CN115927899B - Silver copper oxide contact material and preparation method thereof - Google Patents
Silver copper oxide contact material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of electrical contact materials, in particular to a silver copper oxide contact material and a preparation method thereof, wherein the preparation method comprises the following steps: smelting and atomizing to prepare powder; oxidizing in the powder; isostatic compaction; vacuum liquid phase sintering; internal oxidation; and (5) extruding. According to the invention, the technical scheme of incomplete powder internal oxidation of low-temperature low-pressure rotary ball milling is adopted, so that the efficiency is improved, caking is prevented, and meanwhile, the impurity introduction of tooling equipment and excessive segregation of copper oxide are avoided; secondly, the invention promotes the effective combination between all interfaces in the sintering process by vacuum liquid phase sintering on one hand, and effectively improves the processing performance and the electrical performance of the contact material; on the other hand, the phenomenon of aggregation of oxide particles is reduced, and the tissue uniformity of the contact material is improved; in addition, the silver-copper oxide contact prepared by using the silver-copper oxide contact material disclosed by the invention has better burning loss resistance, fusion welding resistance and electric life.
Description
Technical Field
The invention relates to the technical field of electrical contact materials, in particular to a silver copper oxide contact material and a preparation method thereof.
Background
The silver copper oxide contact material is a novel environment-friendly contact material, has excellent arc erosion resistance, wear resistance and fusion welding resistance, and has better service performance on a direct current contactor than silver cadmium oxide or silver tin oxide materials. At present, the preparation process of the silver copper oxide contact material mainly comprises a powder metallurgy method, an alloy internal oxidation method, a chemical method and a powder internal oxidation method. The powder internal oxidation method combines the advantages of the powder metallurgy method and the alloy internal oxidation method, avoids the problems of complex process, chemical pollution in the preparation process and the like of the chemical method, is suitable for batch preparation, and has good application prospect.
The traditional preparation process flow of the powder internal oxidation method comprises the following steps: smelting, atomizing and pulverizing, oxidizing in powder, ball milling and crushing, isostatic compaction, sintering, hot extrusion, drawing or rolling, and finally producing and processing into corresponding contact finished products. The process has the following disadvantages:
(1) The silver copper oxide contact material prepared by the traditional powder internal oxidation production process has poor electrical property, poor arc erosion resistance and fusion welding resistance and short service life;
(2) In the high-temperature and high-pressure powder internal oxidation process, tooling equipment such as a material tray, a material rack and the like can form oxide skin under the high-temperature and high-pressure condition, so that impurities are introduced into the powder;
(3) In the powder oxidation stage, the thermodynamic stability of copper oxide is higher than that of silver oxide, so that copper oxidation is higher than that of silver, copper oxide segregation is formed on the surface of the powder, and silver contact and diffusion between the powder are seriously hindered in the subsequent sintering process, so that the green body has poor sinterability, and the material has poor processing plasticity, low yield, uneven structure and poor electrical property.
Disclosure of Invention
In order to solve the technical problems, the invention provides a silver copper oxide contact material and a preparation method thereof, wherein the preparation method shortens the production period, improves the production efficiency, and the prepared silver copper oxide contact material has the advantages of less impurities, high yield, uniform material structure and excellent performance.
First, the invention provides a method for preparing a silver copper oxide contact material, which comprises the following steps:
(1) Smelting and atomizing to prepare powder: weighing 79-95 parts of silver, 5-18 parts of copper and 0-3 parts of metal simple substance to obtain a mixture, and atomizing the mixture to prepare powder after smelting in a medium-frequency smelting furnace to obtain silver-copper alloy powder;
(2) Powder internal oxidation: adding silver-copper alloy powder, additive powder and ball material into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment to obtain silver-copper oxide composite powder with the oxidation rate of 70-90%, wherein the additive powder comprises metal simple substance or metal compound;
(3) Isostatic compaction: isostatic compaction is carried out on the silver copper oxide composite powder to obtain silver copper oxide ingot blanks;
(4) Vacuum liquid phase sintering: vacuum liquid phase sintering is carried out on the silver copper oxide ingot blank at the temperature of more than or equal to 890 ℃ and less than 962 ℃;
(5) Internal oxidation: reducing the temperature, and carrying out further internal oxidation on the sintered silver copper oxide ingot blank;
(6) Extruding: and (5) carrying out hot extrusion on the product obtained in the step (5) to obtain the silver copper oxide contact material.
