high yield and stable performance, and can greatly reduce the production cost of products.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic flow chart of a method for preparing a weak current rare earth modified silver copper-oxide electrical contact material in an embodiment of the invention;
FIG. 2 is a pressed metallographic structure diagram of an AgCuCe-Zn-Mg alloy powder according to an embodiment of the present invention;
FIG. 3 is a metallographic structure of a ZnO and MgO contact according to an embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the present invention.
The embodiment of the invention provides a preparation method of a weak current rare earth modified silver copper-oxide electric contact material, and with reference to fig. 1, the method comprises the following steps:
s1, putting the silver, the copper, the rare earth elements and the additive metal Me into a smelting furnace according to a preset proportion for smelting to obtain molten metal;
in some specific embodiments, the weight parts of each material are: 1-5 parts of copper, 0.1-1 part of rare earth element, 0.5-2 parts of additive metal Me0.5, and the balance of silver; the rare earth element is a rare earth element capable of modifying the silver-copper alloy, and the additive metal Me is any one or more of non-rare earth metals of which oxides can be reduced by hydrogen. At present, Ag alloy materials are mostly adopted in the field of weak current, and because the requirement on the stability of contact resistance is higher in the field of weak current, the Ag content of the electric contact materials used in the field is relatively higher at home and abroad, and is more than 90 percent, but the alloy states have the defect that fusion welding is easy to occur to lose efficacy. To overcome this drawback, an appropriate oxide and a rare earth element are added to the electric contact material in the present embodiment. Wherein, the copper forms an alloy state with Ag to achieve the aim of realizing solid solution strengthening so as to greatly improve the wear resistance and strength of the material. The rare earth elements have the purpose of regulating and controlling the comprehensive electrical properties of the material, such as prolonging the electrical service life of a product and reducing the arc energy, namely achieving the effect of 'industrial monosodium glutamate', and the processing plasticity of the material is sharply reduced due to too many rare earth elements. The additive metal Me subsequently evolves to an oxide, which can serve the purpose of improving the solder resistance of the material, and if the additive metal Me is added in too large an amount, this can directly lead to unstable contact resistance.
In some specific embodiments, silver, copper, rare earth elements and additive metal Me are smelted in a smelting furnace in proportions that include: the smelting temperature is 900-1200 ℃, the smelting time is 15-60 min, and the smelting atmosphere is a vacuum environment or a non-oxygen protective atmosphere.
In some preferred embodiments, the vacuum environment is a furnace pressure of 10 or less-3Pa, the non-oxygen protective atmosphere, i.e. the reducing atmosphere, is a nitrogen or argon atmosphere.
S2, atomizing the molten metal to prepare powder, and obtaining AgCu rare earth-Me alloy powder;
in some specific embodiments, atomizing molten metal into powder comprises: and carrying out high-pressure water atomization on the molten metal to prepare AgCu rare earth-Me alloy powder, drying, and sieving with a 100-mesh and 600-mesh sieve to obtain the AgCu rare earth-Me alloy powder.
S3, oxidizing AgCu rare earth-Me alloy powder under high pressure, and generating AgCuO-rare earth oxide-MeO powder in situ;
in some specific embodiments, a high pressure oxidized AgCu rare earth-Me alloy powder comprises: the pressure of oxygen is 0.3-5 Mpa, the temperature is 400-800 ℃, and the time is 1.5-60 h.
The in-situ generation of AgCuO rare earth oxide-MeO powder refers to the fact that Cu, rare earth elements and Me are dissolved in an Ag matrix in advance in a smelting mode to form alloy powder particles, and then are oxidized into CuO, rare earth oxides and MeO, and the obtained effect is that the oxide MeO is generated in situ and is uniformly dispersed in single silver-copper alloy powder particles.
S4, reducing the AgCuO-rare earth oxide-MeO powder to obtain AgCu rare earth-MeO powder;
in some specific embodiments, the reduction treatment of the AgCuO-rare earth oxide-MeO powder is a selective reduction treatment comprising: introducing hydrogen to reduce CuO in AgCuO-rare earth oxide-MeO powder, because the rare earth element and the additive metal Me have stronger activity than H when selecting the rare earth element and the additive metal Me, CuO can be reduced by H2Reduction, while rare earth oxides and MeO cannot be substituted by H2Reducing, so that only CuO in AgCuO-rare earth oxide-MeO powder can be reduced through hydrogen reduction treatment; wherein the gas flow of the hydrogen is 0.3-5 m3The reaction time is 12-60 h, and the temperature is 500-800 ℃.
