CN111961910B - Preparation method of silver tin oxide electric contact material - Google Patents
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- CN111961910B CN111961910B CN202010725802.4A CN202010725802A CN111961910B CN 111961910 B CN111961910 B CN 111961910B CN 202010725802 A CN202010725802 A CN 202010725802A CN 111961910 B CN111961910 B CN 111961910B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- C22C1/00—Making non-ferrous alloys
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- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-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
- C22C32/0005—Non-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 at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
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- H01H1/02—Contacts characterised by the material thereof
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Abstract
The invention discloses a preparation method of a silver tin oxide electric contact material, which comprises the following steps: (1) putting the raw materials into a smelting furnace for smelting, and preparing alloy powder after water atomization; (2) drying the alloy powder in a microwave oven, and oxidizing the alloy powder in the microwave oven to obtain oxidized alloy powder; (3) oxidizing the alloy powder to form an ingot blank; (4) sintering the ingot blank in an oxygen pressure atmosphere to prepare a sintered ingot blank; (5) and (3) pressing the sintered ingot blank into a wire material, using the wire material for cold heading to make a rivet contact, and rolling and punching the plate material to produce a sheet contact to obtain the silver tin oxide electric contact material. The silver tin oxide electric contact material prepared by the invention has the advantages of small arcing energy, long electric service life, simple designed process route, high material utilization rate and short production period, is suitable for large-scale production, and can be widely popularized and applied.
Description
Technical Field
The invention belongs to the technical field of electric contact material preparation, and particularly relates to a preparation method of a silver tin oxide electric contact material.
Background
In the prior art, methods for preparing the silver tin oxide electrical contact material include a chemical method, a powder mixing method, an internal oxidation method and a pre-oxidation method, wherein the pre-oxidation method has the characteristics of uniform distribution of oxide particles, simple processing technology, short flow and the like and is popularized and applied.
The traditional heating method for preparing the silver tin oxide electric contact material is that the surface of an object is heated firstly by means of heating the surrounding environment in a heat radiation or hot air convection mode, and then the surface of the object is conducted to the inside of the object through heat conduction. In addition, the silver tin oxide electric contact material prepared by the prior art has the problems of large arcing energy and short electric service life, and can not meet the use requirements of electric equipment such as an alternating current contactor, a relay and the like.
Disclosure of Invention
The invention provides a preparation method of a silver tin oxide electric contact material, which aims to solve the problems of large arcing energy and short electric service life of the silver tin oxide electric contact material prepared by the prior art and can not meet the use requirements of electric equipment such as an alternating current contactor, a relay and the like.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a silver tin oxide electric contact material comprises the following steps:
s1: the composite material comprises the following raw materials in parts by weight: 63-72 parts of silver powder, 16-28 parts of tin powder, 1-2 parts of graphite powder, 0.3-0.5 part of europium powder, 2-4 parts of rubidium carbonate powder, 6-8 parts of copper powder, 3-5 parts of bismuth powder and 2.7-5.6 parts of molybdenum carbide powder are put into a smelting furnace to be smelted, and alloy powder is prepared after water atomization;
s2: putting the alloy powder prepared in the step S1 into a microwave oven, drying the alloy powder at the temperature of 400-430 ℃ and the spreading thickness of the powder is 6.2-7.4mm, and then heating the alloy powder to 520-550 ℃ at the speed of 6.3-8.2 ℃/min in the microwave oven to oxidize the alloy powder to prepare oxidized alloy powder;
s3: pressing the oxide alloy powder prepared in the step S2 into an ingot blank with the diameter of 60-100mm at the temperature of 560-;
s4: sintering the ingot blank prepared in the step S3 for 20-30min at the oxygen pressure of 2-3MPa and the temperature of 650-680 ℃ to prepare a sintered ingot blank;
s5: and (3) pressing the sintered ingot blank prepared in the step (S4) at the temperature of 690 and 700 ℃ into a wire material with the specification of phi 4 mm-phi 6mm, using the wire material for cold heading to punch a rivet contact, and rolling and punching the plate to produce a sheet contact to prepare the silver tin oxide electrical contact material.