According to the invention, through changing the high-temperature and high-pressure conditions to low-temperature and low-pressure conditions in the powder internal oxidation stage in the prior art, on one hand, additive powder can be added into silver-copper alloy powder, so that the electrical property of the silver-copper oxide contact material is effectively improved, and the service life of the silver-copper oxide contact material is prolonged; on the other hand, the tool equipment can be prevented from being oxidized at high temperature and high pressure in the traditional process, so that impurities are introduced into the material.
In addition, the invention adopts the technical scheme of carrying out rotary ball milling treatment while oxidizing in the powder, solves the agglomeration problem of the surface layer in the oxidation process of the silver-copper alloy powder, shortens the internal oxidation time, omits the process of independently carrying out ball milling after the internal oxidation of the powder in the traditional process, and improves the preparation efficiency.
And the invention solves the technical problems of poor processing plasticity, low yield, uneven structure and poor electrical property of the material caused by copper oxide segregation by the technical proposal of low-temperature low-pressure incomplete powder internal oxidation and vacuum liquid phase sintering. Specifically, the technical scheme of incomplete oxidation of low-temperature low-pressure rotary ball milling effectively reduces the generation of copper oxide segregation, and secondly, the invention can repeatedly diffuse silver copper oxide ingot blank through the technical scheme of vacuum liquid phase sintering, and increase the contact between powders, so that the sintering property of the blank is better.
In addition, it should be noted that, in the process of vacuum liquid phase sintering, in order to avoid the phenomenon that after the sintering reaches the melting point of pure silver, the silver copper oxide ingot is excessively melted, and the structure is uneven, the temperature of the vacuum liquid phase sintering is lower than the melting point of silver (962 ℃).
Preferably, the metal element in the step (1) includes one or more of Sn, in, ni, zn, bi, al, te, sb.
Preferably, the silver-copper oxide composite powder prepared in the step (2) comprises the following components in parts by mass: 97-100 parts of silver-copper alloy powder and 0-3 parts of additive powder.
Preferably, the additive powder comprises Co, fe, W, mo, co 2 O 3 、Fe 2 O 3 、WO 3 、MoO 3 、La 2 O 3 、Y 2 O 3 、CeO 2 One or more of WC, tiC, tiN powder.
By adding the additive powder, the electrical property and the service life of the silver copper oxide contact material prepared by the invention are improved, and the arc erosion resistance and fusion welding resistance of the silver copper oxide contact material are effectively enhanced.
Additive Co, fe, W, mo, co of the invention 2 O 3 、Fe 2 O 3 、WO 3 、MoO 3 WC, tiC, tiN powder, la due to the inability to form alloys during smelting 2 O 3 、Y 2 O 3 、CeO 2 The powder is easy to oxidize in the smelting process, and cannot be directly added into a smelting furnace for smelting, so that the powder can be uniformly added into the silver-copper alloy powder by setting the technical scheme of low-temperature low-pressure rotary ball milling internal oxidation, thereby improving the electrical property of the silver-copper oxide contact material.
Preferably, the conditions of the low-temperature low-pressure rotary ball milling internal oxidation in the step (2) are as follows: the temperature is 350-550 ℃, the oxygen partial pressure is 0.02-0.1 MPa, the rotation speed is 10-50 r/min, and the internal oxidation time is 1-4 h.
