CN1743477A - Preparation of copper-chromium alloy contact material by aluminothermal reduction-electromagnetic casting process - Google Patents
Preparation of copper-chromium alloy contact material by aluminothermal reduction-electromagnetic casting process Download PDFInfo
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Abstract
This invention relates to a method for preparing CuCr alloy contactor material by the thermit-magnetic casting method, which takes CuO Cr2O3 as the raw material, Al powder as the recovery agent and adds suitable CaF2 or Ni, Co elements to mix them evenly and put them into a self-spread reaction oven to initiate thermit recovery reaction and separate metal and slag stirred by the magnetic field to get high temperature CuCr alloy melt, which is quickly cooled by circulation water in a graphite die to get the CuCr ingot.
Description
Technical Field
The invention belongs to the technical field of alloy material preparation, and particularly relates to a method for preparing a copper-chromium alloy contact material by an aluminothermic reduction-electromagnetic casting method.
Background
The contact material is a key factor determining the performance of the vacuum circuit breaker, and the ideal contact material must have the following electrical properties: large breaking current capacity, high voltage resistance, reliable fusion welding resistance, high electric conductivity and thermal conductivity, low arc burning loss rate, low current interception value and the like. In recent years, with the development of high-power vacuum high-voltage switch technology, CuCr series alloy contact materials gradually replace traditional W-Cu and Cu-Bi series alloy contact materials with a plurality of excellent performances, and are widely applied to medium-high voltage high-power vacuum switch circuits, and the application range of the CuCr series alloy contact materials is expected to be wider along with the continuous improvement of the performances. From the Cu-Cr alloy phase diagram, the CuCr alloy belongs to immiscible series alloy. The solid solubility of Cr in Cu is very low, and only 0.7 percent of Cr is dissolved in Cu at 1080 ℃; it is almost insoluble below 600 deg.C, and 1.28% of Cu dissolves in Cr at this temperature, so CuCr alloy can be considered as a pseudo alloy of two-component mechanical mixing. When the liquid phase Cu or Cr alloy is solidified, Cr tends to be co-crystallized and to segregate in specific gravity, resulting in macro-segregation. Therefore, the CuCr alloy cannot be produced by a conventional melting method.
The electrical property of the CuCr alloy high-voltage contact material depends on the microstructure thereof, and the microstructure depends on the preparation process thereof. Therefore, the preparation process and technology for developing the CuCr alloy are put to the first place in all countries in the world. At present, the processes for preparing the CuCr alloy mainly comprise a powder metallurgy method, an infiltration method and a vacuum arc melting method. The CuCr alloy prepared by the powder sintering method is prepared by fully and uniformly mixing copper powder and chromium powder in a certain proportion, compacting, and then sintering and forming. The main disadvantage of the powder sintering process is the severe quality requirements for the powder, especially for chromium powder. The product prepared by the process has relatively low quality, the fluctuation of the oxygen content is large and can reach 0.2 percent, and the service life of the product is seriously influenced. The infiltration method for preparing CuCr alloy is that proper amount of copper powder and all chromium powder are fully mixed and pressed into compact, and the compact is sintered into porous chromium skeleton under vacuum or reducing atmosphere, the sintering temperature is controlled near the melting point of copper (1083 ℃), and then the compact is immersed into molten copper under vacuum, so that the compact is fully immersed into the pre-sintered chromium skeleton under the action of capillary force. The drawback of the infiltration process is the low production efficiency, the relatively coarse chromium particles and the substantial proportion of chromium content. It is difficult to prepare alloys with less chromium, such as Cu-25% Cr, due to the limitations of the preparation principle of the process itself. The CuCr contact material is prepared by an arc melting method, which is characterized in that a CuCr alloy ingot which is subjected to isostatic pressing and then is sintered in vacuum is used as a consumable electrode, the electrode is rapidly melted under the action of direct current arc in vacuum (or inert gas atmosphere), and then the electrode is rapidly cooled and solidified to form an ingot. However, the method needs a vacuum system and a direct current arc power supply with high cost and complex structure, the production cost is high, and a plurality of process parameters need to be further searched and perfected.
The traditional CuCr alloy preparation process has own defects and shortcomings, for example, the defects which are difficult to overcome by the powder metallurgy and infiltration framework sintering process lead to lower product performance, product yield, unavailable unqualified products and the like, so the popularization and the application of the CuCr alloy contact material are seriously limited. Further, there are methods such as plasma spraying and laser surface alloying, but they are under study.
Disclosure of Invention
Aiming at the defects of the prior art for preparing the CuCr alloy contact material, the invention provides a method for preparing a copper-chromium alloy contact material by an aluminothermic reduction-electromagnetic casting method.