Preferably, the particle size of the silver powder in step S1 is 0.2-13.3. mu.m.
Preferably, the particle size of the tin powder in step S1 is 0.5 to 11.8 μm.
Preferably, the particle size of the graphite powder in step S1 is 1.2 to 10.3 μm.
Preferably, the particle size of the europium powder in step S1 is 1.2-3.4 μm.
Preferably, the particle size of the rubidium carbonate powder in the step S1 is 0.7-5.2 μm.
Preferably, the particle size of the copper powder in step S1 is 0.9-8.5 μm.
Preferably, the particle size of the bismuth powder in step S1 is 0.3 to 7.4 μm.
Preferably, the particle size of the molybdenum carbide powder in step S1 is 0.6 to 9.2 μm.
Preferably, the specification of the wire rod in the step S5 is phi 4 mm-phi 6 mm.
The invention has the following beneficial effects:
(1) the arcing energy of the silver tin oxide electric contact material prepared by the invention is obviously lower than that of the silver tin oxide electric contact material prepared by the prior art, and is at least lower than 33.5 percent; the average value of the arcing energy of the silver tin oxide electric contact material prepared by the invention is less than or equal to 948.13MJ, which shows that the silver tin oxide electric contact material has very small arcing energy and can meet the use requirements of electric appliances such as alternating current contactors, relays and the like.
(2) The method utilizes the reducibility of the graphite, can greatly reduce the thickness and continuity of an oxide film formed on the surface of the silver tin oxide electric contact material in the electric contact process, and greatly reduce the temperature rise in the electric contact process; in addition, the invention also utilizes the fusion welding resistance of the graphite, and can greatly reduce the fusion welding tendency of the silver tin oxide electric contact material in the contact process.
(3) The europium added in the invention is a surface active element, and the europium is gathered on the surface of the silver tin oxide electric contact material to show positive adsorption effect, so that the surface free energy of the electric contact material can be effectively reduced, the surface tension of the electric contact material is reduced, and the wettability of the electric contact material is further improved. In addition, europium can further play a role of microalloying, and the europium is easy to segregate at crystal boundaries, so that the crystal boundaries are strengthened, further the crystal lattice heat energy and thermoelectric conversion energy barrier are reduced, and the arcing energy is further reduced. The europium atom has a larger radius, and can play a role in refining grains and improving the structure, thereby promoting the reaction of tin and silver in the electric contact material. The rubidium carbonate can improve the conductivity and the thermoelectric property in the preparation of the silver tin oxide electric contact material, thereby reducing the arcing energy. In addition, molybdenum carbide is extremely easy to decompose under the action of electric arc, the formed molybdenum is extremely easy to oxidize, and much heat is taken away along with the sublimation of molybdenum oxide at high temperature, so that the energy of the electric arc can be reduced. Europium powder, rubidium carbonate powder and molybdenum carbide powder are added in the silver tin oxide electrical contact material, and the europium powder, the rubidium carbonate powder and the molybdenum carbide powder play a synergistic role, so that the arcing energy is synergistically reduced.
(4) The silver tin oxide electric contact material prepared by the invention has uniform metallographic structure and small discreteness of mechanical and physical properties, has at least 19.8 percent higher electric service life than the silver tin oxide electric contact material prepared by the prior art, and is more durable.
(5) The invention adopts microwave heating drying and powder oxidation, the temperature uniformity in the oxidation process is good, the oxidation is more uniform, and the prepared silver tin oxide electrical contact material has extremely high stability in the processing process.