Preferably, the isostatic compaction conditions in step (3) are: isostatic pressure of 50-300 MPa and dwell time of 10-300 s.
Preferably, the conditions of the vacuum liquid phase sintering in the step (4) are as follows: the temperature is 890-940 ℃ and the time is 1-2 h.
According to the invention, the silver copper oxide composite powder with the oxidation rate of 70-90% is utilized, the melting point of the silver copper oxide composite powder is above 890 ℃, and the silver copper oxide ingot blank is subjected to vacuum liquid phase sintering, so that on one hand, the diffusion speed of substances in the sintering process is improved, the effective combination between all interfaces in the sintering process is promoted, the densification speed of the sintered ingot blank is accelerated, the density of the sintered ingot blank is greatly improved, and the processing performance and the electrical performance of a contact material are further effectively improved; on the other hand, in the vacuum liquid phase sintering process, the oxide in the silver-copper oxide composite powder is uniformly diffused and redistributed from the high-concentration area of the outer layer to the low-concentration area of the inner layer, so that the aggregation phenomenon of oxide particles is reduced, and the tissue uniformity of the contact material is improved.
Preferably, the internal oxidation conditions in the step (5) are: the temperature is 700-850 ℃, the oxygen partial pressure is 0.2-2.0 MPa, and the time is 2-8 h.
The invention further provides the silver copper oxide contact material prepared by the preparation method.
In addition, the invention also provides a preparation method and application of the silver copper oxide contact material in preparation of silver copper oxide contacts.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, through the technical scheme of rotary ball milling in the powder internal oxidation process, the preparation period is shortened, and the preparation efficiency is improved;
(2) According to the invention, through adopting a technical scheme of low-temperature low-pressure internal oxidation in the powder internal oxidation stage, the impurity content, the product purity, the tissue uniformity and the material processing plasticity of the prepared silver copper oxide contact material are reduced;
(3) According to the invention, by adding the additive powder, the electrical property and the service life of the silver copper oxide contact material prepared by the method are improved, and the arc erosion resistance and fusion welding resistance of the silver copper oxide contact material are effectively enhanced;
(4) According to the technical scheme of vacuum liquid phase sintering, on one hand, the diffusion speed of substances in the sintering process is improved, the effective combination among all interfaces in the sintering process is promoted, the densification speed of a sintered ingot blank is accelerated, the density of the sintered ingot blank is greatly improved, and the processability and the electrical property of a contact material are further effectively improved; on the other hand, in the vacuum liquid phase sintering process, the oxide in the silver-copper oxide composite powder is uniformly diffused and redistributed from the high-concentration area of the outer layer to the low-concentration area of the inner layer, so that the aggregation phenomenon of oxide particles is reduced, and the tissue uniformity of the contact material is improved.
Drawings
Fig. 1 shows a 200-fold metallographic structure of a silver copper oxide contact material according to example 2 of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and specific examples. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. In addition, the embodiments of the present invention referred to in the following description are typically only some, but not all, embodiments of the present invention. Therefore, all other embodiments, which can be made by one of ordinary skill in the art without undue burden, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
Example 1
(1) Weighing 93.1 parts of silver, 6.5 parts of copper, 0.2 part of bismuth and 0.2 part of copper, smelting the materials in a medium-frequency induction smelting furnace, and then atomizing to prepare powder, drying and screening to obtain silver-copper alloy powder;
(2) Weighing 99.6 parts of silver-copper alloy powder, 0.1 part of molybdenum, 0.3 part of yttrium oxide and 5:1 of ball material in mass ratio, and adding the mixture into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment. The low-temperature low-pressure rotary ball milling internal oxidation conditions are as follows: the temperature is 500 ℃, the oxygen partial pressure is 0.02MPa, the rotating speed is 25r/min, the internal oxidation time is 3h, and the silver copper oxide composite powder with the oxidation rate of 82% is obtained;
(3) Isostatic compaction is carried out on the silver copper oxide composite powder, the isostatic pressure is controlled to be 150MPa, and the pressure maintaining time is 180s, so that a silver copper oxide ingot blank is obtained;
(4) Carrying out vacuum liquid phase sintering on the obtained silver copper oxide ingot blank at 950 ℃ for 1.5 hours;
(5) Internal oxidation is carried out under the condition that the temperature of the sintered silver copper oxide ingot blank is reduced to 780 ℃, the partial pressure of internal oxidation oxygen is 0.6MPa, and the internal oxidation time is 5 hours;
(6) And (5) performing hot extrusion on the silver copper oxide ingot blank obtained in the step (5) to obtain the silver copper oxide contact material.
