CN112475295A - Silver iron oxide electric contact material with oxide particles dispersed and distributed and preparation method thereof - Google Patents
Silver iron oxide electric contact material with oxide particles dispersed and distributed and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silver iron oxide electric contact material with oxide particles dispersed and distributed and a preparation method thereof, wherein the preparation method comprises the following steps: (1) smelting silver and modified additive metal, and atomizing into alloy powder; (2) drying the alloy powder, and sieving with a 200-mesh sieve to prepare alloy powder of-200 meshes; (3) mixing atomized alloy powder of-200 meshes with iron powder; (4) carrying out powder rolling on the powder mixed in the step (3) to form a strip; (5) annealing the strip followed by further cold rolling; (6) and internally oxidizing the rolled strip, and then performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain the plate or wire. The silver ferric oxide electric contact material prepared by the method has the advantages of fine oxide particle size, uniform tissue, obviously improved material yield compared with the conventional multiple extrusion process, and suitability for mass production.
Description
Technical Field
The invention belongs to the technical field of electrical contacts, and particularly relates to a silver iron oxide electrical contact material with oxide particles dispersed and distributed and a preparation method thereof.
Background
In the field of the existing electric contact, silver-based electric contact materials are the most widely applied materials at present. This is because silver has high electrical and thermal conductivity, good machining characteristics; and because the silver oxide is unstable at high temperature and is easily decomposed into simple substance silver and oxygen, the low and stable contact resistance of the silver-based electric contact material can be ensured.
At present, the silver-based electric contact materials are mainly divided into three types: silver-metal oxides, silver-based pseudo alloys, silver-based alloys, wherein silver metal oxides play an important role in the whole electrical contact material system due to their excellent overall electrical properties. The silver iron oxide material as a silver metal oxide electric contact material has low and stable contact resistance, good electric conduction, heat conduction and stable and excellent temperature rise characteristics, and has more excellent fusion welding resistance than silver nickel and silver tungsten materials which are widely applied particularly under the application condition of a high-current switch.
Because the solid solubility between silver and iron is limited, the common preparation process of silver iron oxide is determined to be divided into two types: powder metallurgy process, chemical codeposition process. The simple process flow of the silver iron oxide powder metallurgy process is as follows: the production process comprises the following steps of mixing silver powder, iron oxide powder and additive powder, isostatic pressing, sintering, re-pressing and hot extrusion to form plates or wires, and has the main defects: because the raw material powder particles are fine and easy to agglomerate, the iron oxide and the additive particles cannot be fully dispersed in the mixing process, so that the defects of oxide or additive powder aggregation and uneven distribution cannot be avoided in a finished product, and the electrical property stability of the material is further influenced. The preparation process of the silver ferric oxide codeposition process is simple as follows: preparing silver, iron and additive metal salt solution with certain concentration, preparing precipitant solution with certain concentration, adding the precipitant solution into the mixed solution at a certain speed for precipitation, cleaning silver, iron and additive coprecipitates, drying the silver, iron and additive coprecipitates, calcining the silver, iron and additive coprecipitates to prepare silver metal oxide composite powder, isostatic pressing, sintering, and finally extruding into plates or wires, although the process can effectively solve the problem of dispersion of oxide particles, but the production process has long flow and more complicated working procedures, the most important defect is that the metal ions used as the precipitating agent are difficult to remove in the subsequent cleaning working procedures, the content of low-melting-point impurities in the finished material is high, the arcing energy of the material is high, the arcing time is long, and the arc burning resistance of the material is greatly reduced.
