CN111118332A - Dynamic internal oxidation method for silver-based metal oxide electrical contact material - Google Patents
Dynamic internal oxidation method for silver-based metal oxide electrical contact material Download PDFInfo
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- CN111118332A CN111118332A CN201911365273.5A CN201911365273A CN111118332A CN 111118332 A CN111118332 A CN 111118332A CN 201911365273 A CN201911365273 A CN 201911365273A CN 111118332 A CN111118332 A CN 111118332A
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- silver
- internal oxidation
- wire
- ingot
- electrical contact
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
- B21C37/047—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire of fine wires
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
Abstract
The invention discloses a dynamic internal oxidation method of a silver-based metal oxide electrical contact material, which comprises the following steps of: firstly, preparing an AgZn alloy spindle, then turning a surface skin, extruding into wires, drawing to 2.0mm, punching into broken wires, rolling and oxidizing the broken wires, pressing into ingots, sintering, extruding, drawing and the like, and finally preparing the finished wire. The invention can obtain the following technical effects: the oxidation treatment is carried out on the alloy wire section by adopting the rolling type oxidation process, the production period of internal oxidation can be shortened, the original 1-day time is changed into 8-10 hours, the oxidation is uniform in the oxidation process, no oxide is accumulated, and the oxygen is thoroughly permeated.
Description
Technical Field
The invention belongs to the field of electrical materials, and particularly relates to a dynamic internal oxidation method for a silver-based metal oxide electrical contact material.
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 zinc oxide (AgZnO) is a widely applied material in silver-based electric contact materials, has better fusion welding resistance and burning resistance, and can be applied to relays and circuit breaker switches with medium and small currents. At present, the main methods for preparing AgZnO include a powder metallurgy method, an alloy internal oxidation method and an atomization process. The traditional method is characterized in that the bottom and the upper part of the material boat are heated differently, and the material section is not fully contacted with oxygen at the bottom of the material boat, so that an oxide aggregation phenomenon can be formed, and the electrical property of the material is influenced. There is therefore a need for improvements to existing internal oxidation processes.
Disclosure of Invention
In order to solve the problems and the defects in the prior art, the invention aims to provide a dynamic internal oxidation method of a silver-based metal oxide electric contact material, which can shorten the production time, improve the material performance and obtain the electric contact material with better electrical performance.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps:
(1) preparing a smelting alloy ingot, namely smelting to form the silver metal alloy ingot according to a formula of a silver-based metal oxide electrical contact material, wherein metal alloy components in the silver metal alloy ingot are other metals except silver and additives;
(2) turning the surface of a silver metal alloy ingot and processing the silver metal alloy ingot into a silver metal alloy wire;
(3) drawing and cutting: drawing the silver metal alloy wire into a filament shape, and then cutting the filament into small sections to obtain silver metal alloy cutting sections;
(4) dynamic internal oxidation: putting the silver metal alloy cutting section below a rotating shaft in a high-temperature internal oxidation furnace, introducing oxygen, starting the high-temperature internal oxidation furnace, heating to 700-780 ℃ for 8-10 hours, starting the internal rotating shaft during heating, uniformly heating the material section in the rotating process, turning over the material section at the bottom to fully contact with the oxygen, avoiding oxide aggregation formed by slow reaction between metal for oxidizing to generate metal oxide and the oxygen due to the fact that the material section at the bottom is in contact with a high-temperature material boat for a long time, and taking out the material after the oxidation is finished;
(4) and pressing ingot, sintering and shaping to obtain the silver-based metal oxide electrical contact material.
It is further provided that the metal alloy component is other metals than silver, including one or more of zinc, copper or cadmium.