(6) The method has the advantages of simple process route, high material utilization rate and short production period, is suitable for large-scale production, and can be widely popularized and applied.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
In an embodiment, the preparation method of the silver tin oxide electrical contact material comprises the following steps:
s1: the composition comprises the following raw materials in parts by weight: 63-72 parts of silver powder, 16-28 parts of tin powder, 1-2 parts of graphite powder, 0.3-0.5 part of europium powder, 2-4 parts of rubidium carbonate powder, 6-8 parts of copper powder, 3-5 parts of bismuth powder and 2.7-5.6 parts of molybdenum carbide powder are put into a smelting furnace to be smelted, and alloy powder is prepared after water atomization;
the granularity of the silver powder is 0.2-13.3 mu m;
the granularity of the tin powder is 0.5-11.8 mu m;
the granularity of the graphite powder is 1.2-10.3 mu m;
the particle size of the europium powder is 1.2-3.4 mu m;
the particle size of the rubidium carbonate powder is 0.7-5.2 mu m;
the granularity of the copper powder is 0.9-8.5 mu m;
the particle size of the bismuth powder is 0.3-7.4 mu m;
the granularity of the molybdenum carbide powder is 0.6-9.2 mu m;
s2: putting the alloy powder prepared in the step S1 into a microwave oven, drying the alloy powder at the temperature of 400-430 ℃ and the spreading thickness of the powder is 6.2-7.4mm, and then heating the alloy powder to 520-550 ℃ at the speed of 6.3-8.2 ℃/min in the microwave oven to oxidize the alloy powder to prepare oxidized alloy powder;
s3: pressing the oxide alloy powder prepared in the step S2 into an ingot blank with the diameter of 60-100mm at the temperature of 560-;
s4: sintering the ingot blank prepared in the step S3 for 20-30min at the oxygen pressure of 2-3MPa and the temperature of 650-680 ℃ to prepare a sintered ingot blank;
s5: and (3) pressing the sintered ingot blank prepared in the step (S4) at the temperature of 690 and 700 ℃ into a wire material with the specification of phi 4 mm-phi 6mm, using the wire material for cold heading to punch a rivet contact, and rolling and punching the plate to produce a sheet contact to prepare the silver tin oxide electrical contact material.
The present invention is illustrated by the following more specific examples.
Example 1
A preparation method of a silver tin oxide electric contact material comprises the following steps:
s1: the composition comprises the following raw materials in parts by weight: putting 65 parts of silver powder, 17 parts of tin powder, 1 part of graphite powder, 0.3 part of europium powder, 2 parts of rubidium carbonate powder, 6 parts of copper powder, 3 parts of bismuth powder and 2.8 parts of molybdenum carbide powder into a smelting furnace for smelting, and performing water atomization to obtain alloy powder;
the granularity of the silver powder is 0.5-13.1 mu m;
the granularity of the tin powder is 0.9-10.2 mu m;
the granularity of the graphite powder is 1.6-10.2 mu m;
the particle size of the europium powder is 1.7-3.2 mu m;
the particle size of the rubidium carbonate powder is 0.8-4.5 mu m;
the granularity of the copper powder is 1.1-8.3 mu m;
the particle size of the bismuth powder is 0.5-7.2 mu m;
the granularity of the molybdenum carbide powder is 0.8-7.8 mu m;
s2: putting the alloy powder prepared in the step S1 into a microwave oven, drying the alloy powder at the temperature of 406 ℃, flatly paving the powder to the thickness of 6.4mm, and then heating the powder to 540 ℃ at the speed of 6.6 ℃/min in the microwave oven to oxidize the alloy powder to prepare oxidized alloy powder;
s3: pressing the oxide alloy powder prepared in the step S2 into an ingot blank with the diameter of 60mm at the temperature of 560 ℃ and the pressure of 300 MPa;
s4: sintering the ingot blank prepared in the step S3 for 28min at the oxygen pressure of 2MPa and the temperature of 660 ℃ to prepare a sintered ingot blank;
s5: and (4) pressing the sintered ingot blank prepared in the step (S4) at the temperature of 690 ℃ to prepare a wire material with the specification of phi 4mm, using the wire material for cold heading rivet contact making, and rolling and punching the plate to produce a sheet contact to prepare the silver tin oxide electrical contact material.
