CN116005020B - Preparation method of CuTe contact material for high-voltage direct-current contactor - Google Patents

Preparation method of CuTe contact material for high-voltage direct-current contactor Download PDF

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CN116005020B
CN116005020B CN202211677174.2A CN202211677174A CN116005020B CN 116005020 B CN116005020 B CN 116005020B CN 202211677174 A CN202211677174 A CN 202211677174A CN 116005020 B CN116005020 B CN 116005020B
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powder
cute
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contact material
current contactor
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CN116005020A (en
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杨晓青
王小军
李鹏
师晓云
张石松
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Shaanxi Sirui Advanced Materials Co Ltd
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Abstract

The invention discloses a preparation method of a CuTe contact material for a high-voltage direct-current contactor, which mainly comprises the following steps: s1, primary batching; s2, vacuum induction melting; s3, secondary feeding; s4, atomizing and pulverizing; s5, screening; s6, secondary batching; s7, mixing materials; s8, pressing; s9, sintering; s10, re-pressing. Compared with the common casting process, the method for manufacturing the mixed powder contact has the advantages that the process is simple, the cost is low, the components are easy to control, and the powder sintering method used by the method is a solid-phase sintering process, so that the manufactured contact has relatively low density and low bonding strength among particles, and therefore, the contact manufactured by the method has relatively high fusion welding resistance compared with the contact manufactured by the common casting method.

Description

Preparation method of CuTe contact material for high-voltage direct-current contactor
Technical Field
The invention relates to the technical field of alloy contact preparation, in particular to a preparation method of a CuTe contact material for a high-voltage direct-current contactor.
Background
In a switching device, an electrical contact directly bears the functions of breaking and switching on a circuit and bearing normal working current or overload current in a certain time, and key functions of various devices, such as the on-off capability of a power distribution device, the electrical service life of a control device and the reliability of a relay depend on the working performance and quality of the contact. Meanwhile, the contact is the weakest link and easy-to-fail part in the switching device: once the contact system fails to function properly, such as a short circuit in the power system, the high voltage circuit breaker contacts refuse to open, which can have very serious consequences.
Along with the rapid development of new energy fields such as new energy automobiles, charging piles, solar energy, wind energy, electric storage systems, industrial automation and the like, the demand for the direct current contactor is continuously increased, and in addition, the grade of the direct current contactor is gradually developed to high voltage and high current. The contact material is used as the core component of the direct current contactor, and the performance of the contact material directly determines the functions of the direct current contactor such as high voltage resistance, load resistance, impact resistance, arc extinguishing capability, breaking capability and the like.
The contact material of the traditional low-voltage contactor is made of pure copper, but with the increase of voltage level and breaking current, the breaking capacity and ablation resistance of pure copper can not meet the requirements gradually, and the use of the dispersed copper contact material existing in the market is severely restricted by higher price and poor weldability, so that the development requirement of the direct-current contactor is met by the contact material with low cost performance. There is therefore a need for a method of preparing CuTe contact materials for use in high voltage dc contactors.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a CuTe contact material for a high-voltage direct-current contactor.
