Nano tin oxide fiber reinforced silver tin oxide low-voltage contact material and preparation method thereof
阅读说明：本技术 纳米氧化锡纤维增强银氧化锡低压触点材料及其制备方法 (Nano tin oxide fiber reinforced silver tin oxide low-voltage contact material and preparation method thereof ) 是由 王军 于 2019-11-12 设计创作，主要内容包括：本发明公开的纳米氧化锡纤维增强银氧化锡低压触点材料及其制备方法,按照质量分数,由以下组分组成：无序纳米氧化锡材料5-40％,微量元素0.5-7％,余量为银元素,以上组分的体积百分比为100％；本发明制备方法通过制备纺丝液、纺丝后退火处理、混合原料过滤、热压烧结、退火处理,得到纳米氧化锡纤维增强银氧化锡低压触点材料。本发明低压触点材料,有完整的导电通道,导电能力优良,具有高硬度和高熔点的特性,使触点材料的硬度和机械性能大幅提高。(The invention discloses a nano tin oxide fiber reinforced silver tin oxide low-voltage contact material and a preparation method thereof, wherein the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material comprises the following components in percentage by mass: 5-40% of disordered nano tin oxide material, 0.5-7% of trace elements and the balance of silver element, wherein the volume percentage of the components is 100%; the preparation method comprises the steps of preparing spinning solution, annealing after spinning, filtering mixed raw materials, hot-pressing sintering and annealing to obtain the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material. The low-voltage contact material has complete conductive channels, excellent conductive capability, high hardness and high melting point, and greatly improves the hardness and mechanical properties of the contact material.)
1. The nano tin oxide fiber reinforced silver tin oxide low-voltage contact material is characterized by comprising the following components in percentage by mass: 5-40% of disordered nano tin oxide material, 0.5-7% of trace elements and the balance of silver element, wherein the volume percentage of the components is 100%.
2. The nano tin oxide fiber reinforced silver tin oxide low voltage contact material according to claim 1, wherein the trace element is specifically any , two, three or four combinations of Cu, W, La or Bi elements.
3. The nano tin oxide fiber reinforced silver tin oxide low voltage contact material according to claim 1, wherein the trace element is any , two or three combinations of elements, in particular Fe, Ni or Co.
4. The nano tin oxide fiber reinforced silver tin oxide low-voltage contact material as claimed in claim 1, wherein the disordered nano tin oxide is prepared by an electrospinning process, the fiber diameter is 50-800nm, and the aspect ratio is not less than 20.
5. The method for preparing a nano tin oxide fiber reinforced silver tin oxide low voltage contact material according to any of claims 1-4, comprising the steps of:
step 1, mixing DMF and ethanol according to a mass ratio of 1:1, adding polyvinylpyrrolidone (PVP), and magnetically stirring for 8-10h until a transparent solution is obtained; dissolving tin tetrachloride pentahydrate in the transparent solution, then adding metal ions, and magnetically stirring for 5-8h to obtain a spinning solution for later use;
wherein the mass of the polyvinyl pyrrolidone is 16-20% of the mass of the spinning solution, and the total mass of the tin tetrachloride pentahydrate and the metal ions is 10-15% of the mass of the spinning solution;
step 2, placing the spinning solution obtained in the step 1 in an electrostatic spinning device for treatment to obtain a disordered nano tin oxide material precursor; placing the disordered nano tin oxide material precursor in a muffle furnace for annealing treatment to obtain disordered SnO2A nanofiber;
step 3, disordered SnO in the step 22Mixing the nano-fiber, the trace elements and the silver powder, putting the mixture into an ethanol solution, magnetically stirring the mixture evenly, then filtering the mixture, and removing clear liquid to obtain Ag-SnO2Powder;
step 4, the Ag-SnO obtained in the step 32And (3) performing cold press molding on the powder, then performing hot press sintering in a vacuum hot press sintering furnace, then performing annealing treatment in a muffle furnace, and performing furnace cooling to obtain the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material.
6. The method for preparing a nano tin oxide fiber reinforced silver tin oxide low-voltage contact material according to claim 5, wherein the metal ions in the step 1 are trace elements, specifically any , two, three or four combinations of Cu, W, La or Bi elements, or any , two or three combinations of Fe, Ni or Co elements.
7. The method for preparing a nano tin oxide fiber reinforced silver tin oxide low-voltage contact material according to claim 5, wherein the annealing treatment parameters in the step 2 are as follows: roasting for 2h at the temperature of 500-600 ℃;
the electrostatic spinning device parameters are as follows: the spinning voltage is 15-20KV, and the spinning distance is 10-20 cm.
8. The method for preparing the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material according to claim 5, wherein the mixing mode in the step 3 is high-energy ball-milling mixing or wet chemical method powder mixing.