The invention also provides a preferable dynamic internal oxidation method of the AgZnO electric contact material, which comprises the following steps:
(1) preparing a smelting alloy ingot: according to the formula of AgZnO, adding an Ag plate, a Zn plate and additives, pre-smelting AgZn alloy, and casting the melt to prepare an AgZn alloy ingot;
(2) turning and extruding: turning a layer of black skin on the surface of a cast AgZn alloy ingot by using a lathe, and processing the black skin into filaments by using an extruder;
(3) drawing and cutting: drawing the extruded alloy wire to the diameter of 2.0mm, and cutting the wire material into small sections of 10-15mm by using a punch;
(4) dynamic internal oxidation: putting the cut material segments below a rotating shaft in a self-made high-temperature internal oxidation furnace, introducing oxygen, starting the oxidation furnace, heating to 700-;
(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 to obtain better compactness;
(6) and (3) extrusion treatment: preheating the sintered ingot blank at 800 +/-10 ℃, and then loading the ingot blank into an oil pressure extruder at the temperature to extrude the ingot blank into a wire with the diameter of 5.8 mm;
(7) drawing; according to the drawing process, drawing the wire with the diameter of 5.8mm into the wire with the diameter of 2.88mm by a medium-frequency drawing machine.
Further setting the rotation number of the rotating shaft in the step (4) to be 50-100 rpm.
Further setting the oxygen pressure of the oxygen introduced in the step (4) to be 0.2-0.8 MPa.
The further setting is that in the step (6), the extrusion treatment adopts a forward extrusion mode for extrusion, the extrusion pressure is 160 +/-10 MPa, and the extrusion speed is 2-8 mm/s.
Further setting the process parameters of the medium-frequency wire drawing machine in the drawing process in the step (7) as wire drawing speed of 5.0Hz and current intensity of 10A.
The AgZnO electric contact material is further prepared from the following raw materials, by weight, 70-85 wt.% of Ag, 5-25 wt.% of Zn, 5-15 wt.% of CuO and the balance of NiO.
The invention can achieve the following beneficial effects:
(1) the traditional static internal oxidation process is changed into dynamic internal oxidation, so that the internal oxidation time is shortened to 8-10 hours from the original 20 hours, the oxide aggregation phenomenon does not occur in the oxidation process, and the gold phase structure after oxidation is uniformly distributed in a step shape;
(2) compared with an atomization process, the material produced by the internal oxidation process has better electric service life under a direct current condition, and tests show that the service life of the material reaches more than 10 ten thousand times under a certain current, and the material has higher fusion welding resistance and burning loss resistance.
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 the examples of the present invention, example 1:
(1) preparing a smelting alloy ingot: manufacturing according to 25kg in a 1 furnace, firstly putting 70 wt.% of Ag plate, 26 wt.% of Zn plate and 2 wt.% of Cu plate and 2 wt.% of Ni, smelting in a medium-frequency smelting way, setting the smelting temperature at 1200 ℃, and the smelting time at 0.5h, stirring by using a graphite rod in the smelting process, then reducing the temperature to 1100 ℃ for refining for 20min, finally pouring the refined alloy solution into a mold, and cooling in water after solidification to finally prepare an AgZn alloy spindle;
(2) turning treatment: removing a layer of oxide skin on the surface of the cast alloy ingot by using a lathe, wherein the turning amount is 1-2mm, and the rotating speed of the lathe is 2000 rpm;
(3) and (3) extrusion treatment: preheating the turned ingot blank, wherein the preheating temperature is 700 +/-10 ℃, the heat preservation time is 2-3 hours, then loading the ingot blank into an extruder at the temperature to extrude the ingot blank into a wire with the diameter of 5.8mm, the extrusion speed is 2-8mm/s, and the extrusion pressure is 150 +/-10 MPa;
(4) drawing and cutting; according to the drawing process, drawing the wire with the diameter of 5.8mm into the wire with the diameter of 2.0mm by a wire drawing machine, and cutting the wire with the diameter of 2.0mm into small sections with the diameter of 10-15mm by a punch.