By search, Chinese patent CN101794636 is a preparation method of silver iron oxide electric contact material. The method mainly comprises the following process steps: preparing a mixed solution of silver nitrate, ferric nitrate and zirconium nitrate with a certain concentration, adding a sodium hydroxide, sodium carbonate or sodium bicarbonate precipitator into the mixed solution to prepare metal carbonate precipitate, cleaning the metal carbonate solution, drying and calcining to prepare silver metal oxide composite powder, and finally sieving, isostatic pressing, sintering and hot extruding the composite powder to form a wire or a plate. According to the method, the synthesized metal carbonate is flocculent and precipitates which are relatively fluffy, so that low-melting-point impurity sodium introduced by adding a precipitator cannot be effectively removed in the cleaning process, and finally the content of the low-melting-point impurity sodium in a finished material is relatively high, so that the material shows relatively high arcing energy and relatively long arcing time in the opening and closing processes of an electric test, and the electric arc burning resistance of the material is finally influenced.
Although the process method adopted by the patent can solve the problem of oxide particle aggregation, low-melting-point impurity metal which cannot be removed in the subsequent cleaning process is introduced in the process; the traditional powder metallurgy process can not effectively realize the uniform dispersion of iron oxide particles and additive particles. Therefore, how to achieve uniform dispersion of oxide particles and ensure that no low-melting-point metal impurities are introduced in the preparation process of the material is a difficult problem in the field of preparation of the material, and therefore, improvement is needed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a silver iron oxide electric contact material with dispersed oxide particles and a preparation method thereof. The silver ferric oxide electric contact material prepared by the method has the advantages of fine oxide particle size, uniform tissue, obviously improved material yield compared with the conventional multiple extrusion process, and suitability for mass production.
In order to achieve the above object, a first aspect of the present invention provides a silver iron oxide electrical contact material in which oxide particles are dispersed. The technical scheme comprises the following steps:
(1) smelting silver and modified additive metal, and atomizing into alloy powder;
(2) drying the alloy powder, and sieving with a 200-mesh sieve to prepare alloy powder of-200 meshes;
(3) mixing atomized alloy powder of-200 meshes with iron powder;
(4) carrying out powder rolling on the powder mixed in the step (3) to form a strip;
(5) annealing the strip followed by further cold rolling;
(6) and internally oxidizing the rolled strip, and then performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain the plate or wire.
The further setting is that the modifying additive metal in the step (1) is one or a combination of more of metal molybdenum, metal yttrium and metal lanthanum.
The further setting is that in the step (1): the atomization temperature is 1000-1300 ℃, and the atomization water pressure is 30-50 MPa.
Further setting the drying parameter conditions in the step (2) as follows: drying temperature: 100-350 ℃; drying time: 3-12 h.
Further setting that the iron powder in the step (3) is carbonyl iron powder, and the laser particle size distribution is as follows: d10 is less than 1.2 mu m, D50 is 1.5-3.5 mu m, and D90 is less than 6 mu m; the parameter process for mixing 200-mesh atomized alloy powder and iron powder comprises the following steps: the single mixing amount is 15-50 kg, and the mixing time is 2-10 h.
The further setting is that the specific implementation method of the powder rolling in the step (4) comprises the following steps: and rolling a strip rolling blank with the thickness of 4-8 mm and the width of 60-100 mm by using the self flowability of the powder and the friction resistance between rolling and the powder by using a two-roller horizontal rolling mill and an inclined feeding machine.
Further setting that the annealing process of the strip material in the step (5) is as follows: annealing temperature: 550-750 ℃ and annealing time: 60-180 min, annealing atmosphere: a hydrogen atmosphere; the annealing mainly aims at removing internal stress caused in the powder rolling process and improving the subsequent plastic processing deformation capacity; and finally rolled into a strip having a thickness of 1.5 mm.
The further setting is that the internal oxidation process in the step (6) is as follows: the oxidation temperature is 600-850 ℃, and the oxidation time is as follows: 24-48 h, oxidation pressure: 0.4-0.95 MPa, and finally performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain a plate or wire.