The method uses CuO and Cr2O3The method comprises the steps of taking Al powder as a reducing agent, obtaining a high-temperature melt of the copper-chromium alloy by adopting an aluminothermic reduction process, and solidifying the copper-chromium alloy under the stirring of an electromagnetic field to obtain an alloy ingot of D40-80. Firstly, the materials are mixed according to a certain proportion, and the mass ratio of CuO to Cr is2O3Al is mixed in a ratio of 100 to (60-115) to (120-160) according to the relative ratio of reactants (CuO and Cr)2O3And Al powder) 0-0.6% by weightThe Cu content of the CuCr alloy is 50-80%, the Cr content is 50-20%, and the Ni content and the Co content are about 0-1%, and the relative amounts of the alloy elements (CuO and Cr) are calculated according to the formula2O3And Al powder) by adding 2-5% of CaF into the raw material2Or Na3A1F6Or NaF, CaO, MgO or a mixture of the compounds, grinding the reaction mixture, uniformly mixing, putting the mixture into a self-made self-propagating reaction furnace, adding Mg powder serving as an ignition agent in the air atmosphere, igniting the mixture by naked fire to initiate an aluminothermic reduction reaction, and instantly finishing the aluminothermic reaction, wherein the general reaction time is about 10s, so that a high-temperature melt is obtained, and the highest temperature of the melt can reach more than 2500K; and then stirring for 6-9 min under the stirring action of an electromagnetic field, carrying out gold slag separation on the high-temperature melt, casting the separated high-temperature melt of the copper-chromium alloy, and rapidly cooling the high-temperature alloy melt under the water cooling condition to solidify to obtain the copper-chromium alloy cast ingot.
The reaction device for preparing the copper-chromium alloy contact material mainly comprises a magnetic stirring device (shown in figure 1 and provided with a circulating cooling system), a reactor (shown in figure 2) and a crystallizer (cylindrical graphite casting mold), wherein a high-temperature melt obtained by reaction of reactants flows outfrom a liquid outlet at the lower part of the reactor and is drained to the crystallizer through a graphite guide pipe for casting.
The method for producing the CuCr alloy firstly comprises an aluminothermic high-temperature reduction stage, namely, grinding and fully mixing a reaction mixture, reacting in an aluminothermic reduction mode to obtain a high-temperature melt, and then separating gold slag under the stirring action of an electromagnetic field to obtain a pure high-temperature copper-chromium alloy melt. This process can be implemented by the following method:
taking CuO and Cr2O3And Al powder in a mass ratio of CuO to Cr2O3Al is mixed in a ratio of 100 to (60-115) to (120-160) according to the relative ratio of reactants (CuO and Cr)2O3And Al powder), 0-0.6% of trace alloy elements such as Ni and Co are added, and 2-5% of CaF is added into the raw materials2Or Na3AlF6Or NaF or CaO or MgO orThe reaction mixture is ground and uniformly mixed by a mortar, the ground particle size of the raw materials reaches 2-100 mu m, the raw materials are placed into a self-propagating reaction furnace, a proper amount of Mg powder is added on the surface layer of the reactants to serve as an ignition agent, the Mg powder is directly ignited by open fire in the air atmosphere, the aluminothermic reduction reaction is further initiated, meanwhile, electromagnetic field stirring is carried out, gold and slag separation is carried out under the electromagnetic field stirring effect, and the high-temperature copper-chromium alloy melt can be obtained. The main reaction equation is:
because the thermite reduction reaction is carried out in an open air atmosphere and the thermite reduction reaction temperature is very high, a large amount of Al is gasified in the reaction process, so that a large amount of Al is volatilized and lost, and the Al is insufficient. In order to compensate for the volatilization loss of Al, the proportion of Al can be increased properly during the material preparation, and the excess of Al powder is 20-50 percent, so as to ensure that CuO and Cr are in the reaction system2O3Is completely reduced.
In addition, as the thermit reduction reaction is carried out in an open system, the heat loss of the reaction system is large, and 0-3% of KClO can be added according to the percentage relative to the total mass of reactants during the batching in order to compensate the heat loss of the system3And the reaction with Al powder in the reactant can release a large amount of reaction heat, so that the loss of heat is compensated.
In order to ensure that the gold slag is fully and effectively separated, 2-5% of CaF added in the raw materials is added in the raw materials2Or Na3AlF6Or NaF, CaO, MgO or the mixture of the compounds, improves the physical properties of the slag system, reduces the melting point of the slag, improves the fluidity of the slag and further strengthens the separation effect of the gold slag.