Example 2
(1) Weighing 91.4 parts of silver, 8 parts of copper, 0.4 part of copper and 0.2 part of antimony, placing the materials into a medium frequency induction smelting furnace for smelting, and then carrying out atomization powder preparation, drying and screening treatment to obtain silver-copper alloy powder;
(2) Weighing 99.3 parts of silver-copper alloy powder, 0.5 part of tungsten and 0.2 part of lanthanum oxide in a mass ratio of 8:1, and adding the mixture into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment. The low-temperature low-pressure rotary ball milling internal oxidation conditions are as follows: the temperature is 550 ℃, the oxygen partial pressure is 0.1MPa, the rotating speed is 40r/min, the internal oxidation time is 3h, and the silver copper oxide composite powder with the oxidation rate of 80 percent is obtained;
(3) Isostatic compaction is carried out on the silver copper oxide composite powder, the isostatic pressure is controlled to be 200MPa, and the pressure maintaining time is 240s, so that a silver copper oxide ingot blank is obtained;
(4) Carrying out vacuum liquid phase sintering on the obtained silver copper oxide ingot blank at the temperature of 950 ℃ for 2 hours;
(5) The sintered silver copper oxide ingot blank is subjected to internal oxidation under the condition that the temperature is reduced to 790 ℃, the partial pressure of internal oxidation oxygen is 1.0MPa, and the internal oxidation time is 6 hours;
(6) And (5) performing hot extrusion on the silver copper oxide ingot blank obtained in the step (5) to obtain the silver copper oxide contact material.
Example 3
(1) Weighing 89.7 parts of silver, 9.8 parts of copper, 0.2 part of nickel and 0.3 part of tellurium, placing the materials into a medium frequency induction smelting furnace for smelting, and then carrying out atomization powder preparation, drying and screening treatment to obtain silver-copper alloy powder;
(2) Weighing 99.4 parts of silver-copper alloy powder, 0.4 part of tungsten oxide, 0.2 part of cerium oxide and a ball material in a mass ratio of 10:1, and adding the mixture into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment. The low-temperature low-pressure rotary ball milling internal oxidation conditions are as follows: the temperature is 500 ℃, the oxygen partial pressure is 0.1MPa, the rotating speed is 45r/min, the internal oxidation time is 2h, and the silver copper oxide composite powder with the oxidation rate of 75 percent is obtained;
(3) Isostatic compaction is carried out on the silver copper oxide composite powder, the isostatic pressure is controlled to be 150MPa, and the pressure maintaining time is 180s, so that a silver copper oxide ingot blank is obtained;
(4) Carrying out vacuum liquid phase sintering on the silver copper oxide ingot blank at the temperature of 940 ℃ for 1h;
(5) The sintered silver copper oxide ingot blank is subjected to internal oxidation under the condition that the temperature is reduced to 770 ℃, the partial pressure of internal oxidation oxygen is 0.8MPa, and the internal oxidation time is 5 hours;
(6) And (5) performing hot extrusion on the silver copper oxide ingot blank obtained in the step (5) to obtain the silver copper oxide contact material.