The technical scheme of the invention is as follows: a preparation method of a CuTe contact material for a high-voltage direct-current contactor mainly comprises the following steps:
s1, primary batching:
the Cu is as follows by weight percent: 98.5-99.7%, and the balance Te, preparing and batching raw materials, wherein Cu in the raw materials adopts anaerobic Cu;
s2, vacuum induction melting:
loading the Cu block into a crucible, putting the Te block into a secondary feeding device, carrying out vacuum induction smelting treatment on the Cu block, and simultaneously preheating a tundish;
s3, secondary feeding:
adding Te blocks through a secondary feeding device until the Cu melt is completely melted, uniformly stirring the Cu melt and the Te melt, and keeping for 3-5 min;
s4, atomizing and pulverizing:
filling inert gas into a vacuum smelting system, and atomizing when the CuTe alloy melt is completely mixed and uniformly mixed and the temperature of a tundish reaches 1083 ℃;
s5, screening:
screening the atomized powder by adopting powder selecting equipment;
s6, secondary batching:
mixing the atomized copper tellurium powder and the electrolytic copper powder according to the weight percentage, wherein the copper tellurium powder accounts for 50-100%, and the balance is the electrolytic copper powder;
s7, mixing materials
Mixing the atomized copper tellurium powder and the electrolytic copper powder weighed in the step S6 in a double-roll spiral mixer, wherein the stirring speed is 30-60 r/min, and the stirring time is 2-7 h;
s8, pressing
Filling the mixed powder into a forming die, and placing the powder into a dry powder automatic forming hydraulic press at a speed of 2.7-4.1 t/cm 3 Is pressed into a blank by the pressing pressure of the roller;
s9, sintering
Placing the pressed blank into a vacuum sintering furnace, and vacuum-sintering at a vacuum degree of 1×10 -3 ~1×10 -1 Sintering under Pa condition, wherein the sintering mode adopts a gradient heating and heat preservation mode, the highest heating temperature is controlled between 800 ℃ and 1050 ℃, and the heat preservation time is 2 hours;
s10, back pressure
Placing the sintered material into a shaping die, compacting the sintered material on a dry powder automatic forming hydraulic press, and according to the pressure-bearing area of the product, obtaining a compact with a pressure-bearing area of 8-12 t/cm 3 Pressing to compact the product to a final density of 8.9g/cm 3 The above.
Description: according to the method, the oxygen-free copper rod and the tellurium block are mixed through vacuum induction smelting, copper tellurium alloy powder is prepared through an atomization method, and then a powder metallurgy method is adopted to prepare the copper tellurium alloy contact. Since the powder sintering process is a solid phase sintering process, contacts are produced having a relatively low density and low bond strength between particles, and thus contacts produced by this process have a relatively high resistance to fusion welding.
Further, the atomization method in step S4 includes water atomization and air atomization.
Description: the copper tellurium alloy powder is prepared by combining water atomization and gas atomization, so that the time required for pulverizing is shortened, the problem that part of alloy is not atomized in the water atomization or gas atomization process is avoided, and the pulverizing rate is increased.
Further, in the step S4, the water atomization pressure is 1500bar, the nozzle adopts a circular seam nozzle, and the water flow is 5m 3 And/ks, adopting 3-6 mm of eye leakage.
Description: through the arrangement, the water mist is sprayed out by the circular seam nozzle, and the copper tellurium alloy melt is carried out by the fine water mist to form copper tellurium alloy powder.
Further, in the step S4, a tightly coupled nozzle is used for the gas atomization treatment, the size of a leakage hole is 3-6 mm, the pressure of atomization gas is 2-8 Mpa, and inert gas is high-purity argon.
Description: according to the arrangement, the inert gas is sprayed out at high pressure by the tightly coupled nozzle to shear the copper tellurium alloy melt to form copper tellurium alloy powder, and the high-purity argon is selected as the inert gas for gas atomization because the high-purity argon has stable chemical property and the characteristics of no combustion and no combustion supporting.
Further, the powder selecting device in the step S5 adopts a 200-mesh sieve.
Description: by the arrangement, the copper tellurium alloy powder with the mesh of-200 can be screened out for subsequent use.
Further, in the step S6, the granularity of the electrolytic copper powder is-200 meshes, the purity is more than or equal to 99.7 percent, and the oxygen content is less than or equal to 700ppm.
Description: the electrolytic copper powder with the mesh of-200 is selected to be conveniently mixed with copper tellurium alloy powder with the mesh of-200.
Further, in the step S8, the outer contour size of the molding area of the molding die is 0.5-0.7 mm smaller than the outer diameter size of the product, and the inner hole and the inner step size are 0.5-0.7 mm larger than the product size.
Description: through the arrangement, the problem that the internal stress of the pressed blank is released in the subsequent sintering process, so that the product is expanded and deformed can be prevented.