Example 2
A preparation method of a silver tin oxide electric contact material comprises the following steps:
s1: the composition comprises the following raw materials in parts by weight: 70 parts of silver powder, 26 parts of tin powder, 2 parts of graphite powder, 0.5 part of europium powder, 3.7 parts of rubidium carbonate powder, 8 parts of copper powder, 5 parts of bismuth powder and 5.4 parts of molybdenum carbide powder are put into a smelting furnace for smelting, and alloy powder is prepared after water atomization;
the granularity of the silver powder is 1-11 mu m;
the granularity of the tin powder is 0.7-10.1 mu m;
the granularity of the graphite powder is 1.4-9.8 mu m;
the particle size of the europium powder is 1.7-3.1 mu m;
the particle size of the rubidium carbonate powder is 0.9-5 mu m;
the granularity of the copper powder is 0.9-6.4 mu m;
the particle size of the bismuth powder is 0.6-5.9 μm;
the granularity of the molybdenum carbide powder is 0.8-8.3 mu m;
s2: putting the alloy powder prepared in the step S1 into a microwave oven, drying the alloy powder at the temperature of 430 ℃, flatly paving the powder to the thickness of 6.7mm, and then heating the powder to 520 ℃ at the speed of 8 ℃/min in the microwave oven to oxidize the alloy powder to prepare oxidized alloy powder;
s3: pressing the oxide alloy powder prepared in the step S2 into an ingot blank with the diameter of 90mm at the temperature of 580 ℃ and the pressure of 300 MPa;
s4: sintering the ingot blank prepared in the step S3 for 22min at the oxygen pressure of 3MPa and the temperature of 670 ℃ to prepare a sintered ingot blank;
s5: and (4) pressing the sintered ingot blank prepared in the step (S4) at 695 ℃ to prepare a wire material with the specification of phi 5mm, using the wire material for cold heading rivet contact making, and rolling and punching the plate to produce a sheet contact to prepare the silver tin oxide electrical contact material.
Example 3
A preparation method of a silver tin oxide electric contact material comprises the following steps:
s1: the composition comprises the following raw materials in parts by weight: 67 parts of silver powder, 23 parts of tin powder, 1.6 parts of graphite powder, 0.4 part of europium powder, 3 parts of rubidium carbonate powder, 7.2 parts of copper powder, 4 parts of bismuth powder and 4.5 parts of molybdenum carbide powder are put into a smelting furnace for smelting, and alloy powder is prepared after water atomization;
the granularity of the silver powder is 0.2-11.6 mu m;
the granularity of the tin powder is 0.7-5 mu m;
the granularity of the graphite powder is 1.3-10.1 mu m;
the particle size of the europium powder is 1.8-2.7 mu m;
the particle size of the rubidium carbonate powder is 0.8-5 mu m;
the granularity of the copper powder is 1.3-6.4 mu m;
the particle size of the bismuth powder is 0.7-5.9 μm;
the granularity of the molybdenum carbide powder is 0.9-9.1 mu m;
s2: putting the alloy powder prepared in the step S1 into a microwave oven, drying the alloy powder at the temperature of 420 ℃, flatly paving the powder to the thickness of 6.8mm, and then heating the powder to 550 ℃ at the speed of 7 ℃/min in the microwave oven to oxidize the alloy powder to prepare oxidized alloy powder;
s3: pressing the oxide alloy powder prepared in the step S2 into an ingot blank with the diameter of 70mm at the temperature of 600 ℃ and the pressure of 270 MPa;
s4: sintering the ingot blank prepared in the step S3 for 26min at the oxygen pressure of 2.4MPa and the temperature of 680 ℃ to prepare a sintered ingot blank;
s5: and (4) pressing the sintered ingot blank prepared in the step (S4) at the temperature of 700 ℃ to prepare a wire material with the specification of phi 6mm, using the wire material for cold heading rivet contact making, and rolling and punching the plate to produce a sheet contact to prepare the silver tin oxide electrical contact material.