(5) Dynamic internal oxidation: adding the cut small sections below a rotating shaft with a plough shovel in an internal oxidation furnace, introducing oxygen, starting the oxidation furnace, heating to 700-; after the set oxidation time is reached, closing the oxygen, evacuating the pressure in the furnace, and taking out the materials;
(6) and (3) ingot pressing treatment: pressing the oxidized material section by using a hydraulic press
The pressure of the hydraulic press is 30 +/-2 Mpa;
(7) sintering treatment: putting the ingot blank into a sintering furnace, and sintering at 700-900 ℃ for 2-6 h;
(8) and (3) extrusion treatment: preheating the sintered ingot blank at 800 +/-10 ℃, keeping the temperature for 2-3h, extruding at the speed of 2-8mm/s and the extrusion pressure of 150 +/-10 MPa, and then putting the preheated ingot blank into an extruder under the condition to extrude the preheated ingot blank into a wire material with the diameter of 5.8 mm;
(9) drawing: according to the drawing process, drawing the wire with the diameter of phi 5.8mm into the wire with the diameter of phi 2.88mm by a medium-frequency drawing machine, wherein the drawing process is as follows:
The rotating speed of the rotating shaft in the moving internal oxidation process is 50-100 rpm;
the process parameters of the medium-frequency wire drawing machine in the drawing process are wire drawing frequency of 5.5Hz and current intensity of 12A;
example 2:
the difference from example 1 was that the charged raw material content was different from that of 1 furnace of 25kg, and 80 wt.% Ag plate, 10 wt.% Zn plate, 5 wt.% Cu plate, and 5 wt.% Ni plate were charged.
Example 3:
the difference from examples 1 and 2 is that the charged raw material contents are different from each other, and the raw material contents are prepared in accordance with 1 furnace 25Kg, 85 wt.% Ag plate and 12 wt.% Zn plate, and 1 wt.% Cu plate and 2 wt.% Ni plate.
The AgZnO/Cu rivet contact prepared by the above embodiment is used for simulating electrical property experiments, and the specifications of the rivet are moving contact R5x1.4(0.5) +3x1.2SR20 and static contact F5x1.4(0.5) +3x 2.5. The experimental conditions for simulating the electrical properties are as follows: 250VAC, 15A, closing force of 100g, breaking force of 65g and contact frequency of 90 times/minute; 24VDC, 12A, closing force of 100g, breaking force of 65g and contact frequency of 90 times/min, and the experimental results are shown in Table 1.
TABLE 1 Electrical Performance test results for AgZnO/Cu rivet contacts
The experimental results show that the electrical properties of example 3 in the three examples are the best, the performances are good under the direct current condition and the alternating current condition, the contact resistance is low, the electrical life is over 12 ten thousand times, and the electrical life of other examples is over 10 ten thousand times, which is mainly attributed to the fact that the moving high-temperature internal oxidation process can permeate the oxygen of the material section without generating oxide aggregation within a preset time and generate uniformly distributed oxides, and the structures of the prepared wire material and the rivet contact material are effectively improved, so that the good electrical properties are obtained. The transverse and longitudinal section shapes of the wire show that most of oxide particles are smaller than 1 mu m in size, the surface of the rivet is clean and has no foreign matters, and the rivet manufactured by the manufacturing method has excellent electrical property.
By adopting the technical scheme, the invention can obtain the following technical effects:
(1) the alloy material section is subjected to internal oxidation treatment by adopting a moving high-temperature internal oxidation process, the production period of internal oxidation is shortened from the original 20 hours to 8-10 hours, no oxide is accumulated in the oxidation process, the oxide is uniformly distributed, and a better AgZnO wire material can be obtained;
(2) compared with the traditional internal oxidation process, the process flow greatly improves the production quality and the production efficiency;
(3) the rivet made of the wire material prepared by the invention has the electric service life of more than 10 ten thousand times, has lower contact resistance, the lowest contact resistance is 0.56 mu omega, and the highest electric service life can reach about 12 ten thousand times.
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 (8)
1. A dynamic internal oxidation method for a silver-based metal oxide electric contact material is characterized by comprising the following steps:
(1) preparing a smelting alloy ingot, namely smelting the silver alloy ingot to form the silver metal alloy ingot according to a formula of a silver-based metal oxide electrical contact material, wherein metal alloy components in the silver metal alloy ingot comprise other metals except silver and additives;
(2) turning the surface of a silver metal alloy ingot and processing the silver metal alloy ingot into a silver metal alloy wire;
(3) drawing and cutting: drawing the silver metal alloy wire into a filament shape, and then cutting the filament into small sections to obtain silver metal alloy cutting sections;
(4) dynamic internal oxidation: putting the silver metal alloy cutting section below a rotating shaft in a high-temperature internal oxidation furnace, introducing oxygen, starting the high-temperature internal oxidation furnace, heating to the temperature of 700-780 ℃ for 8-10 hours, starting the internal rotating shaft during heating, uniformly heating the material section in the rotating process, turning over the material section at the bottom to fully contact with the oxygen, avoiding oxide aggregation formed by slow reaction of metal used for oxidizing to generate metal oxide and the oxygen due to long-time contact of the material section at the bottom with a high-temperature material boat, and finally taking out the material after the oxidation is finished;
(4) and pressing ingot, sintering and shaping to obtain the silver-based metal oxide electrical contact material.
