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CN113488354A - Silver tin oxide electric contact material and preparation method thereof - Google Patents

Silver tin oxide electric contact material and preparation method thereof Download PDF

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Publication number
CN113488354A
CN113488354A CN202110586650.9A CN202110586650A CN113488354A CN 113488354 A CN113488354 A CN 113488354A CN 202110586650 A CN202110586650 A CN 202110586650A CN 113488354 A CN113488354 A CN 113488354A
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alloy
wire
tin oxide
contact material
temperature
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Inventor
陈杨方
李�杰
颜小芳
柏小平
张明江
杨昌麟
陈松扬
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Zhejiang Fuda Alloy Materials Technology Co Ltd
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Fuda Alloy Materials Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H49/00Apparatus or processes specially adapted to the manufacture of relays or parts thereof
    • 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
    • C22C32/0021Matrix based on noble metals, Cu or alloys thereof
    • CCHEMISTRY; METALLURGY
    • 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
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10Oxidising
    • C23C8/12Oxidising using elemental oxygen or ozone
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/021Composite material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H50/00Details of electromagnetic relays
    • H01H50/54Contact arrangements

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Contacts (AREA)
  • Manufacture Of Switches (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a preparation method of a silver tin oxide electric contact material, which comprises the following steps: firstly, preparing an AgSn alloy spindle by utilizing one or more of Ag ingot, Sn, In, Cu, Co, Li, Ni and rare earth, then turning a surface skin, heating and extruding into a wire material, drawing to the diameter of 2.0mm, shearing into a short wire, dynamically oxidizing internally, pressing into an ingot, sintering, hot extrusion, drawing and the like, and finally preparing a finished wire material. The invention has the advantages that: through using the vacuum suspension smelting technique in the smelting process to and use dynamic internal oxidation technique, make the material each part be heated evenly in smelting the process, alloy melt does not take place the contact with the crucible simultaneously, smelt the mode with the tradition and compare, the alloy ingot composition that obtains is more even, and no segregation produces, has avoided the alumina that brings in the traditional smelting furnace simultaneously, and the silica impurity reuses dynamic internal oxidation technique, has shortened the internal oxidation time, has promoted the production efficiency of material.