In addition, the invention also provides the oxide particle dispersion distribution silver iron oxide electric contact material prepared by the preparation method, the components and the content of the iron oxide electric contact material are that the content of iron oxide is 5-15 wt%, the content of a modification additive is 0.01-2 wt%, and the balance is silver, and the modification additive is one or the combination of more of molybdenum oxide, yttrium oxide and lanthanum oxide. The size of the oxide particles of the silver iron oxide material prepared by the method is less than or equal to 1 mu m, and the maximum size of the aggregated oxide particles in the metallographic structure of the whole transverse and longitudinal sections of the finished wire or plate is less than or equal to 5 mu m.
The invention has the advantages that:
1) the silver and the modified additive are melted and atomized into alloy powder, and the formed powder is alloy powder, so that the dispersion uniformity of the additive metal components is atomic-level dispersion, and the problem of the dispersion uniformity of the additive components in the conventional powder metallurgy process can be fundamentally solved;
2) mixing atomized alloy powder with iron powder, then carrying out powder rolling on the mixed powder to form a strip and carrying out subsequent cold rolling plastic deformation on the strip to a certain thickness: further dispersion is achieved by utilizing the particle rearrangement of the metal simple substance iron powder in the powder rolling process; by utilizing the coordinated plastic deformation of the elementary substance metal iron particles in the cold rolling process, the elementary substance iron particles are further refined, and finally, the iron oxide particles are fine and are in dispersed distribution;
3) compared with a codeposition preparation process, the method avoids low-melting-point impurities introduced by adding a precipitator (potassium, sodium carbonate or bicarbonate), so that the material does not contain low-melting-point impurity metal content, the arcing characteristic of the material is effectively improved, the anti-arc burning loss characteristic of the material is improved, and the method has the characteristics of short and simple manufacturing process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a flow chart of a process for preparing an ultrafine oxide particle silver iron oxide electrical contact material;
FIG. 2 preparation of AgFe by traditional powder metallurgy process2O3(total content of oxide is 6.4%) horizontal and longitudinal metallographic structure photographs of the material;
FIG. 3 AgFe prepared by the method of the invention2O3(total content of oxide is 6.4%) of the material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
The first embodiment is as follows:
the implementation case is carried out according to the following steps:
1) according to the weight percentage of the final product, Ag is Fe2O3:MoO325.318kg of silver ingot was weighed out and melted in a medium frequency induction furnace, followed by the addition of 0.182 pieces of molybdenum metal to form a silver-molybdenum alloy, as required for 93.6:5.4: 1. Controlling the atomization temperature of the solution at 1280 +/-20 ℃, and atomizing the silver-molybdenum alloy into alloy powder under the pressure of 40 +/-5 MPa of atomization water pressure.
2) Drying the silver-molybdenum atomized alloy powder at 250 +/-10 ℃ for 8h +/-10 min to thoroughly remove water in the powder;
3) sieving the dried powder with a 200-mesh sieve, wherein the undersize is used as raw material powder for subsequent mixing with iron powder;
4) 18.854kg of silver-molybdenum alloy powder with a particle size of-200 meshes and 0.756kg of carbonyl iron powder are weighed and mixed in a plough share mixer for 4h +/-10 min.
5) And (3) rolling the mixed powder by using a two-roll horizontal rolling mill and an inclined feeding machine according to the self flowability of the powder and the frictional resistance between the roller and the powder to roll a strip rolling blank with the thickness of 6mm and the width of 70 mm.
6) Performing hydrogen annealing on the strip at 600 ℃ for 120 +/-10 min, wherein the annealing is mainly used for removing internal stress caused in the powder rolling process and improving the subsequent plastic processing deformation capacity; and finally rolled into a strip having a thickness of 1.5 mm.
