CN112355323A - Ultrafine oxide particle silver ferric oxide electric contact material and preparation method thereof - Google Patents

Ultrafine oxide particle silver ferric oxide electric contact material and preparation method thereof Download PDF

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CN112355323A
CN112355323A CN202011059044.3A CN202011059044A CN112355323A CN 112355323 A CN112355323 A CN 112355323A CN 202011059044 A CN202011059044 A CN 202011059044A CN 112355323 A CN112355323 A CN 112355323A
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silver
oxide
metal salt
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CN112355323B (en
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杨昌麟
张秀芳
颜小芳
周克武
林应涛
曹庆
柏小平
张明江
陈松扬
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Zhejiang Fuda Alloy Materials Technology Co Ltd
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    • B22F9/30Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/06Alloys based on silver
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
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    • H01H1/023Composite material having a noble metal as the basic material
    • H01H1/0237Composite material having a noble metal as the basic material and containing oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/021Composite material
    • H01H1/023Composite material having a noble metal as the basic material
    • H01H1/0237Composite material having a noble metal as the basic material and containing oxides
    • H01H2001/02378Composite material having a noble metal as the basic material and containing oxides containing iron-oxide as major component

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Abstract

The invention discloses an ultrafine oxide particle silver ferric oxide electric contact material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) preparing composite metal salt precursor powder, uniformly mixing metal salt solution, and then preparing the composite metal salt precursor powder from the metal salt solution with the adjusted pH on spray drying equipment; (2) carrying out stepped heating calcination decomposition on the composite metal salt precursor powder prepared in the step (1) to prepare silver oxide composite powder, wherein the silver oxide composite powder contains ultrafine oxide particles; (3) and (3) carrying out cold isostatic pressing, sintering, repressing and hot extrusion on the silver oxide composite powder prepared in the step (2) to obtain the plate or wire of the ultrafine oxide particle silver iron oxide electric contact material. The scheme can realize uniform dispersion and superfine particle size of oxide particles, and ensures that low-melting-point metal impurities are not introduced in the preparation process of the material.

Description

Ultrafine oxide particle silver ferric oxide electric contact material and preparation method thereof
Technical Field
The invention belongs to the technical field of electrical contact materials, and particularly relates to an ultrafine oxide particle silver ferric oxide electrical contact material 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.
Due to the limited solid solubility between silver and iron, the common preparation processes for silver iron oxide electrical contact materials are classified into two types: powder metallurgy process, chemical codeposition process. The powder metallurgy process for preparing silver iron oxide is briefly 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 by codeposition process is 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 publication No. CN101794636 discloses a method for preparing a silver iron oxide electrical 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 electrical property process, and the 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 an ultrafine oxide particle silver iron oxide electric contact material and a preparation method thereof. The scheme can realize uniform dispersion and superfine particle size of oxide particles, and ensures that low-melting-point metal impurities are not introduced in the preparation process of the material.
In order to achieve the above object, a first technical means of the present invention is to provide a method for preparing an ultrafine oxide particle silver iron oxide electrical contact material, comprising the steps of:
(1) preparing composite metal salt precursor powder: preparing a metal salt solution, wherein the metal salt solution comprises a silver nitrate solution, an iron nitrate solution and one or more solutions of molybdenum nitrate, yttrium nitrate and lanthanum nitrate; uniformly mixing the metal salt solution, and adjusting the pH value of the solution to be between 5 and 10 by using ammonia water; then preparing composite metal salt precursor powder from the metal salt solution with the adjusted pH value on spray drying equipment;
(2) carrying out stepped heating calcination decomposition on the composite metal salt precursor powder prepared in the step (1), and decomposing silver oxide into silver to obtain composite powder of silver and other component metal oxides, and marking the composite powder as silver oxide composite powder, wherein the silver oxide composite powder contains ultrafine oxide particles; because of the high temperature instability of silver oxide, the silver oxide can be decomposed into simple substance silver at the temperature of more than 300 ℃, so that the simple substance silver is generated by subsequent step temperature calcination (the other component metal oxides are high temperature stability and still exist in the most stable oxide form in the calcination process), and finally the powder formed after the high temperature calcination is determined to be silver oxide powder. In the step, a proper amount of ammonia water is added for mainly adjusting the pH of the solution, so that the corrosion of an acidic medium to equipment is avoided, and the purpose of protecting the equipment is achieved.