S5, carrying out cold isostatic pressing treatment on the AgCu rare earth-MeO powder to obtain an AgCu rare earth-MeO spindle;
in some specific embodiments, the AgCu rare earth-MeO powder is subjected to cold isostatic pressing, comprising: the pressure intensity of the cold isostatic pressing treatment is 80-350 MPa.
S6, sintering the AgCu rare earth-MeO spindle to obtain a blank;
the step is to carry out high-temperature sintering and diffusion solid solution on the AgCu rare earth-MeO spindle, and then H is introduced2Under high-temperature sintering, Cu and Ag are diffused and further subjected to solid solution to form an AgCu alloy structure, so that the aim of solid solution strengthening is fulfilled. In some specific embodiments, the AgCu rare earth-MeO spindle is sintered, comprising: filling the AgCu rare earth-MeO spindle into a sintering furnace, and filling H2Under the protection of gas, the sintering temperature is 750-950 ℃, the time is 4-60 h, and the gas flow is 0.3-1.5 m3H, then cooling with the furnaceAnd discharging the product from the furnace at room temperature.
S7, carrying out hot extrusion treatment on the blank to obtain the weak current rare earth modified silver copper-oxide electric contact material.
In some specific embodiments, the green body is subjected to a hot extrusion process comprising: and (3) extruding the hot extrusion at a heating temperature of 600-850 ℃, an extrusion ratio of 30-450 and an extrusion speed of 1-15 cm/min into a wire or a plate to obtain the rare earth modified silver-copper electrical contact material with the oxide reinforcing phase uniformly dispersed and distributed.
In some specific embodiments, after the hot extrusion process is performed on the blank, the method further includes: the weak current rare earth modified silver copper-oxide electric contact material is made into an electric contact with a required shape and size, and the electric contact is a metal oxide dispersion reinforced silver copper rare earth contact.
According to the preparation method of the rare earth modified silver copper-oxide electric contact material, oxide MeO is generated in AgCu alloy particles in situ through oxidation, compared with a powder mixing/grinding direct adding process, the process has a more uniform structure and less pollution, and the oxide particles are finer and more uniform, while the powder is mixed/ground. Meanwhile, the more fine and smooth the oxide powder and the more uniform the distribution, the better the final material performance. In addition, because the combined action of oxide dispersion distribution strengthening, metal solid solution strengthening and rare earth modification is realized by combining an oxidation-reduction process with high-temperature sintering diffusion solid solution treatment, the rare earth modified silver copper-oxide electric contact material has better wear resistance, better fusion welding resistance, more stable contact resistance and longer service life, and the stability of the contact prepared by adopting the process and the service life of the product are obviously improved.
In the embodiment of the invention, through the combination of metal solid solution strengthening, oxide dispersion distribution strengthening and rare earth modification, a small amount of oxides with high fusion welding resistance are generated in situ, so that the advantage complementation of the materials is fully realized, the electric contact material not only has good wear resistance and arc erosion resistance of the silver-copper rare earth solution, but also can increase the fusion welding resistance, thereby greatly improving the fusion welding resistance and prolonging the service life of the silver-copper oxide electric contact material.
The method provided by the embodiment of the invention has the advantages of simple processing method, easiness in batch production, high yield and stable performance, and can greatly reduce the production cost of the product.
The embodiment of the invention also provides a weak current rare earth modified silver copper-oxide electrical contact material, which is obtained by adopting the preparation method of the weak current rare earth modified silver copper-oxide electrical contact material in the embodiment, and the rare earth modified silver copper oxide electrical contact material has a microstructure that oxide MeO is uniformly dispersed and distributed in single silver copper alloy particles. The material realizes the in-situ generation of metal oxide and the uniform dispersion distribution of the metal oxide in single powder particles through an oxidation-reduction process, so that the uniform dispersion and high fusion welding resistance of the final electric contact material tissue are ensured, and meanwhile, the rare earth modification is favorable for further improving the wear resistance of the material. The electric contact material produced by the process has excellent wear resistance, arc erosion resistance, good fusion welding resistance, stable contact resistance and longer service life.