Further, the thickness of the blank is pressed in the step S8 according to ρ 2 *V 2 /(ρ 1 *S 1 ) Calculating, wherein ρ 2 V for final density of product 2 For the final volume of the product ρ 1 Is the initial press density of the product, S 1 Is the initial pressure area of the product.
Description: the thickness of the blank prepared by mixing and pressing copper tellurium alloy powder and electrolytic copper powder can be calculated through the formula.
Further, in step S9, the gradient heating and heat preservation method is as follows: heating to 300 ℃ from room temperature and preserving heat for 2 hours, heating to 500 ℃ from 300 ℃ and preserving heat for 2 hours, heating to 3 hours, heating to 800-1050 ℃ from 500 ℃ and preserving heat for 3 hours, heating to 2-5 hours, closing heating, cooling to 60 ℃ along with furnace, and discharging.
Description: by utilizing a gradient heating mode in the sintering process, the problems that the temperature is excessively fast in the sintering process and a blank in the sintering process is likely to crack are avoided, the continuity of the subsequent process is ensured, and the waste of materials is avoided.
Further, the outside diameter and the inner hole of the shaping die in S10 are the same as the product in size.
Description: by the arrangement, the sintered material can be subjected to a re-pressing process to reach the required size.
The beneficial effects of the invention are as follows:
(1) According to the invention, the copper tellurium contact material is prepared by using a powder mixing process, the tellurium copper alloy material has good free cutting property and excellent electric and heat conduction properties, and simultaneously has corrosion resistance and electric ablation resistance, and good cold and hot processing property, and can be forged, cast, extruded, drawn and stamped, and the performance and price of the copper tellurium contact material are applied to the existing direct current contactor to take advantage.
(2) Compared with the conventional casting process, the method for manufacturing the powder mixing contact has the advantages of simple process, low cost and easy control of components.
(3) The powder sintering method used in the invention is a solid phase sintering process, and the prepared contact has relatively low density and low bonding strength among particles, so that the contact manufactured by the method provided by the invention has relatively high fusion welding resistance compared with the contact manufactured by a common fusion casting method.
Detailed Description
The invention will be described in further detail with reference to the following embodiments to better embody the advantages of the invention.
Example 1
A preparation method of a CuTe contact material for a high-voltage direct-current contactor mainly comprises the following steps:
s1, primary batching:
the Cu is as follows by weight percent: 98.5 percent and the balance Te, preparing and batching raw materials, wherein the Cu in the raw materials adopts anaerobic Cu;
s2, vacuum induction melting:
loading the Cu block into a crucible, putting the Te block into a secondary feeding device, carrying out vacuum induction smelting treatment on the Cu block, and simultaneously preheating a tundish;
s3, secondary feeding:
adding Te blocks through a secondary feeding device until the Cu melt is completely melted, uniformly stirring the Cu melt and the Te melt, and keeping for 5min;
s4, atomizing and pulverizing:
filling high-purity argon into a vacuum smelting system, and performing water atomization and gas atomization treatment when the CuTe alloy melt is completely mixed and uniformly mixed and the temperature of a tundish reaches 1083 ℃, wherein the water atomization pressure is 1500bar, a circular seam nozzle is adopted as a nozzle, and the water flow is 5m 3 The gas atomization treatment adopts a tightly coupled nozzle, the size of the leakage hole is 5mm, and the atomization pressure is 6Mpa;
s5, screening:
sieving the atomized powder by adopting a 200-mesh sieve;
s6, secondary batching:
mixing the atomized copper tellurium powder and the electrolytic copper powder according to the weight percentage, wherein the copper tellurium powder accounts for 50 percent, and the balance is the electrolytic copper powder, the granularity of the electrolytic copper powder is-200 meshes, the purity is 99.9 percent, and the oxygen content is 600ppm;
s7, mixing materials
Mixing the atomized copper tellurium powder and the electrolytic copper powder weighed in the step S6 in a double-roll spiral mixer, wherein the stirring speed is 60r/min, and the stirring time is 7h;
