CN115927900B - Ag-Ti3SiC2Component regulation method of electric contact material - Google Patents
Ag-Ti3SiC2Component regulation method of electric contact material Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 40
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052709 silver Inorganic materials 0.000 claims abstract description 81
- 239000004332 silver Substances 0.000 claims abstract description 76
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 36
- 230000008595 infiltration Effects 0.000 claims abstract description 30
- 238000001764 infiltration Methods 0.000 claims abstract description 30
- 239000011812 mixed powder Substances 0.000 claims abstract description 29
- 238000007731 hot pressing Methods 0.000 claims abstract description 23
- 239000013354 porous framework Substances 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims description 46
- 238000010438 heat treatment Methods 0.000 claims description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- 239000003517 fume Substances 0.000 claims description 7
- 239000011268 mixed slurry Substances 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
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- 230000001105 regulatory effect Effects 0.000 claims 1
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- 238000011065 in-situ storage Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910009817 Ti3SiC2 Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of silver-based electric contact materials, and particularly relates to a component regulation and control method of an Ag-Ti 3SiC2 electric contact material. According to the method, silver powder and Ti 3SiC2 powder are weighed to prepare mixed powder, the corresponding hot-pressing sintering temperature and pressure are matched according to the addition amount of the silver powder, a mixed powder porous framework with a Ti 3SiC2 continuous three-dimensional interpenetrating structure is prepared, and then the metal silver is infiltrated at a high temperature, so that the Ag-Ti 3SiC2 electric contact material with continuous two phases and high metal silver content is obtained. Compared with the skeleton molding and high-temperature infiltration process, the method improves the proportion of silver content in the electric contact material by a metal occupation method, is beneficial to improving the conductivity of the electric contact material, can reduce closed pores formed by Ti 3SiC2 powder, is beneficial to improving the toughness of the electric contact material, and ensures the electric contact material to have the characteristics of arc erosion resistance, fusion welding resistance, wear resistance and the like.
Description
Technical Field
The invention belongs to the technical field of silver-based electric contact materials, and particularly relates to a component regulation and control method of an Ag-Ti3SiC2 electric contact material.
Background
Silver is widely used as an electric contact material for low-voltage appliances, communication and aerospace electric contact components because of excellent electric conduction, thermal conduction, good processability and good oxidation resistance. However, the silver contact has low hardness, low melting point, poor arc erosion resistance and wear resistance, and has great limitation on application, and particularly under the condition of long-term low voltage, the silver contact is not resistant to electric wear and tear, and is easy to generate arc erosion and fusion welding phenomena to influence the stable operation of a power circuit. The metal ceramic Ti 3SiC2 is a ternary lamellar compound with excellent performances of metal and ceramic, and has the characteristics of good metal electrical conductivity, thermal conductivity and processability, high hardness, high melting point, high thermal stability, oxidation resistance, wear resistance and the like. The ternary layered Ti 3SiC2 metal ceramic is used as a reinforcing phase, has good wettability with silver, and does not generate in-situ reaction. Compared with the traditional ceramic material, the Ti 3SiC2 reinforced silver-based composite material is prepared on the premise of good electric conduction, heat conduction and high strength, and the arc erosion resistance, fusion welding resistance, mechanical property and wear resistance of the composite material are improved.