The operation is carried out in an open air atmosphere, so the operation is simple, no potential safety hazard exists, and the method is very suitable for industrial production. But is made ofThe volatilization loss of Al in the reaction process is compensated, and the proper increase of the proportioning of Al during the material preparation needs to be ensured. Simultaneously, 2-5% of CaF is added into the reaction raw materials2Or Na3AlF6Or NaF, CaO, MgO or the mixture of the compounds, the separation effect of the gold slag is strengthened, the purity of the obtained copper-chromium alloy melt is ensured, and inclusions such as metal oxides and the like carried in the alloy melt are avoided.
The other important process stage is the solidification process of the high-temperature alloy melt in the aluminothermic high-temperature reduction stage, namely, the high-temperature alloy melt is rapidly cooled in a graphite casting mould by adopting circulating water cooling under the stirring action of an electromagnetic field to obtain the CuCr alloy cast ingot. This process can be implemented by the following method:
firstly, preheating a graphite mold to 600-700 ℃, starting circulating water for circulating water cooling, directly casting a copper-chromium alloy melt into a graphite casting mold with the preheating temperature of 600-700 ℃, continuing electromagnetic stirring, controlling the electromagnetic stirring time to be 6-9 min, then stopping stirring, continuing circulating water cooling, and cooling an alloy cast ingot to room temperature. Because the high-temperature melt is stirred by the electromagnetic field and is rapidly cooled and solidified under the circulating water cooling condition, the obtained alloy ingot has uniform components, fine microstructure and high density, and the defects of macro segregation and the like are avoided.
The main equipment adopted by the invention is shown in the attached drawings, wherein, figure 1 is a structural schematic diagram of a magnetic stirring device, and figure 2 is a structural schematic diagram of a graphite reactor adopted by self-propagating reaction. When the device is used, the graphite reactor is fixed above the neodymium iron boron permanent magnetic stirrer 3 through a tripod, and an opening at the bottom of the graphite reactor is connected with a crystallizer (graphite casting mold) 1 through a graphite guide pipe to realize casting of alloy liquid; the motor 4 and the neodymium iron boron permanent magnetic stirrer 3 are driven by a chain.
The invention has the following advantages:
1. with CuO and Cr2O3The raw material is Al powder which is used as a reducing agent, so that the raw material cost is greatly reduced;
2. an aluminothermic reduction reaction mode is adopted, the reaction heat of the reaction is fully utilized, and the energy consumption is reduced;
3. all operations are carried out in air atmosphere, and the aluminothermic reduction reaction is ignited by open fire, so that the operation is simple, the requirements on process conditions are low, and a foundation is laid for industrial production;
4. the high-temperature copper-chromium alloy melt obtained by the aluminothermic reduction reaction is stirred under the action of an electromagnetic field, so that the uniform mixing of liquid Cu and Cr is ensured;
5. because the slag performance is improved and the gold slag separation effect is enhanced, the purity of the obtained copper-chromium alloy melt is very high;
6. the high-temperature melt of the copper-chromium alloy is rapidly cooled and solidified by adopting circulating water cooling under the condition of stirring of an electromagnetic field, so that the obtained copper-chromium alloy ingot has uniform components and high density, and macrosegregation is avoided;
7. the method not only can prepare large-size copper-chromium alloy cast ingots, but also can prepare CuCr20～CuCr50Copper-chromium alloys of equivalent series for the preparation of CuCr25The copper-chromium alloys of the series with lowchromium content have the technical advantages of themselves.
Drawings
FIG. 1 is a schematic structural view of a magnetic stirring apparatus, in which: 1 crystallizer (graphite casting mould), 2 circulating water outlet, 3 neodymium iron boron permanent magnetic stirrer and 4 motor.
FIG. 2 is a schematic view of a graphite reactor used for the self-propagating reaction.
Detailed Description
Example 1:
taking CuO and Cr2O3And Al powder in a mass ratio of CuO to Cr2O3Mixing Al powder in the ratio of 100 to 114 to 160 to ensure that the Al powder is excessive by 50 percent and simultaneously corresponding to reactants (CuO and Cr)2O3And Al powder) in percentage by massAdding 5 percent of CaF into the raw materials2The reactants are mixed homogeneously, howeverThen the reaction mixture is put into an aluminothermic reduction reaction furnace, a proper amount of Mg powder is added on the surface layer of the reactant as an ignition agent, and the Mg powder is ignited by heating open fire in the air atmosphere to initiate the aluminothermic reduction reaction. And meanwhile, starting an electromagnetic stirring device, carrying out a gold slag separation process under the stirring action of an electromagnetic field to obtain a high-temperature copper-chromium alloy melt, starting circulating water for circulating water cooling, and continuously casting the separated high-temperature alloy melt into a graphite casting mold, wherein the preheating temperature of the graphite mold is 600 ℃. Continuing to perform electromagnetic stirring, simultaneouslyperforming circulating water cooling, stirring for 7min, stopping stirring, and continuously cooling to room temperature to obtain CuCr50The copper-chromium alloy ingot.