s8, pressing
Filling the mixed powder into a forming die, and placing the powder into a dry powder automatic forming hydraulic press at a speed of 4.1t/cm 3 The outer contour size of the molding area of the molding die is 0.5mm smaller than the outer diameter size of the product, the inner hole and the inner step size are 0.5mm larger than the product size, and the thickness of the pressed blank is according to ρ 2 *V 2 /(ρ 1 *S 1 ) Calculating, wherein ρ 2 V for final density of product 2 For the final volume of the product ρ 1 Is the initial press density of the product, S 1 Is the initial pressure area of the product;
s9, sintering
Placing the pressed blank into a vacuum sintering furnace, and vacuum-sintering at a vacuum of 1×10 -3 ×10 -1 Sintering under Pa, heating to 300 deg.C from room temperature and keeping the temperature for 2h, heating to 500 deg.C from 300 deg.C and keeping the temperature for 2h, heatingThe time is 3 hours, then the temperature is raised to 1050 ℃ from 500 ℃ and kept for 3 hours, then the heating is closed, the furnace is cooled to 60 ℃ and the furnace is taken out;
s10, back pressure
Placing the sintered material into a shaping die, and compacting the sintered material on a dry powder automatic molding hydraulic press, wherein the outer diameter, inner hole and inner step of the shaping die are the same as the product in size, and the pressure-bearing area of the product is 12t/cm 3 Pressing to obtain a final density of 11.6g/cm 3
Example 2
This example is substantially identical to example 1, except that in step S1, cu:99%, the remainder being Te.
Example 3
This example is substantially identical to example 1, except that in step S1, cu:99.7%, the remainder being Te.
Example 4
This example is basically the same as example 1, except that in step S3, the Cu melt and the Te melt are stirred uniformly and kept for 3min.
Example 5
This example is basically the same as example 1, except that in step S3, the Cu melt and the Te melt are stirred uniformly and kept for 4 minutes.
Example 6
The present example is substantially the same as example 1, except that in step S6, the copper tellurium powder is 80% by weight, and the balance is the electrolytic copper powder.
Example 7
The embodiment is basically the same as the embodiment 1, except that in the step S6, the copper tellurium powder accounts for 100% according to the weight percentage.
Example 8
This example is substantially the same as example 1, except that in step S7, the stirring speed was 30r/min and the stirring time was 2 hours.
Example 9
This example is substantially the same as example 1, except that in step S7, the stirring speed was 45/min and the stirring time was 4.5 hours.
Example 10
The present example is substantially the same as example 1 except that in step S8, the mixed powder is charged into a molding die and is fed to a dry powder automatic molding hydraulic press at a speed of 3.4t/cm 3 Is pressed into a compact by the pressing pressure of the die.
Example 11
This example is essentially the same as example 1 except that in step S8, the blended powder is charged into a forming die and is fed to a dry powder automatic forming hydraulic press at a speed of 2.7t/cm 3 Is pressed into a compact by the pressing pressure of the die.
Example 12
This example is substantially the same as example 1, except that in step S9, the temperature is raised from 500℃to 900℃and kept for 3 hours.
Example 13
This example is substantially the same as example 1, except that in step S9, the temperature is raised from 500℃to 800℃and maintained for 3 hours.
Example 14
The present embodiment is substantially the same as that of example 1 except that in step S10, the pressure area of the product is 10t/cm 3 Pressing to obtain a final density of 9.7g/cm 3
Example 15
The present example is substantially the same as example 1 except that in step S10, the pressure area of the product is 8t/cm 3 Pressing to obtain a final density of 8.9g/cm 3
Experimental example
1. The influence of different Cu and Te contents on the tensile strength and hardness of the contact is explored
TABLE 1 influence of different Cu and Te contents on tensile Strength and hardness of contacts in examples 1 to 3
Conclusion: as can be seen from the data in table 1, the different Cu and Te contents have a certain influence on the tensile strength and density of the contact, and the higher the Te content in the contact material, the higher the tensile strength and density of the contact, and thus the method for manufacturing the CuTe contact in example 1 is the optimal method.