7) Carrying out internal oxidation on the rolled strip, and setting the oxidation parameters as follows: the oxidation temperature is 800 +/-10 ℃, and the oxidation time is as follows: 28 +/-0.5 h, oxidation pressure: 0.6 +/-0.05 MPa. And then, performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain a plate or a wire. AgFe prepared by adopting the process2O3(5.4％)MoO3(1%) wire was subsequently drawn to
The physical and mechanical property test results of the finished wire are as follows:
example two:
the implementation case is carried out according to the following steps:
1) according to the weight percentage of the final product, Ag is Fe2O3:Y2O325.286kg of silver ingot was weighed out and melted in a medium frequency induction furnace as required for 93.6:5.4:1, followed by the addition of 0.214 mass of metallic yttrium to form a silver yttrium alloy. Controlling the atomization temperature of the solution at 1200 +/-20 ℃, and atomizing the silver-yttrium alloy into alloy powder under the pressure of the atomization water pressure of 40 +/-5 MPa.
2) Drying the silver-yttrium atomized alloy powder at 250 +/-10 ℃ for 8h +/-10 min to thoroughly remove moisture in the powder;
3) sieving the dried powder with a 200-mesh sieve, wherein the undersize is used as raw material powder for subsequent mixing with iron powder;
4) 18.878kg of silver-yttrium alloy powder with a particle size of-200 meshes and 0.756kg of carbonyl iron powder are weighed and mixed in a plough shovel type mixer for 4h +/-10 min.
5) And (3) rolling the mixed powder by using a two-roll horizontal rolling mill and an inclined feeding machine according to the self flowability of the powder and the frictional resistance between the roller and the powder to roll a strip rolling blank with the thickness of 6mm and the width of 70 mm.
6) Performing hydrogen annealing on the strip at 600 ℃, wherein the annealing time is 120 +/-10 min, and the annealing is mainly used for removing internal stress caused in the powder rolling process and improving the subsequent plastic processing deformation capacity; and finally rolled into a strip having a thickness of 1.5 mm.
7) Carrying out internal oxidation on the rolled strip, and setting the oxidation parameters as follows: the oxidation temperature is 800 +/-10 ℃, and the oxidation time is as follows: 28 +/-0.5 h, oxidation pressure: 0.6 +/-0.05 MPa. And then, performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain a plate or a wire. AgFe prepared by adopting the process2O3(5.4％)Y2O3(1%) wire was subsequently drawn to
The physical and mechanical property test results of the finished wire are as follows:
example three:
the implementation case is carried out according to the following steps:
1) according to the weight percentage of the final product, Ag is Fe2O3:La2O325.27kg of silver ingot was weighed out and melted in a medium frequency induction furnace as required for 93.6:5.4:1, followed by the addition of 0.23 mass of lanthanum metal to form a silver lanthanum alloy. Controlling the atomization temperature of the solution at 1250 +/-20 ℃, and atomizing the silver-lanthanum alloy under the pressure of the atomization water pressure of 40 +/-5 MPaAlloying powder.
2) Drying the silver-lanthanum atomized alloy powder at 250 +/-10 ℃ for 8h +/-10 min to thoroughly remove water in the powder;
3) sieving the dried powder with a 200-mesh sieve, wherein the undersize is used as raw material powder for subsequent mixing with iron powder;
4) weighing 18.89kg of-200-mesh silver-lanthanum alloy powder and 0.756kg of carbonyl iron powder, and mixing the powder in a plough share mixer for 4h +/-10 min.
5) And (3) rolling the mixed powder by using a two-roll horizontal rolling mill and an inclined feeding machine according to the self flowability of the powder and the frictional resistance between the roller and the powder to roll a strip rolling blank with the thickness of 6mm and the width of 70 mm.
6) Performing hydrogen annealing on the strip at 600 ℃, wherein the annealing time is 120 +/-10 min, and the annealing is mainly used for removing internal stress caused in the powder rolling process and improving the subsequent plastic processing deformation capacity; and finally rolled into a strip having a thickness of 1.5 mm.