Example 4
(1) Weighing 87.1 parts of silver, 12.2 parts of copper, 0.3 part of indium, 0.2 part of copper and 0.2 part of tellurium, placing the materials into a medium frequency induction smelting furnace for smelting, and then carrying out atomization powder preparation, drying and screening treatment to obtain silver-copper alloy powder;
(2) Weighing 99.5 parts of silver-copper alloy powder, 0.1 part of molybdenum trioxide and 0.4 part of lanthanum oxide in a mass ratio of 10:1, and adding the mixture into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment. The low-temperature low-pressure rotary ball milling internal oxidation conditions are as follows: the temperature is 550 ℃, the oxygen partial pressure is 0.1MPa, the rotating speed is 45r/min, the internal oxidation time is 1.5h, and the silver copper oxide composite powder with the oxidation rate of 78 percent is obtained;
(3) Isostatic compaction is carried out on the silver copper oxide composite powder, the isostatic pressure is controlled to be 200MPa, and the pressure maintaining time is 240s, so that a silver copper oxide ingot blank is obtained;
(4) Carrying out vacuum liquid phase sintering on the silver copper oxide ingot blank at the temperature of 935 ℃ for 1h;
(5) Internal oxidation is carried out under the condition that the temperature of the sintered silver copper oxide ingot blank is reduced to 810 ℃, the partial pressure of internal oxidation oxygen is 1.5MPa, and the internal oxidation time is 5 hours;
(6) And (5) performing hot extrusion on the silver copper oxide ingot blank obtained in the step (5) to obtain the silver copper oxide contact material.
Example 5
(1) Weighing 79 parts of silver, 18 parts of copper, 2.5 parts of indium and 0.5 part of bismuth, placing the materials into a medium-frequency induction smelting furnace for smelting, and then carrying out atomization powder preparation, drying and screening treatment to obtain silver-copper alloy powder;
(2) Weighing 97 parts of silver-copper alloy powder, 1 part of cobalt, 2 parts of tungsten carbide and a ball material in a mass ratio of 10:1, and then adding the mixture into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment. The low-temperature low-pressure rotary ball milling internal oxidation conditions are as follows: the temperature is 550 ℃, the oxygen partial pressure is 0.1MPa, the rotating speed is 50r/min, the internal oxidation time is 4 hours, and the silver copper oxide composite powder with 70 percent of oxidation rate is obtained;
(3) Isostatic compaction is carried out on the silver copper oxide composite powder, the isostatic pressure is controlled to be 300MPa, and the pressure maintaining time is 300s, so that a silver copper oxide ingot blank is obtained;
(4) Carrying out vacuum liquid phase sintering on the obtained silver copper oxide ingot blank at 890 ℃ for 2 hours;
(5) Internal oxidation is carried out under the condition that the temperature of the sintered silver copper oxide ingot blank is reduced to 850 ℃, the partial pressure of internal oxidation oxygen is 2MPa, and the internal oxidation time is 8 hours;
(6) And (5) performing hot extrusion on the silver copper oxide ingot blank obtained in the step (5) to obtain the silver copper oxide contact material.
Example 6
(1) Weighing 95 parts of silver and 5 parts of copper, placing the materials into a medium-frequency induction smelting furnace for smelting, and then carrying out atomization powder preparation, drying and screening treatment to obtain silver-copper alloy powder;
(2) And (3) weighing the silver-copper alloy powder and the ball material according to the mass ratio of 10:1, and then adding the weighed silver-copper alloy powder and ball material into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment. The low-temperature low-pressure rotary ball milling internal oxidation conditions are as follows: the temperature is 350 ℃, the oxygen partial pressure is 0.02MPa, the rotating speed is 10r/min, the internal oxidation time is 1h, and the silver copper oxide composite powder with the oxidation rate of 90 percent is obtained;
(3) Isostatic compaction is carried out on the silver copper oxide composite powder, the isostatic pressure is controlled to be 50MPa, and the pressure maintaining time is 10s, so that a silver copper oxide ingot blank is obtained;
(4) Carrying out vacuum liquid phase sintering on the obtained silver copper oxide ingot blank at the temperature of 960 ℃ for 1h;
(5) Internal oxidation is carried out under the condition that the temperature of the sintered silver copper oxide ingot blank is reduced to 700 ℃, the partial pressure of internal oxidation oxygen is 0.2MPa, and the internal oxidation time is 2 hours;
(6) And (5) performing hot extrusion on the silver copper oxide ingot blank obtained in the step (5) to obtain the silver copper oxide contact material.