2. The influence of the stirring time on the mixing degree of the Cu melt and the Te melt was examined
TABLE 2 influence of stirring time on the degree of mixing of Cu and Te melts in examples 1, 4 and 5
Conclusion: from the data in Table 2, it is found that the stirring time has a certain influence on the degree of mixing of the Cu melt and the Te melt, and that the longer the stirring time is, the higher the degree of mixing of the Cu melt and the Te melt is, whereby the method of example 1 is the optimum method.
3. Investigation of the influence of the ratio of electrolytic copper powder on the conductivity of the contact
TABLE 3 influence of the ratio of electrolytic copper powder on the conductivity of contacts in examples 1, 6 and 7
Conclusion: from the data in Table 3, it is found that the ratio of electrolytic copper powder has a certain effect on the conductivity of the contact, and the more the electrolytic copper powder ratio is, the higher the conductivity of the contact is, whereby the method of example 1 can be obtained as the optimum method.
4. Study of the effect of stirring time and stirring rate on the degree of mixing of electrolytic copper powder with copper tellurium powder table 4 the effect of stirring time and stirring rate on the degree of mixing of electrolytic copper powder with copper tellurium powder in examples 1, 8, 9
Conclusion: as can be seen from the data in table 4, the stirring time and stirring rate have a certain influence on the degree of mixing of the electrolytic copper powder with the copper tellurium powder, and the longer the stirring time is, the higher the degree of mixing of the electrolytic copper powder with the copper tellurium powder is. The faster the stirring rate, the higher the degree of mixing of the electrolytic copper powder with the copper tellurium powder, so the method of example 1 is the optimal method.
5. Investigation of the influence of the compaction pressure on the green body initial pressure density
TABLE 5 influence of pressing pressure on initial press density of embryo body for examples 1, 10, 11
Conclusion: as can be seen from the data in table 5, the pressing pressure has a certain influence on the initial pressure density of the green body, and the higher the pressing pressure, the higher the initial pressure density of the green body, and thus the method of example 1 is the optimal method.
6. Investigation of the influence of temperature on porosity and shrinkage after sintering of green bodies
TABLE 6 effects of temperatures of examples 1, 12 and 13 on porosity and shrinkage after green body sintering
Conclusion: from the data in Table 6, it is found that the temperature has a certain influence on the porosity and shrinkage after sintering of the green body, and that the higher the temperature, the lower the porosity after sintering of the green body, and the higher the temperature, the higher the shrinkage after sintering of the green body, whereby the method in example 1 is the optimum method.
7. The influence of the difference of applied pressure on the final density of the product during the re-pressing is investigated
TABLE 7 influence of pressure difference applied on final Density of product at double pressing of examples 1, 14 and 15
Conclusion: as can be seen from the data in table 7, the final density of the obtained product was different depending on the pressure applied to the product during the re-pressing, and the higher the applied pressure was, the higher the final density of the product was, whereby the method in example 1 was the optimum method.