At present, the related technology is searched as follows regarding a component regulation method of an infiltration Ag-Ti 3SiC2 electric contact material: (1) The invention of patent publication No. CN 110499435A is a silver-based electric contact material and a preparation method thereof; (2) The invention of patent publication No. CN 101343700A is an Ag/Ti 3SiC2 electric contact material and a preparation process thereof; (3) The patent publication No. CN 102312150A is named Ag/Ti 3SiC2 electric contact composite material. The preparation technology of the silver-based electric contact material mainly comprises a powder metallurgy process, wherein Ti 3SiC2 powder or Ti 3SiC2 powder subjected to silver plating treatment, silver powder or silver alloy powder and other additives are subjected to ball milling and mixing uniformly, sintering, hot extrusion treatment and other processes, so that the silver-based electric contact material with Ti 3SiC2 as a reinforcing phase is obtained. By adopting a powder metallurgy process, the Ti 3SiC2 is used as a silver-based electric contact material of a reinforcing phase, compared with a matrix, the reinforcing phase has low addition content, so that the reinforcing phase is unevenly and discontinuously distributed in the matrix, the mechanical property, arc erosion resistance, fusion welding resistance and wear resistance of the silver-based electric contact material are seriously influenced, and particularly under the action of an arc, silver liquid drops are easily evaporated and splashed in a silver-rich area, so that the contact point of the electric contact material is invalid.
The technology is a technology of preparing a ceramic Ti 3SiC2 skeleton and re-infiltrating metal, the retrieved technology is patent application number 202210312764.9, the invention is named as a silver-Ti 3SiC2 electric contact material and a preparation method thereof, the technology adopts hot-pressed sintering pure Ti 3SiC2 powder to prepare a porous Ti 3SiC2 skeleton, and finally, the high-temperature infiltration of metallic silver is carried out to obtain the Ti 3SiC2 reinforced silver-based electric contact material, wherein the hot-pressed sintering temperature of the skeleton is not lower than 900 ℃, the technology is favorable for improving the strength of the silver-based electric contact material, the bending strength is not lower than 520MPa, and the silver-based electric contact material has good arc erosion resistance and wear resistance. However, the process is influenced by the hot-pressing sintering temperature and the hot-pressing sintering pressure, the porosity of the framework cannot be further improved, and the content of metallic silver in the prepared electric contact material cannot be improved, so that the electric contact material is poor in electric conductivity, and the electric conductivity is not higher than 7.5MS/m; secondly, ti 3SiC2 powder generates closed pores in a framework at the higher hot-press sintering temperature of 1200 ℃ and 1400 ℃ due to arch bridge effect, so that molten silver cannot fill the pores to become defects, the proportion and connectivity of metallic silver in the silver-based electric contact material are seriously affected, and the silver-based electric contact material is low in conductivity, poor in toughness and easy to cause brittle fracture.
Therefore, the patent develops a component regulation and control method of the infiltration Ag-Ti 3SiC2 electric contact material, has important significance for improving the performance and service reliability of the electric contact material, and is hopeful to be used as a novel silver-based electric contact material to replace the existing oxide and carbide reinforced silver-based electric contact material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a component regulation method of an Ag-Ti 3SiC2 electric contact material, which mainly aims to prepare a silver-based electric contact material with excellent electric conduction and thermal conductivity, high strength and abrasion resistance by a simple process.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
A component regulation and control method of an Ag-Ti 3SiC2 electric contact material comprises the following steps:
Step 1, preparing mixed powder: filling Ti 3SiC2 powder and silver powder into a container with alcohol according to a certain proportion, fully immersing the mixed powder with alcohol, filling zirconium balls, performing wet ball milling, pouring the mixed slurry into the container after the mixing is completed, performing powder precipitation, removing upper alcohol, and drying until the alcohol volatilizes to obtain Ti 3SiC2 -Ag mixed powder;
Step 2, preparing a Ti 3SiC2 -Ag composite porous framework: placing Ti 3SiC2 -Ag mixed powder into a mould, placing the mould into a hot-pressing sintering furnace, matching corresponding hot-pressing sintering temperature and pressure according to the addition amount of silver powder, and then sintering under the protection atmosphere and/or vacuum condition to obtain a Ti 3SiC2 -Ag composite porous skeleton;
Step 3, a high-temperature infiltration step: putting a silver block and Ti 3SiC2 -Ag composite porous skeleton into a container, adding the silver block in an amount sufficient to fill the skeleton gaps, putting the container into a furnace chamber of a heating furnace, and carrying out high-temperature infiltration treatment under the protection atmosphere and/or vacuum conditions to finally obtain the Ag-Ti 3SiC2 electric contact material.