Description

Silver tin oxide electric contact material and preparation method thereof
Technical Field
The invention belongs to the field of manufacturing of electrical materials, and particularly relates to a silver tin oxide electrical contact material and a preparation method thereof.
Background
Silver-based electrical contact materials have excellent electrical and thermal conductivity, and due to the low hardness and poor resistance to electrical wear of pure silver, it is usually necessary to add other additives to the silver matrix to enhance the electrical properties of the material, such as the welding resistance, electrical life, and resistance to arc burning of the contacts. Silver tin oxide (AgSnO)2) The silver-based electric contact material has better fusion welding resistance and burning resistance, and can be applied to relays and contactor switches with large current.
Preparation of AgSnO currently2The main methods of the electric contact material include an alloy internal oxidation method and an atomization method, wherein the alloy internal oxidation method prepares the electric contact material by alloy smelting and alloy oxidation, but because the defects of component segregation, inclusion, oxide aggregation and the like cannot be avoided in the traditional internal oxidation process during the preparation of alloy melt and the internal oxidation, the distribution condition of oxide particles of the prepared material has certain problems in the metallographic phase, and the production process is longer, the atomization process atomizes the alloy melt into powder by air or cooling water, the alloy oxide powder is prepared by the powder preoxidation and high-temperature oxidation processes, and the powder is finally pressed and molded to prepare the electric contact material, the atomization process also has long production process, and the oxide exists in the metallographic phase of the materialThe problems of aggregation, some alumina and silicon oxide inclusion and the like cause the wire to be broken during processing, and the wire is cracked during cold heading forming of a contact rivet, so that the service performance of the material is influenced.
Therefore, there is a need for an improved process for preparing silver-based electrical contact materials to overcome the above-mentioned problems.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art, and provides a silver tin oxide electric contact material and a preparation method thereof.
The technical scheme of the invention is to provide a preparation method of a silver tin oxide electric contact material, which comprises the following steps:
(1) preparing an AgSn alloy ingot: processing Ag, Sn and one or more of In, Cu, Co, Li, Ni and rare earth into alloy melt by a vacuum suspension smelting process, heating and pouring the alloy melt into a mold to form an alloy blank, and treating a layer of oxide skin on the surface of the alloy blank for later use;
(2) carrying out hot extrusion molding on the alloy blank obtained in the step (1) to obtain an alloy wire, wherein the heating temperature of the hot extrusion is 700-800 ℃, and hydrogen is used for protection in the heating process;
(3) drawing and cutting: drawing the alloy wire obtained in the step (2) into an alloy wire with a smaller diameter, and cutting the alloy wire into wire segments with the diameter of 10-15 mm;
(4) internal oxidation: placing the cut small sections of the wire material into a preheated liner of a high-temperature oxidation furnace, introducing oxygen after the material is loaded, starting the high-temperature oxidation furnace, keeping the oxygen pressure at 0.2-0.8MPa at the temperature of 650 plus materials of 800 ℃ for 10-30h, starting a liner rotary switch in the heat preservation process, turning over the wire sections by using a stirrer arranged in the liner, ensuring that the wire sections at all parts are uniformly heated and contacted with the oxygen, preventing the occurrence of nonuniform oxidation and bonding phenomena among the wire sections, and finally taking out the material after the oxidation is finished;
(5) and (3) ingot pressing and sintering: pressing the oxidized material obtained in the step (4) into a spindle, and sintering the material by using a high-temperature sintering furnace at the sintering temperature of 800-900 ℃ for 8-10 hours;
(6) extruding: heating the spindle sintered in the step (5) at the temperature of 700-;
(7) drawing; and (4) further drawing the semi-finished wire product obtained in the step (6) into a finished wire product with smaller diameter by a medium-frequency drawing machine according to a drawing process.
Further setting the steps that in the step (1), the raw materials are smelted by using vacuum suspension smelting equipment to obtain the alloy solution, wherein the power supply power is 100-.
The further setting is that the prepared silver tin oxide electric contact material comprises the components of, by weight, Ag 85-92 wt.%, SnO2 5~10wt.%,CuO 0.5~1wt.%,In2O3 1.5~4.5wt.%,Li2O 0.5-1wt%,Ni2O and rare earth element La2O30.5~1.5wt.%。
The method is further provided that the alloy blank in the step (1) and the spindle in the step (5) are both cylindrical in shape.
A second aspect of the present invention is to provide a silver tin oxide electrical contact material prepared by the above method.
The further setting is that the components of the alloy comprise, by weight, Ag 85-92 wt.%, SnO2 5~10wt.%,CuO 0.5~1wt.%,In2O3 1.5~4.5wt.%,Li2O 0.5-1wt%,Ni2O and rare earth element La2O30.5~1.5wt.%。
The invention has the advantages that:
the invention uses vacuum suspension smelting technique and rotary dynamic internal oxidation technique, the alloy solution is in suspension state by electromagnetic force, the alloy solution does not contact with the crucible, avoids the pollution of the material in the crucible to the alloy solution in the traditional smelting technique, leads the wire to be broken in processing, and the problem of cracking in contact rivet cold heading forming, influences the use performance of the material, changes the hump value by adjusting the distribution of the electromagnetic field in smelting, realizes the stirring function of the alloy solution in smelting, and fully fuses all the components, uses a rotary device to turn over the material in the internal oxidation process, uniformly heats all the components, fully reacts with oxygen, reduces the oxide aggregation in the material gold phase (as shown in figure 1), and the service life of the prepared electric contact material reaches more than 10 ten thousand times under certain current condition, has better fusion welding resistance and burning loss resistance.
The silver tin oxide material prepared by the invention has the advantages that the oxide particles are uniformly distributed, no oxide aggregation exists in the metallographic phase, no stress concentration phenomenon exists in the material processing, the material has better processing performance, and under the two technologies, the prepared rivet type contact shows better electric service life under the conditions of alternating current and direct current.
Drawings
FIG. 1 shows a gold phase diagram of a material by a conventional process and a process according to an embodiment of the present invention, wherein the left diagram is a conventional process and the right diagram is a process according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the following examples.
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 below.
A method for manufacturing a silver tin oxide electric contact material comprises the following steps:
(1) preparing an AgSn alloy ingot: the glass was manufactured In a 1 furnace of 25kg, In which 85 wt.% of an Ag plate and 9 wt.% of an Sn plate, 0.5 wt.% of Cu, 3.9 wt.% of In, 0.6 wt.% of Li, 1 wt.% of NiO and rare earth element La were charged. Smelting in a vacuum suspension smelting furnace, wherein the smelting temperature is set to 1200 ℃, the hump value is 2.0, the smelting time is 0.5h, the stirring purpose is realized by adjusting the electromagnetic field distribution in the smelting process, and then the temperature is reduced to 1150 ℃ for refining for 14 min.
(2) AgSn extrusion: and (3) forming the alloy blank prepared in the previous step into a wire rod with the diameter of 6.0mm by using a hot extrusion machine, wherein the heating temperature is 700 ℃, and hydrogen is used for protection in the heating process.
(3) Drawing and cutting: drawing the alloy wire obtained in the step (2) to the diameter of 2.0mm, and cutting the wire into small sections of 10-15mm by using a punch;
(4) internal oxidation: putting the cut materials into a preheated liner of a high-temperature oxidation furnace, introducing oxygen after the materials are loaded, starting the high-temperature oxidation furnace, keeping the temperature at 650 ℃ for 30h under the oxygen pressure of 0.8MPa, starting a liner rotary switch in the heat preservation process, turning over the wire sections by using a stirrer arranged in the liner, ensuring that the wire sections at all parts are uniformly heated and contact with the oxygen, preventing the occurrence of nonuniform oxidation and bonding between the wire sections, and taking out the materials after the materials are finally oxidized to prepare for the next process;
(5) pressing ingots and sintering: pressing the oxidized material into a cylindrical spindle by using a hydraulic press, and sintering by using a high-temperature sintering furnace at 850 ℃ for 10 hours to obtain higher compactness;
(6) extruding: the sintered AgSnO2Heating the spindle at 800 ℃ for 3 hours, and then forming the wire into a phi 6mm specification by using an extruder;
(7) drawing: according to the drawing process, drawing the wire with the diameter of 6mm into the wire with the diameter of 1.9mm by a medium-frequency wire drawing machine.
The drawing process comprises the following steps:
Φ6.0Δ→→Φ5.6→→Φ5.2→→Φ4.9Δ→→Φ4.5→→Φ4.2→→Φ3.9Δ→→Φ3.6→→Φ3.4→→Φ3.2Δ→→Φ3.0→→Φ2.8→→Φ2.5→→Φ2.4Δ→→Φ2.2Δ→→Φ2.0→→Φ1.9Δ
Δ represents annealing, annealing temperature: keeping the temperature at 600 ℃ for 3h, and annealing in air. "→ →" represents the drawing.
The process parameters of the wire drawing machine in the drawing process are wire drawing speed of 200-800 rpm.
Example 2:
the difference from example 1 was that, In the case of the charge of raw materials having different contents, 88.5 wt.% Ag plate and 7.5 wt.% Sn plate, Cu 0.5 wt.%, In 2.4 wt.%, Li 0.6 wt.%, NiO and rare earth element La 0.5 wt.% were charged In accordance with the configuration of 1 furnace of 25kg
Example 3:
the difference from example 1 and example 2 is that the raw materials are charged in different amounts, and the preparation is carried out according to 1 furnace of 25kg, 86.5 wt.% Ag plate and 9.5 wt.% Sn plate, Cu 0.5 wt.%, In1.9wt.%, Li 0.6 wt.%, NiO and rare earth element La 1 wt.%.
The AgSnO is prepared by the method2A simulated electrical property experiment is carried out on a/Cu rivet contact, and the specifications of the rivet are moving contact R4.0x1.4(0.5) +2.5x1.2SR15 and static contact F4x1.4(0.5) +2.5x 1.2. The experimental conditions for simulating the electrical properties are as follows: 250VAC, 5A, closing force of 100g, breaking force of 60g and contact frequency of 90 times/min; 20VDC, 9A, 100g closing force, 50g breaking force and 90 contact frequencies/min, and the experimental results are shown in Table 1.
In particular, the contact material used in the comparative example was manufactured by a conventional contact material internal oxidation process, and was processed into a rivet of the same specification to perform an electrical property test.
TABLE 1 parameter settings and test results for various examples and comparative examples
Figure BDA0003087827840000051
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.