Because the particle size range of the oxide MeO is mainly related to the fusion welding resistance, the particle size is too fine, the processing difficulty is higher, but the fusion welding resistance is better; the grain size is too coarse and the processing is easier, but the fusion welding resistance is poor. Thus, in some preferred embodiments, the oxide MeO has a particle size of 1 to 10 μm.
The following will explain in more detail the method for preparing the weak current rare earth modified silver copper-oxide electrical contact material of the present invention using examples and comparative examples. The preparation methods in the following examples were carried out according to the process flow diagram shown in FIG. 1.
Example 1
S1, carrying out intermediate frequency smelting on 5 parts of Cu blocks, 1 part of Ce blocks and 1 part of metal Zn blocks under the protection of an argon atmosphere, wherein the smelting temperature is 1000 ℃, the smelting time is 30min, and the smelting atmosphere is a vacuum environment protective atmosphere.
And S2, after the smelting time is up, carrying out high-pressure water atomization to prepare powder, preparing AgCuCe-Zn alloy powder, drying and sieving with a 200-mesh sieve.
S3, carrying out high-pressure oxidation treatment on the sieved alloy powder at 1Mpa for 40h and at 600 ℃ to obtain AgCuOCeO2-ZnO composite powder.
S4, then carrying out H passing on the powder2Selective reduction with gas flow 3m3And/h, 40 h. Because the active form of H is stronger than Cu and weaker than Ce and Zn, CuO is reduced into Cu and CeO after selective reduction2And ZnO is kept unchanged, and CeO is finally obtained2Rare earth modified AgCu-ZnO powder.
S5, reducing the CeO2And (3) modifying the AgCu-ZnO powder by using rare earth, and carrying out isostatic pressing under the pressure of 150Mpa to obtain the AgCuCe-ZnO spindle.
S6, sintering the ingot at 800 ℃ for 60 hours, and introducing H at high temperature2Sintering, after reduction, Cu is dissolved into Ag matrix again through diffusion to obtain ZnO particle dispersion strengthening, Cu solid solution strengthening and CeO2Rare earth modified AgCu-ZnO spindle.
And S7, extruding the spindle into a wire material, wherein the heating temperature of the extrusion is 700 ℃, the extrusion ratio is 450, and the extrusion speed is 1cm/min, so as to obtain the electrical contact material wire material.
The contact is processed by the electrical contact material wire, the ZnO particle size of the contact is 1-3 um, ZnO is generated by in-situ oxidation and is uniformly dispersed in an AgCu alloy matrix, so that ZnO dispersion enhancement and CeO dispersion enhancement are realized2Rare earth modification and Cu solid solution strengthening.
Example 2
S1, carrying out intermediate frequency smelting on 1 part of Cu block, 0.5 part of La block and 2 parts of metal Mg block under the protection of argon atmosphere, wherein the smelting temperature is 1200 ℃, the smelting time is 15min, and the smelting atmosphere is N2An environmentally protective atmosphere.
And S2, after the smelting time is up, carrying out high-pressure water atomization to prepare powder, preparing AgCuLa-Mg alloy powder, drying and sieving with a 600-mesh sieve.
S3, carrying out high-pressure oxidation treatment on the sieved alloy powder for 0.3Mpa60h, 400 ℃ to obtain AgCuOLa2O3-MgO composite powder.
S4, then carrying out H passing on the powder2Selective reduction with gas flow rate of 0.3m3The temperature is 500 ℃ and the time is 12 h. Because the active form of H is stronger than Cu and weaker than Mg and La, CuO is reduced into Cu and La after selective reduction2O3And MgO are kept unchanged, and La is finally obtained2O3Rare earth modified AgCu-MgO powder.
S5, La after reduction2O3Rare earth modified AgCu-MgO powder is subjected to isostatic pressing at a pressure of 80MPa to obtain La2O3Rare earth modified AgCu-MgO spindle.
S6, sintering the ingot at 750 deg.C for 4H, introducing H at high temperature2Sintering, after reduction, Cu can be dissolved into Ag matrix again through diffusion to obtain MgO particle dispersion strengthening, Cu solid solution strengthening and La2O3Rare earth modified AgCu-MgO spindle.
And S7, extruding the spindle into a wire material, wherein the heating temperature of the extrusion is 850 ℃, the extrusion ratio is 150, and the extrusion speed is 15cm/min, so as to obtain the electrical contact material wire material.