Comparative example 1
The method for preparing the silver tin oxide electrical contact material is basically the same as that of the silver tin oxide electrical contact material prepared in the example 3, except that europium powder, rubidium carbonate powder and molybdenum carbide powder are absent in the preparation raw materials.
Comparative example 2
The method for preparing a silver tin oxide electrical contact material was substantially the same as that of example 3, except that europium powder was absent from the raw materials.
Comparative example 3
The method for preparing a silver tin oxide electrical contact material was substantially the same as that used in example 3, except that rubidium carbonate powder was absent from the starting materials.
Comparative example 4
The method of preparing a silver tin oxide electrical contact material was substantially the same as that of example 3, except that molybdenum carbide powder was absent from the raw materials.
Comparative example 5
The silver tin oxide electric contact material is prepared by the method of the embodiment 1 and 2 in the Chinese patent application document 'a method for preparing the silver tin oxide electric contact material by microwave heating (application publication number: CN 108010772A)'.
Firstly, an arc energy comparison experiment.
The silver tin oxide electric contact materials prepared in the examples 1 to 3 and the comparative examples 1 to 5 were subjected to an alternating current resistive load under a voltage of 220V and a current of 20A, and the average arcing energy was calculated at 5000 points from the recorded parameters after 8 ten thousand tests in an electric property simulation tester, and the results are shown in the following table.
From the above table, it can be seen that: (1) as can be seen from the data of examples 1-3 and comparative example 5, the average value of the arcing energy of the silver tin oxide electric contact materials prepared in examples 1-3 is significantly lower than that of the silver tin oxide electric contact material prepared in comparative example 5 (prior art), and is at least 33.5% lower; meanwhile, as can be seen from the data of the examples 1-3, the average value of the arcing energy is less than or equal to 948.13MJ, which shows that the arcing energy of the silver tin oxide electric contact material is very small and can meet the application requirements; in addition, as can be seen from the data of examples 1-3, example 3 is the most preferred example.
(2) As can be seen from the data of example 1 and comparative examples 1 to 4, europium powder, rubidium carbonate powder and molybdenum carbide powder play a synergistic role in preparing the silver tin oxide electric contact material, and the arc energy is synergistically reduced, which is that: europium is a surface active element, is gathered on the surface of the silver tin oxide electric contact material to show positive adsorption effect, and can effectively reduce the surface free energy of the electric contact material, so that the surface tension of the electric contact material is reduced, and the wetting property of the electric contact material is further improved. Moreover, europium can further play a role of microalloying, and the europium is easy to segregate at a crystal boundary, so that the crystal boundary is strengthened, the crystal lattice heat energy and the thermoelectric conversion energy barrier are further reduced, and the arcing energy is further reduced. The europium atom has a larger radius, and can play a role in refining grains and improving the structure, thereby promoting the reaction of tin and silver in the electric contact material. The rubidium carbonate can improve the conductivity and the thermoelectric property in the preparation of the silver tin oxide electric contact material, thereby reducing the arcing energy. In addition, molybdenum carbide is extremely easy to decompose under the action of electric arc, the formed molybdenum is extremely easy to oxidize, and much heat is taken away along with the sublimation of molybdenum oxide at high temperature, so that the energy of the electric arc can be reduced. Europium powder, rubidium carbonate powder and molybdenum carbide powder are added in the silver tin oxide electrical contact material, and the europium powder, the rubidium carbonate powder and the molybdenum carbide powder play a synergistic role, so that the arcing energy is synergistically reduced.
And secondly, electrical property comparison experiments.
The wires prepared in examples 1 to 3 and comparative example 5 were used for cold heading rivet contact, sheet-like contacts were produced from the sheet after rolling-punching, and the relay was assembled for electrical life test, three times for each example or comparative example, taking average values of electrical life, and relay test conditions are shown in the following table.
The electrical properties results are shown in the table below.