2. The method of claim 1, wherein the silver-based metal oxide electrical contact material is dynamically oxidized internally: the metal alloy component is other metals except silver, and comprises one or more of zinc, copper, nickel or cadmium.
3. A dynamic internal oxidation method of AgZnO electric contact material is characterized by comprising the following steps:
(1) preparing a smelting alloy ingot: according to the formula of AgZnO, adding an Ag plate, a Zn plate and additives, pre-smelting AgZn alloy, and casting the melt to prepare an AgZn alloy ingot;
(2) turning and extruding: turning a layer of black skin on the surface of a cast AgZn alloy ingot by using a lathe, and processing the black skin into filaments by using an extruder;
(3) drawing and cutting: drawing the extruded alloy wire to the diameter of 2.0mm, and cutting the wire into small sections of 10-15mm by using a punch;
(4) dynamic internal oxidation: putting the cut material segments below a rotating shaft in a self-made high-temperature internal oxidation furnace, introducing oxygen, starting the oxidation furnace, heating to 700-780 ℃ for 8-10 hours, starting the internal rotating shaft during heating, uniformly heating the material segments during rotation, turning over the material segments at the bottom to fully contact with the oxygen, avoiding oxide aggregation formed by slow reaction of Zn and the oxygen due to long-time contact of the material segments at the bottom with a high-temperature material boat, and taking out the material after the oxidation is finished to prepare for ingot pressing;
(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 to obtain better compactness;
(6) and (3) extrusion treatment: preheating the sintered ingot blank at 800 +/-10 ℃, and then loading the ingot blank into an oil pressure extruder at the temperature to extrude the ingot blank into a wire with the diameter of 5.8 mm;
(7) drawing; according to the drawing process, drawing the wire with the diameter of 5.8mm into the wire with the diameter of 2.88mm by a medium-frequency drawing machine.
4. The AgZnO electrical contact material dynamic internal oxidation method of claim 3, wherein: the revolution of the rotating shaft in the step (4) is 50-100 rpm.
5. The AgZnO electrical contact material dynamic internal oxidation method of claim 3, wherein: and (4) introducing oxygen into the reactor at an oxygen pressure of 0.2-0.8 MPa.
6. The AgZnO electrical contact material dynamic internal oxidation method of claim 3, wherein: and (6) extruding in a forward extrusion mode, wherein the extrusion pressure is 160 +/-10 MPa, and the extrusion speed is 2-8 mm/s.
7. The AgZnO electrical contact material dynamic internal oxidation method of claim 3, wherein: the process parameters of the medium-frequency wire drawing machine in the drawing process in the step (7) are wire drawing speed of 5.0Hz and current intensity of 10A.
8. The AgZnO electrical contact material dynamic internal oxidation method of claim 3, wherein: the AgZnO electric contact material comprises, by weight, 70-85 wt.% of Ag, 5-25 wt.% of Zn, 5-15 wt.% of CuO and the balance of NiO.
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Cited By (3)
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| CN112151291A (en) * | 2020-08-18 | 2020-12-29 | 福达合金材料股份有限公司 | Long-life silver metal oxide electric contact material and preparation method thereof |
| CN112725652A (en) * | 2020-12-24 | 2021-04-30 | 福达合金材料股份有限公司 | Silver zinc oxide electric contact material and preparation method thereof |
| CN113488354A (en) * | 2021-05-27 | 2021-10-08 | 福达合金材料股份有限公司 | Silver tin oxide electric contact material and preparation method thereof |
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