Claims (6)

1. The preparation method of the silver tin oxide electric contact material is characterized by comprising the following steps:
(1) preparing an AgSn alloy ingot: processing Ag, Sn and one or more of In, Cu, Co, Li, Ni and rare earth into alloy melt by a vacuum suspension smelting process, heating and pouring the alloy melt into a mold to form an alloy blank, and treating a layer of oxide skin on the surface of the alloy blank for later use;
(2) carrying out hot extrusion molding on the alloy blank obtained in the step (1) to obtain an alloy wire, wherein the heating temperature of the hot extrusion is 700-800 ℃, and hydrogen is used for protection in the heating process;
(3) drawing and cutting: drawing the alloy wire obtained in the step (2) into an alloy wire with a smaller diameter, and cutting the alloy wire into wire segments with the diameter of 10-15 mm;
(4) internal oxidation: placing the cut small sections of the wire material into a preheated liner of a high-temperature oxidation furnace, introducing oxygen after the material is loaded, starting the high-temperature oxidation furnace, keeping the oxygen pressure at 0.2-0.8MPa at the temperature of 650 plus materials of 800 ℃ for 10-30h, starting a liner rotary switch in the heat preservation process, turning over the wire sections by using a stirrer arranged in the liner, ensuring that the wire sections at all parts are uniformly heated and contacted with the oxygen, preventing the occurrence of nonuniform oxidation and bonding phenomena among the wire sections, and finally taking out the material after the oxidation is finished;
(5) and (3) ingot pressing and sintering: pressing the oxidized material obtained in the step (4) into a spindle, and sintering the material by using a high-temperature sintering furnace at the sintering temperature of 800-900 ℃ for 8-10 hours;
(6) extruding: heating the spindle sintered in the step (5) at the temperature of 700-;
(7) drawing; and (4) further drawing the semi-finished wire product obtained in the step (6) into a finished wire product with smaller diameter by a medium-frequency drawing machine according to a drawing process.
2. The method for preparing a silver tin oxide electrical contact material according to claim 1, characterized in that: in the step (1), the raw material is smelted by using vacuum suspension smelting equipment to obtain the alloy solution, wherein the power supply power is 100-.
3. Silver oxide according to claim 1The preparation method of the tin-plated electric contact material is characterized by comprising the following steps: the prepared silver tin oxide electrical contact material comprises, by weight, 85-92 wt.% of Ag and SnO2 5~10wt.%,CuO 0.5~1wt.%,In2O3 1.5~4.5wt.%,Li2O 0.5-1wt%,Ni2O and rare earth element La2O30.5~1.5wt.%。
4. The method for preparing a silver tin oxide electrical contact material according to claim 1, characterized in that: the shape of the alloy blank in the step (1) and the shape of the spindle in the step (5) are both cylindrical.
5. A silver tin oxide electrical contact material prepared by the preparation method according to claim 1.
6. The silver tin oxide electrical contact material of claim 5, wherein: the components of the alloy comprise, by weight, Ag 85-92 wt.%, SnO2 5~10wt.%,CuO 0.5~1wt.%,In2O31.5~4.5wt.%,Li2O 0.5-1wt%,Ni2O and rare earth element La2O30.5~1.5wt.%。
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CN114086020A (en) * 2021-10-28 2022-02-25 浙江福达合金材料科技有限公司 Preparation method of silver tin oxide electric contact material based on spontaneous thermal oxidation process and product thereof
CN114093698A (en) * 2021-10-28 2022-02-25 浙江福达合金材料科技有限公司 Silver tin oxide electric contact material and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114086020A (en) * 2021-10-28 2022-02-25 浙江福达合金材料科技有限公司 Preparation method of silver tin oxide electric contact material based on spontaneous thermal oxidation process and product thereof
CN114093698A (en) * 2021-10-28 2022-02-25 浙江福达合金材料科技有限公司 Silver tin oxide electric contact material and preparation method thereof
CN114086020B (en) * 2021-10-28 2022-06-14 浙江福达合金材料科技有限公司 Preparation method of silver tin oxide electric contact material based on spontaneous thermal oxidation process and product thereof

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