(3) And (3) carrying out cold isostatic pressing, sintering, repressing and hot extrusion on the silver oxide composite powder prepared in the step (2) to obtain the plate or wire of the ultrafine oxide particle silver iron oxide electric contact material.
Further setting the initial concentration of the silver nitrate solution in the step (1) to be 0.1-1.5 mol/L, the initial concentration of the ferric nitrate solution to be 0.1-1.5 mol/L, the initial solubility of the adopted molybdenum nitrate solution, yttrium nitrate or lanthanum nitrate solution to be 0.05-0.5 mol/L and the initial concentration of the ammonia water solution to be 0.5-5 mol/L.
Further setting that ammonia water is adopted to adjust the pH value of the metal salt solution to be 5-10 in the step (1).
The further setting is that the step of preparing the precursor powder of the composite metal salt on the spray drying equipment in the step (1) is specifically as follows:
a) feeding the metal salt solution with the adjusted pH value into an atomizer arranged at the top of a spray drying device by using a feeding pump, wherein the feeding amount of the feeding pump is set to be 1-3L/min;
b) setting the rotating speed of the high-speed centrifugal atomizer to 10000-;
c) and setting the drying temperature of spray drying equipment, controlling the temperature of an air inlet to be 200-250 ℃ and the temperature of an air outlet to be 70-80 ℃, drying and dehydrating the droplets of the metal salt solution, and finally preparing the composite metal salt precursor powder.
The method is further characterized in that the composite metal salt precursor powder in the step (2) is decomposed by stepped heating calcination, and the stepped heating process route is as follows: keeping the temperature at 250 deg.C for 120min, keeping the temperature at 450 deg.C for 180min, keeping the temperature at 600 deg.C for 120min, and keeping the temperature at 800 deg.C for 120 min. The main purpose of adopting the step heating is to slow down the decomposition speed of metal salt particles and avoid the abnormal splashing of a large amount of gas generated due to overhigh temperature to powder particles;
further setting the isostatic pressure of the silver oxide composite powder in the step (3) to be 120-220 MPa and the diameter of the isostatic pressing rubber sleeve
Figure BDA0002711697500000041
The sintering process in the step (3) is further set as follows: the sintering temperature is 800-935 ℃, the heat preservation time is 2-8 h, and the sintering atmosphere is air.
Further setting the repressing pressure in the step (3) to be 16-24 MPa and the pressure maintaining time to be 10-30 s; the heating process of the hot extrusion spindle comprises the following steps: the heating temperature is 600-850 ℃, and the heat preservation time is 1.5-4.5 h.
In addition, the invention also provides an ultrafine oxide particle silver iron oxide electric contact material prepared by the preparation method, which comprises the following components: the silver iron oxide material prepared by the method has the oxide particle size of 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 the finished wire or plate is less than or equal to 5 mu m.
The innovative mechanism of the invention is as follows:
1) because of the high temperature instability of silver oxide, the silver oxide can be decomposed into simple substance silver at the temperature of more than 300 ℃, so that the simple substance silver is generated by subsequent step temperature calcination (the other component metal oxides are high temperature stability and still exist in the most stable oxide form in the calcination process), and finally the powder formed after the high temperature calcination is determined to be silver oxide powder. In the step, a proper amount of ammonia water is added for mainly adjusting the pH of the solution, so that the corrosion of an acidic medium to equipment is avoided, and the purpose of protecting the equipment is achieved.