Comparative example 1
(1) Weighing 91.4 parts of silver, 8 parts of copper, 0.4 part of copper and 0.2 part of antimony, placing the materials into a medium frequency induction smelting furnace for smelting, and then carrying out atomization powder preparation, drying and screening treatment to obtain silver-copper alloy powder;
(2) Placing the obtained silver-copper alloy powder into an oxidation furnace for internal oxidation, wherein the internal oxidation temperature is 720 ℃, the oxygen partial pressure is 0.6MPa, the oxidation time is 6 hours, and then ball milling and crushing the oxidized silver-copper oxide powder to obtain silver-copper oxide composite powder;
(3) Isostatic compaction is carried out on the silver copper oxide composite powder, the isostatic pressure is controlled to be 200MPa, and the pressure maintaining time is 240s, so that a silver copper oxide ingot blank is obtained;
(4) Sintering the obtained silver copper oxide ingot blank at 890 ℃ for 4 hours;
(5) And (3) carrying out hot extrusion on the silver copper oxide ingot blank prepared in the step (4) to obtain the silver copper oxide contact material.
Comparative example 2
This comparative example differs from example 2 only in that the remainder of the same is not described herein in more detail as .
The internal oxidation temperature of the low-temperature low-pressure rotary ball mill is 500 ℃, the oxygen partial pressure is 0.02MPa, the rotation speed is 40r/min, the internal oxidation time is 2h, and the silver copper oxide composite powder with the oxidation rate of 50% is obtained.
Comparative example 3
This comparative example differs from example 2 only in that the remainder of the same is not described herein in more detail as .
The conditions of vacuum liquid phase sintering are as follows: the temperature was 970℃for 2h.
Comparative example 4
This comparative example differs from example 2 only in that the remainder of the same is not described herein in more detail as .
The conditions of vacuum liquid phase sintering are as follows: the temperature was 880℃for 2h.
[ Performance detection ]
After the silver copper oxide contact materials prepared in example 2 and comparative examples 1 to 4 were processed into silver copper oxide contacts corresponding to 200A dc contactors, the electrical life of the contact materials was measured on an electrical property tester. The test parameters were as follows: test voltage DC60V; test current 200A; coil voltage 48V; energizing time 1s; the interval is 9s.
The test results are shown in table 1 below:
TABLE 1 silver copper oxide contact life and fusion welding condition test table
As shown in Table 1, compared with the traditional powder internal oxidation method, the preparation method provided by the invention can effectively improve the uniformity of the structure and the interface bonding performance of the electrical contact material, and the prepared silver-copper oxide contact has better burning loss resistance, fusion welding resistance and electrical life.
It can be seen from comparative examples 2 and 2 that, under the same conditions of the rest of the tests, the oxidation rate of the silver-copper oxide composite powder, such as 50% of that of comparative example 2, was reduced by changing the oxidation time and oxygen partial pressure of the oxidation stage in the powder, and the service life of the silver-copper oxide contact prepared at this time was only 2.1 ten thousand times, fusion welding occurred when the operation was performed to 1.4 ten thousand times, whereas the service life of the silver-copper oxide contact prepared at 80% of that of the silver-copper oxide composite powder of example 2 was as high as 3.6 ten thousand times, and the occurrence of fusion welding did not occur during the test, and it was found that not all of the silver-copper oxide contact materials prepared at the incomplete oxidation ratio in the powder had excellent electrical life and burning loss resistance.