9. The method for preparing the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material as claimed in claim 5, wherein the parameters of the cold press molding in the step 4 are as follows: cold-pressing and molding under the pressure of 50 tons in a universal testing machine, wherein the pressure is not less than 30 Mpa; (ii) a
The parameters of the hot-pressing sintering are as follows: the temperature is 850-;
the parameters of the annealing treatment are as follows: the temperature is 450 ℃ and 500 ℃ for 2 h.
10. The method for preparing the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material according to claim 5, wherein the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material in the step 3 comprises the following components in percentage by mass: 5-40% of disordered nano tin oxide material, 0.5-7% of trace elements and the balance of silver element, wherein the mass percent of the components is 100%;
the diameter of the disordered nano tin oxide fiber is 50-800nm, and the length-diameter ratio is not less than 20.
Technical Field
The invention belongs to the technical field of low-voltage contact materials, and particularly relates to kinds of nano tin oxide (SnO)2) Fiber-reinforced silver tin oxide (Ag-SnO)2) The invention also relates to kinds of nano tin oxide (SnO)2) Fiber-reinforced silver tin oxide (Ag-SnO)2) A preparation method of a low-voltage contact material.
Background
The contact material is an electrical contact element widely applied to of low-voltage switching appliances such as relays, circuit breakers, contactors and the like, and mainly plays a role in connecting and disconnecting circuits and load current, and the performance of the contact element is directly related to the stability of the low-voltage switching appliances.
Conventional silver-metal oxide (Ag-MeO) low-voltage contact materials, including Ag-SnO2Ag-CdO, Ag-CuO and Ag-ZnO contacts, in which the second phase metal oxide (MeO) is distributed in the form of particles in a silver matrix, enhancing the mechanical properties and the electrical breaking properties of the material, but the range of applications in low-voltage electrical appliances is limited because of the respective drawbacks.
Ag-SnO2The contact has good arc erosion resistance, wear resistance and fusion welding resistance, and is mainly applied to various low-voltage switches; however, since SnO2Poor wettability of particles and liquid silver, SnO under the action of electric arc2The particles are easy to be enriched on the surface of the contact material, so that the contact resistance of the contact material is increased, the temperature rise is high, and the electrical performance of the contact material is seriously influenced.
Ag-CdO contacts have long been known as "universal contacts" in medium load switches due to their excellent arc erosion resistance, weld resistance, and relatively low contact resistance. However, since Cd steam generated in the arcing process of the Ag-CdO contact is toxic and harmful to the environment and human bodies, the Ag-CdO contact has been gradually replaced by environment-friendly contact materials from the last 90 years.
At present, Ag-CuO contacts are mainly applied to miniature circuit breakers and direct current contactors and become more ideal contact materials for replacing Ag-CdO contacts with environment-friendly defects.
The Ag-ZnO contact material has good large current impact resistance, good breaking performance and ablation resistance, and is mainly applied to small-capacity switching appliances. However, the problems of large contact resistance, too fast temperature rise and poor processability of contact materials are caused by the problems of high hardness of ZnO particles and poor wettability of liquid silver, so that the application of the Ag-ZnO contact in a high-power low-voltage electric appliance is limited.
Disclosure of Invention
The th purpose of the invention is to provide nano tin oxide fiber reinforced silver tin oxide low-voltage contact materials, which solve the problem of the prior SnO2Poor wettability of particles and liquid silver, SnO under the action of electric arc2Particles tend to concentrate on the surface of the contact material, causing a problem that the contact resistance of the contact material increases.
The second purpose of the invention is to provide a preparation method of nano tin oxide fiber reinforced silver tin oxide low-voltage contact materials.
The technical scheme adopted by the invention is that the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material comprises the following components in percentage by mass: 5-40% of disordered nano tin oxide material, 0.5-7% of trace elements and the balance of silver element, wherein the volume percentage of the components is 100%.
The present invention is also characterized in that,
the microelement is specifically any kinds, two kinds, three kinds or four kinds of combination of Cu, W, La or Bi elements.
The microelement is specifically any kinds, two or three kinds of combination of Fe, Ni or Co elements.
The disordered nano tin oxide is prepared by an electrostatic spinning process, the fiber diameter is 50-800nm, and the length-diameter ratio is not less than 20.
The technical scheme adopted by the invention is that the preparation method of the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material comprises the following steps:
step 1, mixing DMF and ethanol according to a mass ratio of 1:1, adding polyvinylpyrrolidone (PVP), and magnetically stirring for 8-10h until a transparent solution is obtained; dissolving tin tetrachloride pentahydrate in the transparent solution, then adding metal ions, and magnetically stirring for 5-8h to obtain a spinning solution for later use;
wherein the mass of the polyvinyl pyrrolidone is 16-20% of the mass of the spinning solution, and the total mass of the tin tetrachloride pentahydrate and the metal ions is 10-15% of the mass of the spinning solution;
step 2, placing the spinning solution obtained in the step 1 in an electrostatic spinning device for treatment to obtain a disordered nano tin oxide material precursor; placing the precursor of the disordered nano tin oxide material in a muffle furnace for annealing treatment to obtain disordered SnO2A nanofiber;
step 3, disordered SnO in the step 22Mixing the nano-fiber, the trace elements and the silver powder, putting the mixture into an ethanol solution, magnetically stirring the mixture evenly, then filtering the mixture, and removing clear liquid to obtain Ag-SnO2Powder;
The present invention is also characterized in that,
in the step 1, the metal ions are trace elements, specifically any , two, three or four combinations of Cu, W, La or Bi elements, or any , two or three combinations of Fe, Ni or Co elements.