Example 2:
taking CuO and Cr2O3And Al powder in a mass ratio of CuO to Cr2O3Mixing Al powder in the ratio of 100 to 110 to 150 to ensure that the Al powder is over 40 percent and the reactants (CuO and Cr) are added2O3And Al powder) 0.6 percent of Ni as an alloy element and 3 percent of heat generating agent KClO according to the percentage of the total mass of reactants3Simultaneously, adding 2% of NaF into the raw materials, uniformly mixing reactants, then putting the reaction mixture into an aluminothermic reduction reaction furnace, adding a proper amount of Mg powder serving as an ignition agent into the surface layer of the reactants, heating open fire in the air atmosphere to ignite the Mg powder, and initiating an aluminothermic reduction reaction. And meanwhile, starting an electromagnetic stirring device, carrying out a gold slag separation process under the stirring action of an electromagnetic field to obtain a high-temperature copper-chromium alloy melt, starting circulating water for circulating water cooling, and continuously casting the separated high-temperature alloy melt into a graphite casting mold, wherein the preheating temperature of the graphite mold is 680 ℃. Continuing to perform electromagnetic stirring, simultaneously performing circulating water cooling, stirring for 9min, stopping stirring, and continuously cooling to room temperature with circulating water to obtain CuCr49Ni1The copper-chromium alloy ingot.
Example 3:
taking CuO and Cr2O3And Al powder in a mass ratio of CuO to Cr2O3Mixing Al powder in the ratio of 100 to 60 to 120 to ensure 20% excess of Al powderAnd 2 percent of heating agent KClO is added3Simultaneously, 3 percent of CaO is added into the raw materials, reactants are uniformly mixed, then the reaction mixture is put into a self-propagating reaction furnace, a proper amount of Mg powder is added on the surface layer of the reactants as an ignition agent, and the Mg powder is ignited by heating open fire in the air atmosphere to initiate the aluminothermic reduction reaction. And meanwhile, starting an electromagnetic stirring device, carrying out a gold slag separation process under the stirring action of an electromagnetic field to obtain a high-temperature copper-chromium alloy melt, starting circulating water for circulating water cooling, and continuously casting the separated high-temperature alloy melt into a graphite casting mold, wherein the preheating temperature of the graphite mold is 700 ℃. Continuing to perform electromagnetic stirring and circulating water cooling, stirring for 6min, stopping stirring, and continuously circulating water cooling to room temperature to obtain CuCr25The copper-chromium alloy ingot.
Claims (3)
1. The preparation method of copper-chromium alloy contact material by using aluminothermic reduction-electromagnetic casting method is characterized by that it uses CuO and Cr2O3Taking Al powder as a reducing agent as a raw material, and taking CuO and Cr in a mass ratio2O3Mixing Al in a ratio of 100 to (60-115) to (120-160), adding 0-0.6% of Ni or Co alloy element and 2-5% of CaF in percentage by mass relative to the total mass of reactants2Or Na3AlF6Or NaF, CaO, MgO or a mixture of the compounds, grinding and uniformly mixing the reaction mixture, putting the mixture into a self-propagating reaction furnace, adding a proper amount of Mg powder intothe surface layer of a reactant, directly igniting the Mg powder by open fire in the air atmosphere to initiate an aluminothermic reduction reaction, simultaneously stirring by an electromagnetic field, and separating gold slag under the stirring action of the electromagnetic field to obtain a copper-chromium alloy melt; and circulating water cooling is started to be introduced, the copper-chromium alloy melt is directly cast into a graphite casting mold with the preheating temperature of 600-700 ℃, electromagnetic stirring is continuously carried out, the electromagnetic stirring time is controlled to be 6-9 min, then stirring is stopped, circulating water cooling is continuously carried out, and the alloy ingot is cooled to the room temperature.
2. The aluminothermic reduction-electromagnetic casting process of claim 1 to produce copper chromeThe gold contact material is characterized in that 0-3% of KClO is added according to the percentage relative to the total mass of reactants during burdening3In the process of aluminothermic reduction reaction, the heat released by the reaction of the aluminum powder and the Al powder in the reactant is utilized to make up the heat loss of the reaction system.
3. The apparatus for preparing Cu-Cr alloy contact material by aluminothermic reduction-electromagnetic casting method according to claim 1, wherein the apparatus comprises a crystallizer, a circulating water outlet, a Nd-Fe-B permanent magnetic stirrer, a motor, and a graphite reactor, wherein the graphite reactor is fixed above the Nd-Fe-B permanent magnetic stirrer through a tripod, the bottom opening of the graphite reactor is connected with the crystallizer through a graphite conduit, and the motor and the Nd-Fe-B permanent magnetic stirrer are driven by a chain.
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