The invention has the following beneficial effects:
1) the mixed metal salt solution is adopted, and all metal elements reach the atomic level mixing level, so that the uniformity of oxide dispersion in the subsequent silver composite oxide powder is ensured to the maximum extent;
2) compared with the conventional powder metallurgy process, the method can fundamentally eliminate the agglomeration defect of the oxide powder, and the prepared oxide particles are fine;
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) the weight percentage of Ag to Fe2O3:MoO3Preparing silver nitrate solution and nitric acid (total weight is 10kg) 93.6:5.4:1Iron solution and molybdenum nitrate solution. According to the requirements of the total weight and the weight percentage, 72.23L of silver nitrate solution with the initial solution solubility of 1.2mol/L, 13.5L of ferric nitrate solution with the initial solution solubility of 0.5mol/L, 6.94L of molybdenum nitrate solution with the initial solution solubility of 0.1mol/L and 50L of ammonia water solution with the initial solubility of 0.6mol/L are prepared.
2) And uniformly mixing the prepared silver nitrate solution, ferric nitrate solution and molybdenum nitrate solution, and adjusting the pH value of the mixed solution to 7.5 by using the prepared ammonia water solution.
3) Preparing composite metal salt precursor powder from the PH-adjusted metal salt solution on spray drying equipment, which comprises the following specific implementation steps:
a) the metal salt solution with the adjusted pH value is sent to an atomizer arranged at the top of the spray drying equipment by a feeding pump, and the feeding amount of the feeding pump is set to be 2L/min;
b) setting the rotating speed of a high-speed centrifugal atomizer to 15000rpm, and carrying out high-speed centrifugal atomization on the liquid material to form fog drops;
c) and setting the drying temperature of spray drying equipment, controlling the temperature of an air inlet at 230 ℃ and the temperature of an air outlet at 70 ℃, and preparing the composite metal salt precursor powder.
4) Keeping the metal salt precursor powder at 250 deg.C for 120min, 450 deg.C for 180min, 600 deg.C for 120min, and finally 800 deg.C for 120min to prepare silver metal oxide powder
5) Isostatic pressing of silver metal oxide powder in a cold isostatic press: isostatic pressure is 180MPa, and isostatic rubber sleeve diameter adopts
Figure BDA0002711697500000061
Sintering the isostatic pressed spindle in an air atmosphere: the sintering temperature is 920 ℃, and the sintering time is 6 hours; re-pressing the sintered spindle: the repressing pressure is 20MPa, and the pressure maintaining time is 20 s; and finally, heating the re-pressed spindle to 830 ℃, and extruding the re-pressed spindle into a plate or wire after heat preservation for 2 hours. AgFe prepared by adopting the process2O3(5.4%)MoO3(1%) wire was subsequently drawn to
Figure BDA0002711697500000071
The physical and mechanical performance indexes of the finished wire are as follows:
Figure BDA0002711697500000072
example two:
the implementation case is carried out according to the following steps:
1) the weight percentage of Ag to Fe2O3:Y2O3A silver nitrate solution, an iron nitrate solution, and an yttrium nitrate solution were prepared in a ratio of 93.6:5.4:1 (total weight: 10 kg). According to the requirements of the total weight and the weight percentage, 72.23L of silver nitrate solution with the initial solution solubility of 1.2mol/L, 13.5L of ferric nitrate solution with the initial solution solubility of 0.5mol/L, 8.85L of yttrium nitrate solution with the initial solution solubility of 0.1mol/L and 50L of ammonia water solution with the initial solubility of 0.6mol/L are prepared.
2) And uniformly mixing the prepared silver nitrate solution, ferric nitrate solution and yttrium nitrate solution, and adjusting the pH value of the mixed solution to 7.5 by using the prepared ammonia water solution.
3) Preparing composite metal salt precursor powder from the metal salt solution subjected to pH adjustment on spray drying equipment, which comprises the following specific implementation steps:
a) the metal salt solution with the adjusted pH value is sent to an atomizer arranged at the top of the spray drying equipment by a feeding pump, and the feeding amount of the feeding pump is set to be 2L/min;
b) setting the rotating speed of a high-speed centrifugal atomizer to 15000rpm, and carrying out high-speed centrifugal atomization on the liquid material to form fog drops;
c) and setting the drying temperature of spray drying equipment, controlling the temperature of an air inlet at 230 ℃ and the temperature of an air outlet at 70 ℃, and preparing the composite metal salt precursor powder.