Claims (10)

1. The preparation method of the CuTe contact material for the high-voltage direct-current contactor is characterized by mainly comprising the following steps of:
s1, primary batching:
the Cu is as follows by weight percent: 98.5-99.7%, and the balance Te, preparing and batching raw materials, wherein Cu in the raw materials adopts anaerobic Cu;
s2, vacuum induction melting:
loading the Cu block into a crucible, putting the Te block into a secondary feeding device, carrying out vacuum induction smelting treatment on the Cu block, and simultaneously preheating a tundish;
s3, secondary feeding:
adding Te blocks through a secondary feeding device until the Cu melt is completely melted, uniformly stirring the Cu melt and the Te melt, and keeping for 3-5 min;
s4, atomizing and pulverizing:
filling inert gas into a vacuum smelting system, and atomizing when the CuTe alloy melt is completely mixed and uniformly mixed and the temperature of a tundish reaches 1083 ℃;
s5, screening:
screening the atomized powder by adopting powder selecting equipment;
s6, secondary batching:
mixing the atomized copper tellurium powder and the electrolytic copper powder according to the weight percentage, wherein the copper tellurium powder accounts for 50-100%, and the balance is the electrolytic copper powder;
s7, mixing materials
Mixing the atomized copper tellurium powder and the electrolytic copper powder weighed in the step S6 in a double-roll spiral mixer, wherein the stirring speed is 30-60 r/min, and the stirring time is 2-7 h;
s8, pressing
Filling the mixed powder into a forming die, and placing the powder into a dry powder automatic forming hydraulic press at a speed of 2.7-4.1 t/cm 3 Is pressed into a blank by the pressing pressure of the roller;
s9, sintering
Placing the pressed blank into a vacuum sintering furnace, and vacuum-sintering at a vacuum degree of 1×10 -3 ~1×10 -1 Sintering under Pa condition, wherein the sintering mode adopts a gradient heating and heat preservation mode, the highest heating temperature is controlled between 800 ℃ and 1050 ℃, and the heat preservation time is 2 hours;
s10, back pressure
Placing the sintered material into a shaping die, compacting the sintered material on a dry powder automatic forming hydraulic press, and according to the pressure-bearing area of the product, obtaining a compact with a pressure-bearing area of 8-12 t/cm 3 Pressing is carried out, and the product is pressed into a compact state.
2. A method for preparing a CuTe contact material for a high voltage dc contactor according to claim 1, wherein the atomizing means in step S4 comprises water atomization and gas atomization.
3. The method for preparing a CuTe contact material for a high voltage direct current contactor as claimed in claim 2, wherein the water atomization pressure in step S4 is 1500bar, the nozzle is a circular seam nozzle, and the water flow rate is 5m 3 And/ks, adopting 3-6 mm of eye leakage.
4. The method for preparing the CuTe contact material for the high-voltage direct current contactor according to claim 2, wherein in the step S4, a tightly coupled nozzle is used for the gas atomization treatment, the size of a leakage hole is 3-6 mm, the pressure of atomization gas is 2-8 Mpa, and the inert gas is high-purity argon.
5. The method for producing a CuTe contact material for a high voltage direct current contactor according to claim 1, wherein the powder selecting apparatus in step S5 employs a 200 mesh sieve.
6. The method for preparing a CuTe contact material for a high voltage direct current contactor as claimed in claim 1, wherein the electrolytic copper powder in step S6 has a particle size of-200 mesh, a purity of 99.7% or more and an oxygen content of 700ppm or less.
7. The method for manufacturing a CuTe contact material for a high voltage direct current contactor according to claim 1, wherein the outer dimension of the molding area of the molding die in step S8 is 0.5 to 0.7mm smaller than the outer dimension of the product, and the inner hole and the inner step are 0.5 to 0.7mm larger than the product.
8. A process for preparing a CuTe contact material for a high voltage DC contactor as claimed in claim 1, wherein the thickness of the green compact in step S8 is determined according to ρ 2 *V 2 /(ρ 1 *S 1 ) Calculating, wherein ρ 2 V for final density of product 2 For the final volume of the product ρ 1 Is the initial press density of the product, S 1 Is the initial pressure area of the product, ρ 2 Is the final density of the product.
9. The method for preparing a CuTe contact material for a high voltage direct current contactor according to claim 1, wherein the gradient heating and heat preserving mode in step S9 is as follows: heating to 300 ℃ from room temperature and preserving heat for 2 hours, heating to 500 ℃ from 300 ℃ and preserving heat for 2 hours, heating to 3 hours, heating to 800-1050 ℃ from 500 ℃ and preserving heat for 3 hours, heating to 2-5 hours, closing heating, cooling to 60 ℃ along with furnace, and discharging.
10. The method for preparing a CuTe contact material for a high voltage direct current contactor according to claim 1, wherein the outside diameter and the inner hole and the inner step of the shaping mold in S10 are the same as the product size.
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