From the above table, it can be seen that: the average electrical life of the silver tin oxide electrical contact materials prepared in examples 1-3 was significantly higher than that of the silver tin oxide electrical contact material prepared in comparative example 5 (prior art), by at least 19.8% or more, indicating that the silver tin oxide electrical contact material of the present invention has a longer electrical life and is more durable.
The above description should not be taken as limiting the invention to the specific embodiments, but rather, as will be readily apparent to those skilled in the art to which the invention pertains, numerous simplifications or substitutions may be made without departing from the spirit of the invention, which should be construed to fall within the scope of the invention as defined in the claims appended hereto.
Claims (7)
1. The preparation method of the silver tin oxide electric contact material is characterized by comprising the following steps:
s1: the composition comprises the following raw materials in parts by weight: 63-72 parts of silver powder, 16-28 parts of tin powder, 1-2 parts of graphite powder, 0.3-0.5 part of europium powder, 2-4 parts of rubidium carbonate powder, 6-8 parts of copper powder, 3-5 parts of bismuth powder and 2.7-5.6 parts of molybdenum carbide powder are put into a smelting furnace to be smelted, and alloy powder is prepared after water atomization;
the particle size of the europium powder is 1.2-3.4 mu m;
the particle size of the rubidium carbonate powder is 0.7-5.2 mu m;
the granularity of the molybdenum carbide powder is 0.6-9.2 mu m;
s2: putting the alloy powder prepared in the step S1 into a microwave oven, drying the alloy powder at the temperature of 400-430 ℃ and the spreading thickness of the powder is 6.2-7.4mm, and then heating the alloy powder to 520-650 ℃ at the speed of 6.3-8.2 ℃/min in the microwave oven to oxidize the alloy powder to prepare oxidized alloy powder;
s3: pressing the oxide alloy powder prepared in the step S2 into an ingot blank with the diameter of 60-100mm at the temperature of 860 ℃ and 900 ℃ and the pressure of 250 ℃ and 300 MPa;
s4: sintering the ingot blank prepared in the step S3 for 20-30min at the oxygen pressure of 2-3MPa and the temperature of 950-;
s5: and (4) pressing the sintered ingot blank prepared in the step (S4) at the temperature of 1000-1100 ℃ to prepare a wire material with the specification of phi 4 mm-phi 6mm, wherein the wire material is used for cold heading rivet contact making, and the sheet material is rolled and punched to produce a sheet contact to prepare the silver tin oxide electrical contact material.
2. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein the particle size of the silver powder in step S1 is 0.2 to 13.3 μm.
3. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein the particle size of the tin powder in step S1 is 0.5 to 11.8 μm.
4. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein the particle size of the graphite powder in step S1 is 1.2 to 10.3 μm.
5. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein the particle size of the copper powder in step S1 is 0.9 to 8.5 μm.
6. The method for producing a silver tin oxide electrical contact material according to claim 1, wherein the particle size of the bismuth powder in step S1 is 0.3 to 7.4 μm.
7. The method for preparing a silver tin oxide electrical contact material according to claim 1, wherein the gauge of the wire in step S5 is Φ 4mm — Φ 6 mm.
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| CN106282640A (en) * | 2016-08-22 | 2017-01-04 | 福达合金材料股份有限公司 | A kind of silver nickel electric contact material and preparation method thereof |
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| CN1036991A (en) * | 1988-03-26 | 1989-11-08 | 多杜科、杜尔瓦希特两合公司 | By silver and tin-oxide is the electric contact work in-process made of matrix material on basis and the powder metallurgy process of production thereof |
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| CN101651054A (en) * | 2009-09-11 | 2010-02-17 | 昆明理工大学 | Preparation method of modified AgSnO2 electric contact material |
| CN102176336A (en) * | 2010-12-30 | 2011-09-07 | 温州宏丰电工合金股份有限公司 | Preparation method of silver-based oxide electrical contact material with filamentary structure |
| CN106282640A (en) * | 2016-08-22 | 2017-01-04 | 福达合金材料股份有限公司 | A kind of silver nickel electric contact material and preparation method thereof |
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