4) Keeping the metal salt precursor powder at 250 deg.C for 120min, 450 deg.C for 180min, 600 deg.C for 120min, and finally 800 deg.C for 120min to prepare silver metal oxide powder
5) Subjecting silver metal oxide powder to cold isostatic pressingThe equipment carries out isostatic pressing: isostatic pressure is 180MPa, and isostatic rubber sleeve diameter adopts
Figure BDA0002711697500000082
Sintering the isostatic pressed spindle in an air atmosphere: the sintering temperature is 920 ℃, and the sintering time is 6 hours; re-pressing the sintered spindle: the repressing pressure is 20MPa, and the pressure maintaining time is 20 s; and finally, heating the re-pressed spindle to 830 ℃, and extruding the re-pressed spindle into a plate or wire after heat preservation for 2 hours. AgFe prepared by adopting the process2O3(5.4%)Y2O3(1%) wire was subsequently drawn to
Figure BDA0002711697500000083
The physical and mechanical performance indexes of the finished wire are as follows:
Figure BDA0002711697500000081
example three:
the implementation case is carried out according to the following steps:
1) the weight percentage of Ag to Fe2O3:La2O3A silver nitrate solution, an iron nitrate solution, and a lanthanum nitrate solution were prepared at a ratio of 93.6:5.4:1 (total weight: 10 kg). According to the requirements of the total weight and the weight percentage, 72.23L of silver nitrate solution with the initial solution solubility of 1.2mol/L, 13.5L of ferric nitrate solution with the initial solution solubility of 0.5mol/L, 6.15L of lanthanum nitrate solution with the initial solution solubility of 0.1mol/L and 50L of ammonia water solution with the initial solution solubility of 0.6mol/L are prepared.
2) And uniformly mixing the prepared silver nitrate solution, ferric nitrate solution and lanthanum nitrate solution, and adjusting the pH value of the mixed solution to 7.5 by using the prepared ammonia water solution.
3) Preparing composite metal salt precursor powder from the pH-adjusted metal salt solution on spray drying equipment, which comprises the following specific implementation steps:
a) the metal salt solution with the adjusted pH value is sent to an atomizer arranged at the top of the spray drying equipment by a feeding pump, and the feeding amount of the feeding pump is set to be 2L/min;
b) setting the rotating speed of a high-speed centrifugal atomizer to 15000rpm, and carrying out high-speed centrifugal atomization on the liquid material to form fog drops;
c) and setting the drying temperature of spray drying equipment, controlling the temperature of an air inlet at 230 ℃ and the temperature of an air outlet at 70 ℃, and preparing the composite metal salt precursor powder.
4) Preserving heat of the metal salt precursor powder at 250 ℃ for 120min, preserving heat at 450 ℃ for 180min, preserving heat at 600 ℃ for 120min, and finally preserving heat at 800 ℃ for 120min to prepare silver metal oxide powder;
5) isostatic pressing of silver metal oxide powder in a cold isostatic press: isostatic pressure is 180MPa, and isostatic rubber sleeve diameter adopts
Figure BDA0002711697500000093
Sintering the isostatic pressed spindle in an air atmosphere: the sintering temperature is 920 ℃, and the sintering time is 6 hours; re-pressing the sintered spindle: the repressing pressure is 20MPa, and the pressure maintaining time is 20 s; and finally, heating the re-pressed spindle to 830 ℃, and extruding the re-pressed spindle into a plate or wire after heat preservation for 2 hours. AgFe prepared by adopting the process2O3(5.4%)La2O3(1%) wire was subsequently drawn to
Figure BDA0002711697500000091
The physical and mechanical performance indexes of the finished wire are as follows:
Figure BDA0002711697500000092
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 ultrafine oxide particle silver ferric oxide electric contact material is characterized by comprising the following steps:
(1) preparing composite metal salt precursor powder: preparing a metal salt solution, wherein the metal salt solution comprises a silver nitrate solution, an iron nitrate solution and one or more solutions of molybdenum nitrate, yttrium nitrate and lanthanum nitrate; uniformly mixing the metal salt solution, and adjusting the pH value of the solution to be between 5 and 10 by using ammonia water; then preparing composite metal salt precursor powder from the metal salt solution with the adjusted pH value on spray drying equipment;
(2) carrying out stepped heating calcination decomposition on the composite metal salt precursor powder prepared in the step (1), and decomposing silver oxide into silver to obtain composite powder of silver and other component metal oxides, and marking the composite powder as silver oxide composite powder, wherein the silver oxide composite powder contains ultrafine oxide particles;
(3) and (3) carrying out cold isostatic pressing, sintering, repressing and hot extrusion on the silver oxide composite powder prepared in the step (2) to obtain the plate or wire of the ultrafine oxide particle silver iron oxide electric contact material.