The contact is processed by the electrical contact material wire, the ZnO particle size of the contact is 5-10 um, MgO is generated by in-situ oxidation and is uniformly dispersed in the AgCu alloy matrix, and MgO dispersion enhancement and La dispersion are realized2O3Rare earth modification and Cu solid solution strengthening.
Example 3
S1, carrying out intermediate frequency smelting on 4.2 parts of Cu block, 0.1 part of Y block and 0.5 part of metal Li block under the protection of atmosphere, wherein the smelting temperature is 900 ℃, the smelting time is 60min, and the smelting atmosphere is N2An environmentally protective atmosphere.
And S2, after the smelting time is up, carrying out high-pressure water atomization to prepare powder, preparing AgCuY-Li alloy powder, drying and sieving with a 100-mesh sieve.
S3, carrying out high-pressure oxidation treatment on the sieved alloy powder under the conditions of 5Mpa and 1.5h at 800 ℃ to obtain AgCuOY2O3-Li2O composite powder.
S4, then carrying out H passing on the powder2Selective reduction with gas flow 5m3The temperature is 800 ℃ and the time is 60 hours. Since H is more active than Cu and less active than Y and Li, CuO is reduced to Cu and Y is reduced to Cu after selective reduction2O3And Li2O remains unchanged and Y is finally obtained2O3Rare earth modified AgCu-Li2And (3) O powder.
S5, Y after reduction2O3Rare earth modified AgCu-Li2O powder is subjected to isostatic pressing at a pressure of 350MPa to obtain Y2O3Rare earth modified AgCu-Li2And (4) an O spindle.
S6, sintering the ingot at 950 ℃ for 18H, and introducing H at high temperature2Sintering, after reduction, Cu is dissolved into Ag matrix again through diffusion to obtain Li2O particle dispersion strengthening, Cu solid solution strengthening, Y2O3Rare earth modified AgCu-ZnO spindle.
And S7, extruding the spindle into a plate, wherein the heating temperature of the extrusion is 600 ℃, the extrusion ratio is 30, and the extrusion speed is 15cm/min, so as to obtain the electric contact material plate.
Machining the electric contact material plate into a contact point, wherein the contact point is Li2The particle size of O is 1-8 um, Li2O is generated by in-situ oxidation and is uniformly dispersed in the AgCu alloy matrix, so that Li is realized2O dispersion strengthened, Y2O3Rare earth modification and Cu solid solution strengthening.
Example 4
S1, carrying out medium-frequency smelting on 3 parts of Cu blocks, 0.6 part of Ce blocks, 1 part of metal Zn and 0.5 part of Mg blocks under the protection of argon atmosphere, wherein the smelting temperature is 1050 ℃, the smelting time is 40min, and the smelting atmosphere is a vacuum environment protective atmosphere.
S2, after the smelting time is up, carrying out high-pressure water atomization for milling to prepare AgCuCe-Zn-Mg alloy powder, drying and sieving with a 100-mesh sieve, wherein the pressed metallographic structure of the AgCuCe-Zn-Mg alloy powder is shown in figure 2.
S3, carrying out high-pressure oxidation treatment on the sieved alloy powder for 2MpaAt the temperature of 700 ℃ for 30h to obtain AgCuOCeO2-ZnO-MgO composite powder.
S4, then carrying out H passing on the powder2Selective reduction with gas flow 3m3And/h, 40 h. Since the active form of H is stronger than Cu and weaker than Ce, Zn and Mg, CuO is reduced to Cu and CeO after selective reduction2MgO and ZnO are kept unchanged, and CeO is finally obtained2Rare earth modified AgCu-ZnO-MgO powder.
S5, reducing the CeO2And (3) modifying the AgCu-ZnO-MgO powder by using the rare earth, and carrying out isostatic pressing under the pressure of 180Mpa to obtain the AgCuCe-ZnO spindle.
S6, sintering the ingot at 950 ℃ for 40H, and introducing H at high temperature2Sintering, after reduction, Cu is dissolved in Ag matrix again by diffusion to obtain MgO and ZnO particle dispersion strengthening, Cu solution strengthening and CeO2A rare earth modified AgCu-ZnO-MgO spindle.
And S7, extruding the spindle into a plate, wherein the heating temperature of the extrusion is 750 ℃, the extrusion ratio is 100, and the extrusion speed is 5cm/min, so as to obtain the electric contact material plate.