7) Carrying out internal oxidation on the rolled strip, and setting the oxidation parameters as follows: the oxidation temperature is 800 +/-10 ℃, and the oxidation time is as follows: 28 +/-0.5 h, oxidation pressure: 0.6 +/-0.05 MPa. And then, performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain a plate or a wire. AgFe prepared by adopting the process2O3(5.4％)La2O3(1%) wire was subsequently drawn to
The physical and mechanical property test results of the finished wire are as follows:
the above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (9)
1. A preparation method of a silver iron oxide electric contact material with dispersed oxide particles is characterized by comprising the following steps:
(1) smelting silver and modified additive metal, and atomizing into alloy powder;
(2) drying the alloy powder, and sieving with a 200-mesh sieve to prepare alloy powder of-200 meshes;
(3) mixing atomized alloy powder of-200 meshes with iron powder;
(4) carrying out powder rolling on the powder mixed in the step (3) to form a strip;
(5) annealing the strip followed by further cold rolling;
(6) and internally oxidizing the rolled strip, and then performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain the plate or wire.
2. The method for producing a silver-iron oxide electrical contact material having oxide particles dispersed therein according to claim 1, characterized in that: the modifying additive metal in the step (1) is one or a combination of more of metal molybdenum, metal yttrium and metal lanthanum.
3. The method for producing a silver-iron oxide electrical contact material having oxide particles dispersed therein according to claim 1, characterized in that: in the step (1): the atomization temperature is 1000-1300 ℃, and the atomization water pressure is 30-50 MPa.
4. The method for producing a silver-iron oxide electrical contact material having oxide particles dispersed therein according to claim 1, characterized in that: the drying parameter conditions in the step (2) are as follows: drying temperature: 100-350 ℃; drying time: 3-12 h.
5. The method for producing a silver-iron oxide electrical contact material having oxide particles dispersed therein according to claim 1, characterized in that: the iron powder in the step (3) is carbonyl iron powder, and the laser particle size distribution is as follows: d10 is less than 1.2 mu m, D50 is 1.5-3.5 mu m, and D90 is less than 6 mu m; the parameter process for mixing 200-mesh atomized alloy powder and iron powder comprises the following steps: the single mixing amount is 15-50 kg, and the mixing time is 2-10 h.
6. The method for producing a silver-iron oxide electrical contact material having oxide particles dispersed therein according to claim 1, characterized in that: the specific implementation method of the powder rolling in the step (4) comprises the following steps: and rolling a strip rolling blank with the thickness of 4-8 mm and the width of 60-100 mm by using the self flowability of the powder and the friction resistance between rolling and the powder by using a two-roller horizontal rolling mill and an inclined feeding machine.
7. The method for producing a silver-iron oxide electrical contact material having oxide particles dispersed therein according to claim 1, characterized in that: the annealing process of the strip material in the step (5) comprises the following steps: annealing temperature: 550-750 ℃ and annealing time: 60-180 min, annealing atmosphere: a hydrogen atmosphere; and finally rolled into a strip having a thickness of 1.5 mm.
8. The method for producing a silver-iron oxide electrical contact material having oxide particles dispersed therein according to claim 1, characterized in that: the internal oxidation process in the step (6) comprises the following steps: the oxidation temperature is 600-850 ℃, and the oxidation time is as follows: 24-48 h, oxidation pressure: 0.4-0.95 MPa, and finally performing punching, ingot pressing, sintering, re-pressing and further hot extrusion on the internally oxidized strip to obtain a plate or wire.
9. An oxide particle dispersion-distributed silver iron oxide electrical contact material prepared by the preparation method according to claim 1, characterized in that: the ferroelectric oxide contact material comprises 5-15 wt% of ferric oxide, 0.01-2 wt% of modified additive and the balance of silver, wherein the modified additive is one or more of molybdenum oxide, yttrium oxide and lanthanum oxide, the size of oxide particles is less than or equal to 1 mu m, and the maximum size of aggregated oxide particles in the metallographic structure of the whole transverse and longitudinal sections of a finished wire or plate is less than or equal to 5 mu m.
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