The parameters of the annealing treatment in the step 2 are as follows: roasting for 2h at the temperature of 500-600 ℃;
parameters of the electrostatic spinning device: the spinning voltage is 15-20KV, and the spinning distance is 10-20 cm.
The mixing mode in the step 3 is high-energy ball milling mixing or wet chemical method mixing powder.
The parameters of cold pressing molding in the
The parameters of hot-pressing sintering are as follows: the temperature is 850-;
the parameters of the annealing treatment are as follows: the temperature is 450 ℃ and 500 ℃ for 2 h.
In the step 3, the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material comprises the following components in percentage by mass: 5-40% of disordered nano tin oxide material, 0.5-7% of trace elements and the balance of silver element, wherein the mass percent of the components is 100%;
the diameter of the disordered nano tin oxide fiber is 50-800nm, and the length-diameter ratio is not less than 20.
The invention has the beneficial effects that: according to the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material, the metal silver is added, so that the contact material has a complete conductive channel, and the contact material has excellent conductive capability; the problem of insufficient arc erosion resistance of the low-voltage contact material is solved by adding the high-content disordered nano tin oxide fiber, the tin oxide fiber is not easy to float to the surface of the contact under the action of an electric arc, the contact resistance performance of the contact is improved, and the hardness and the mechanical performance of the contact material are greatly improved due to the fact that the disordered nano tin oxide fiber has the characteristics of high hardness and high melting point.
Drawings
FIG. 1 is SnO obtained by the preparation method of example 1 of the present invention2Fiber micrographs;
FIG. 2 is SnO obtained by a preparation method in example 2 of the invention2Fiber micrographs;
FIG. 3 is SnO obtained by a preparation method in example 3 of the invention2Fiber micrographs;
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The nano tin oxide fiber reinforced silver tin oxide low-voltage contact material comprises the following components in percentage by mass: 5-40% of disordered nano tin oxide material, 0.5-7% of trace elements and the balance of silver element, wherein the volume percentage of the components is 100%; the disordered nano tin oxide is prepared by an electrostatic spinning process, the fiber diameter is 50-800nm, and the length-diameter ratio is not less than 20.
The microelement is specifically any , two, three or four combinations of Cu, W, La or Bi elements, or any , two or three combinations of Fe, Ni or Co elements.
The preparation method of the nano tin oxide fiber reinforced silver tin oxide low-voltage contact material comprises the following steps:
step 1, mixing DMF and ethanol according to a mass ratio of 1:1, adding polyvinylpyrrolidone (PVP), and magnetically stirring for 8-10h until a transparent solution is obtained; dissolving tin tetrachloride pentahydrate in the transparent solution, then adding metal ions, and magnetically stirring for 5-8h to obtain a spinning solution for later use;
wherein the vinyl pyrrolidone accounts for 16-20% of the mass of the spinning solution, and the total mass of the tin tetrachloride pentahydrate and the metal ions accounts for 10-15% of the mass of the spinning solution;
adding required metal ions as trace elements, specifically any , two, three or four combinations of Cu, W, La or Bi elements, or any , two or three combinations of Fe, Ni or Co elements, for example Cu element is copper sulfate CuNO3And (4) adding in a form.
Step 2, placing the spinning solution obtained in the step 1 in an electrostatic spinning device for processing, setting the spinning voltage to be 15-20KV and the spinning distance to be 10-20cm, and obtaining a disordered nano tin oxide material precursor; placing the precursor of the disordered nano tin oxide material in a muffle furnace, roasting at the temperature of 500-600 ℃ for 2h, and annealing to obtain the disordered SnO2A nanofiber;
step 3, disordered SnO in the step 22Mixing the nano-fiber, the trace elements and the silver powder, putting the mixture into an ethanol solution, magnetically stirring the mixture evenly, then filtering the mixture, and removing clear liquid to obtain Ag-SnO2Powder;
the mixing mode is high-energy ball milling mixing or wet chemical method mixing powder.
the parameters of cold press molding are as follows: cold-pressing and molding under the pressure of 50 tons in a universal testing machine, wherein the pressure is not less than 30 Mpa; the parameters of hot-pressing sintering are as follows: the temperature is 850-; the parameters of the annealing treatment are as follows: the temperature is 450 ℃ and 500 ℃ for 2 h.
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