When the contact material plate is processed into a contact, as shown in a contact metallographic structure shown in fig. 3, compared with fig. 2 and fig. 3, the change condition of the material structure from an AgCuCe-Zn-Mg alloy state to a final state can be seen, the sizes of ZnO and MgO particles of the contact are 4-9 um, ZnO and MgO are generated by in-situ oxidation and are uniformly dispersed and distributed in an AgCu alloy matrix, so that the dispersion strengthening of ZnO and MgO and the dispersion strengthening of CeO are realized2Rare earth modification and Cu solid solution strengthening.
Comparative example
And (3) carrying out intermediate frequency smelting on 5 parts of Cu blocks and 1 part of Ce metal Zn blocks under the protection of an argon atmosphere, wherein the smelting temperature is 1000 ℃, the smelting time is 30min, and the smelting atmosphere is a vacuum environment protective atmosphere.
And after the smelting time is up, carrying out high-pressure water atomization to prepare powder, preparing AgCuCe alloy powder, drying and sieving by a 200-mesh sieve.
And (3) carrying out isostatic pressing on the reduced Ce rare earth modified AgCu powder under the pressure of 150Mpa to obtain the AgCuCe spindle.
Sintering the ingot at 800 deg.C for 60H, and introducing H at high temperature2Sintering, and obtaining the Ce rare earth modified AgCuCe spindle.
And extruding the ingot into a wire material, wherein the heating temperature of the extrusion is 700 ℃, the extrusion ratio is 450, and the extrusion speed is 1cm/min, so as to obtain the wire material of the electrical contact material.
The contact is processed by the electric contact material wire, and the contact Ce is modified by rare earth and is dissolved and strengthened in an AgCu alloy matrix to obtain the AgCuCe contact.
The rare earth oxide modified AgCu-MeO electric contact material samples prepared in the examples 1 to 4 and the pure AgCu rare earth electric contact material prepared in the comparative example were subjected to the evaluation of the running electric life performance and the evaluation of the overall yield, and the detailed results are shown in Table 1.
Comparison of Table 1 shows that examples 1-4 have significant advantages over the comparative examples in terms of operating life performance, particularly the rare earth La in example 22O3The modified AgCuO-MgO electric contact composite material has the best performance; the overall yield is also greatly improved.
TABLE 1. different contact points in model airplane motor converter service life and overall yield data
It can be seen from table 1 that the combination of metal solid solution strengthening, oxide dispersion distribution strengthening and rare earth modification is realized by the technologies of smelting, oxidation-selective reduction, high-temperature sintering solid solution and the like, the complementary advantages of the materials are fully realized by generating a small amount of oxides with high fusion welding resistance in situ, and the high-performance rare earth oxide modified AgCu-MeO electrical contact composite material with high yield and long service life is prepared.
The foregoing description has described specific embodiments of the present invention. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The above-described preferred features may be used in any combination without conflict with each other.
Claims (10)
1. A preparation method of a weak current rare earth modified silver copper-oxide electric contact material is characterized by comprising the following steps:
putting silver, copper, rare earth elements and additive metal Me into a smelting furnace according to a preset proportion for smelting to obtain molten metal;
atomizing the molten metal to prepare powder, and obtaining AgCu rare earth-Me alloy powder;
oxidizing the AgCu rare earth-Me alloy powder under high pressure to generate AgCuO-rare earth oxide-MeO powder in situ;
reducing the AgCuO-rare earth oxide-MeO powder to obtain AgCu rare earth-MeO powder;
carrying out cold isostatic pressing treatment on the AgCu rare earth-MeO powder to obtain an AgCu rare earth-MeO spindle;
sintering the AgCu rare earth-MeO spindle to obtain a blank;
and carrying out hot extrusion treatment on the blank to obtain the weak current rare earth modified silver copper-oxide electrical contact material.
2. The preparation method of the weak current rare earth modified silver copper-oxide electrical contact material as claimed in claim 1, wherein in the process of putting silver, copper, rare earth elements and additive metal Me into a smelting furnace according to a preset proportion for smelting, the weight parts of each substance are as follows: 1-5 parts of copper, 0.1-1 part of rare earth element, 0.5-2 parts of additive metal Me0.5, and the balance of silver.
3. The preparation method of the weak current rare earth modified silver copper-oxide electrical contact material as claimed in claim 1, wherein the step of putting silver, copper, rare earth elements and additive metal Me into a smelting furnace according to a preset proportion for smelting comprises the following steps: the rare earth element is a rare earth element capable of modifying the silver-copper alloy, and the additive metal Me is any one or more of non-rare earth metals of which oxides can be reduced by hydrogen.