It can be seen from comparative examples 2 and 3 that, under the same conditions of the rest of the tests, the temperature of the vacuum liquid phase sintering was increased only to be higher than the melting point of silver, and the service life of the silver copper oxide contact manufactured at this time was 1.9 ten thousand times, and fusion welding occurred when the contact was operated to 1.1 ten thousand times.
It can be seen from comparative examples 2 and 4 that, under the same conditions of the rest of the tests, the sintering temperature is reduced based on the present invention, for example, 880 ℃ in the prior art, and the service life of the silver copper oxide contact prepared at this time is closer to that of the prior art, so that the selection of the vacuum liquid phase sintering temperature has a larger influence on the fusion welding resistance, i.e. the electrical life of the silver copper oxide contact material.
In summary, the invention effectively improves the burning resistance, fusion welding resistance and electric life of the silver copper oxide contact material through the ingenious combination of a plurality of technical schemes and the good control of the numerical range.
Claims (5)
1. A method for preparing a silver copper oxide contact material, comprising the steps of:
(1) Smelting and atomizing to prepare powder: weighing 79-95 parts of silver, 5-18 parts of copper and 0-3 parts of metal simple substance to obtain a mixture, and atomizing the mixture to prepare powder after smelting in a medium-frequency smelting furnace to obtain silver-copper alloy powder; the metal simple substance comprises one or more of Sn, in, ni, zn, bi, al, te, sb;
(2) Powder internal oxidation: adding silver-copper alloy powder, additive powder and ball material into a rotary internal oxidation furnace for low-temperature low-pressure rotary ball milling internal oxidation treatment to obtain silver-copper oxide composite powder with oxidation rate of 70-90%, wherein the additive powder comprises Co, fe, W, mo, co 2 O 3 、Fe 2 O 3 、WO 3 、MoO 3 、La 2 O 3 、Y 2 O 3 、CeO 2 One or more of WC, tiC, tiN powder; the silver copper oxide composite powder comprises the following components in parts by mass: 97-100 parts of silver-copper alloy powder and 0-3 parts of additive powder; the conditions of the low-temperature low-pressure rotary ball milling internal oxidation are as follows: the temperature is 350-550 ℃, the oxygen partial pressure is 0.02-0.1 MPa, the rotation speed is 10-50 r/min, and the internal oxidation time is 1-4 h;
(3) Isostatic compaction: isostatic compaction is carried out on the silver copper oxide composite powder to obtain silver copper oxide ingot blanks;
(4) Vacuum liquid phase sintering: vacuum liquid phase sintering is carried out on the silver copper oxide ingot blank at the temperature of more than or equal to 890 ℃ and less than 962 ℃;
(5) Internal oxidation: reducing the temperature, and carrying out further internal oxidation on the sintered silver copper oxide ingot blank; the internal oxidation conditions are as follows: the temperature is 700-850 ℃, the oxygen partial pressure is 0.2-2.0 MPa, and the time is 2-8 h;
(6) Extruding: and (5) carrying out hot extrusion on the product obtained in the step (5) to obtain the silver copper oxide contact material.
2. The method according to claim 1, wherein the isostatic compaction conditions in step (3) are: isostatic pressure of 50-300 MPa and dwell time of 10-300 s.
3. The method according to claim 1, wherein the conditions for vacuum liquid phase sintering in step (4) are: the temperature is 890-940 ℃ and the time is 1-2 h.
4. A silver copper oxide contact material produced by the production method according to any one of claims 1 to 3.
5. Use of a method according to any one of claims 1 to 3 or a silver copper oxide contact material according to claim 4 for the production of silver copper oxide contacts.
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| CN103184384B (en) * | 2013-03-12 | 2015-12-09 | 宁波汉博贵金属合金有限公司 | A kind of preparation method of Composite silver stannic oxide electric contact material |
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