2. The method for preparing an ultrafine oxide particle silver iron oxide electrical contact material according to claim 1, characterized in that: in the step (1), the initial concentration of the silver nitrate solution is 0.1-1.5 mol/L, the initial concentration of the ferric nitrate solution is 0.1-1.5 mol/L, the initial solubility of the adopted molybdenum nitrate solution, yttrium nitrate or lanthanum nitrate solution is 0.05-0.5 mol/L, and the initial concentration of the ammonia water solution is 0.5-5 mol/L.
3. The method for preparing an ultrafine oxide particle silver iron oxide electrical contact material according to claim 1, characterized in that: and (1) adjusting the pH value of the metal salt solution to 5-10 by adopting ammonia water.
4. The method for preparing an ultrafine oxide particle silver iron oxide electrical contact material according to claim 1, characterized in that: the step of preparing the composite metal salt precursor powder on the spray drying equipment in the step (1) specifically comprises the following steps:
a) feeding the metal salt solution with the adjusted pH value into an atomizer arranged at the top of a spray drying device by using a feeding pump, wherein the feeding amount of the feeding pump is set to be 1-3L/min;
b) setting the rotating speed of the high-speed centrifugal atomizer to 10000-;
c) and setting the drying temperature of spray drying equipment, controlling the temperature of an air inlet to be 200-250 ℃ and the temperature of an air outlet to be 70-80 ℃, drying and dehydrating the droplets of the metal salt solution, and finally preparing the composite metal salt precursor powder.
5. The method for preparing an ultrafine oxide particle silver iron oxide electrical contact material according to claim 1, characterized in that: the composite metal salt precursor powder in the step (2) is decomposed by stepped heating calcination, and the stepped heating process route is as follows: keeping the temperature at 250 deg.C for 120min, keeping the temperature at 450 deg.C for 180min, keeping the temperature at 600 deg.C for 120min, and keeping the temperature at 800 deg.C for 120 min.
6. The method for preparing an ultrafine oxide particle silver iron oxide electrical contact material according to claim 1, characterized in that: the isostatic pressure of the silver oxide composite powder in the step (3) is 120-220 MPa, and the diameter of the isostatic pressing rubber sleeve
Figure 1
7. The method for preparing an ultrafine oxide particle silver iron oxide electrical contact material according to claim 1, characterized in that: the sintering process in the step (3) comprises the following steps: the sintering temperature is 800-935 ℃, the heat preservation time is 2-8 h, and the sintering atmosphere is air.
8. The method for preparing an ultrafine oxide particle silver iron oxide electrical contact material according to claim 1, characterized in that: in the step (3), the repressing pressure is 16-24 MPa, and the pressure maintaining time is 10-30 s; the heating process of the hot extrusion spindle comprises the following steps: the heating temperature is 600-850 ℃, and the heat preservation time is 1.5-4.5 h.
9. An ultrafine oxide particle silver iron oxide electrical contact material prepared by the preparation method according to claim 1, characterized by comprising the following components: the wire or plate comprises 5-15 wt% of iron oxide, 0.01-2 wt% of modified additive and the balance of silver, wherein the modified additive is one or a combination 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 the finished wire or plate is less than or equal to 5 mu m.
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