4. The preparation method of the weak current rare earth modified silver copper-oxide electrical contact material as claimed in claim 1, wherein the step of putting silver, copper, rare earth elements and additive metal Me into a smelting furnace according to a preset proportion for smelting comprises the following steps: the smelting temperature is 900-1200 ℃, the smelting time is 15-60 min, and the smelting atmosphere is a vacuum environment or a non-oxygen protective atmosphere.
5. The method for preparing the weak current rare earth modified silver copper-oxide electrical contact material according to claim 1, wherein the atomizing the molten metal into powder comprises: and carrying out high-pressure water atomization on the molten metal to prepare AgCu rare earth-Me alloy powder, drying, and sieving with a 100-mesh and 600-mesh sieve to obtain the AgCu rare earth-Me alloy powder.
6. The preparation method of the weak current rare earth modified silver copper-oxide electrical contact material as claimed in claim 1, wherein the high pressure oxidation of the AgCu rare earth-Me alloy powder comprises: the pressure of oxygen is 0.3-5 Mpa, the temperature is 400-800 ℃, and the time is 1.5-60 h.
7. The method for preparing the weak current rare earth modified silver copper-oxide electrical contact material as claimed in claim 1, wherein the reduction treatment of the AgCuO-rare earth oxide-MeO powder comprises: introducing hydrogen to reduce the CuO in the AgCuO-rare earth oxide-MeO powder; wherein the gas flow of the hydrogen is 0.3-5 m3The reaction time is 12-60 h, and the temperature is 500-800 ℃.
8. The method for preparing the weak current rare earth modified silver copper-oxide electrical contact material according to claim 1, wherein the AgCu rare earth-MeO spindle is sintered, and comprises the following steps: filling the AgCu rare earth-MeO spindle into a sintering furnace, and filling H2Under the protection of gas, the sintering temperature is 750-950 ℃, the time is 4-60 h, and the gas flow is 0.3-1.5 m3And h, cooling the mixture to room temperature along with the furnace, and discharging the mixture.
9. The method for preparing the weak current rare earth modified silver copper-oxide electrical contact material according to claim 1, wherein the hot extrusion treatment of the blank comprises: the heating temperature of hot extrusion is 600-850 ℃, the extrusion ratio is 30-450, the extrusion speed is 1-15 cm/min, and the wire material or the plate material is extruded.
10. A weak current rare earth modified silver copper-oxide electrical contact material is characterized by being obtained by the preparation method of the weak current rare earth modified silver copper-oxide electrical contact material as claimed in any one of claims 1 to 9, wherein the rare earth modified silver copper oxide electrical contact material has a microstructure that oxide MeO is uniformly dispersed and distributed on a single silver copper alloy particle, and the particle size of the oxide MeO is 1-10 μm.
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| JPH055139A (en) * | 1991-06-26 | 1993-01-14 | Sumitomo Metal Mining Co Ltd | Production of silver or silver-copper alloy-metal oxide composite material |
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| CN101217074A (en) * | 2008-01-14 | 2008-07-09 | 中希合金有限公司 | A silver tin/copper oxide compound electrical contact and preparation method |
| CN101358305A (en) * | 2005-05-12 | 2009-02-04 | 马渊马达株式会社 | Commutator material and brush material for DC minimotor, clad composite material, and dc minimotor using the same |
| CN111468718A (en) * | 2020-03-07 | 2020-07-31 | 福达合金材料股份有限公司 | Silver copper oxide sheet-shaped electric contact and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH055139A (en) * | 1991-06-26 | 1993-01-14 | Sumitomo Metal Mining Co Ltd | Production of silver or silver-copper alloy-metal oxide composite material |
| US5865980A (en) * | 1997-06-26 | 1999-02-02 | Aluminum Company Of America | Electrolysis with a inert electrode containing a ferrite, copper and silver |
| CN1637158A (en) * | 2003-11-26 | 2005-07-13 | 马渊马达株式会社 | Material for sliding contacts, clad composite material and small-sized DC motor using the same |
| CN101358305A (en) * | 2005-05-12 | 2009-02-04 | 马渊马达株式会社 | Commutator material and brush material for DC minimotor, clad composite material, and dc minimotor using the same |
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