In the step 1, the ball milling mixing time is at least 48 hours.
In the step 1, the drying treatment is carried out in a fume hood or a 40 ℃ drying oven.
In the step 1, the raw material powder is Ti 3SiC2 powder and silver powder, wherein the size of the Ti 3SiC2 powder is 0.5-50 mu m, the size of the silver powder is 3-25 mu m, the volume fraction of the silver powder is 20-30%, and the volume fraction of the Ti 3SiC2 powder is 70-80%.
In the step 2, the hot-pressed sintering is performed at a heating rate of 10 ℃/min, the temperature is raised to 750-800 ℃ from the room temperature, the pressure is increased from 0 to 5-10 MPa while heating is started, the furnace cooling and pressure maintaining are carried out, the furnace cooling is carried out, and the heat preservation and pressure maintaining time of the sintering treatment is 0.5-1 h.
In the step2, the vacuum degree is 10 -3 Pa, and the protective atmosphere is argon.
In the step 2, the porosity of the Ti 3SiC2 -Ag composite porous skeleton is 25-50%.
In the step 3, the silver block is 90-120 g.
In the step 3, the temperature in the furnace chamber of the heating furnace is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then is raised to the infiltration treatment temperature of 1100-1300 ℃ at the temperature raising speed of 5 ℃/min, the heat preservation time is at least 1h, and finally the furnace is cooled to the room temperature; the high temperature infiltration treatment temperature is higher than the melting point of silver.
In the step 3, silver blocks are placed on the Ti 3SiC2 -Ag composite porous framework up and down.
In the step 2 and the step 3, the crucible and the die are made of graphite.
In the method, the volume fraction of silver in the Ag-Ti 3SiC2 electric contact material is 40% -70%, preferably 45% -65%, and the balance is Ti 3SiC2.
Preferably, the bending strength of the Ag-Ti 3SiC2 electric contact material is 700-900 Mpa.
Preferably, the fracture toughness value of the Ag-Ti 3SiC2 electric contact material is 15-20 MPa m 1/2.
Preferably, the hardness of the Ag-Ti 3SiC2 electric contact material is 1.2-1.5 GPa.
Preferably, the conductivity of the Ag-Ti 3SiC2 electric contact material is 15.5-21.7 MS/m.
Compared with the prior art, the component regulation method of the Ag-Ti 3SiC2 electric contact material has the following beneficial effects:
The invention provides a component regulation method of an infiltration Ag-Ti 3SiC2 electric contact material, which adopts a metal occupation method, mixes silver powder and Ti 3SiC2 in a certain proportion by a wet method to prepare mixed powder, selects matched hot-pressing sintering temperature and pressure according to the added silver powder amount to prepare a Ti 3SiC2 -Ag composite porous skeleton, and finally infiltrates metallic silver at high temperature to obtain the silver-based electric contact material. The purpose of adding silver powder is to occupy space, and then the silver powder is melted through infiltration. The composite material prepared by mixing silver powder with other powder and adopting a powder metallurgy process has the problem that impurities such as oxide films of the silver powder are difficult to avoid to introduce, and impurities can be reduced to a great extent by adopting infiltration block silver. Compared with a powder metallurgy process and a framework infiltration method, the regulation and control method can effectively regulate and control the silver content in the electric contact material, wherein the regulation and control method can be matched with corresponding hot-pressing sintering temperature and pressure according to the addition amount of silver powder, so that not only can the silver powder contained in mixed powder be prevented from being extruded, but also the contact area between Ti 3SiC2 powder can be reduced by the added silver powder, the Ti 3SiC2 phase in the Ti 3SiC2 -Ag composite porous framework can be ensured to form a continuous three-dimensional interpenetrating structure, and then the metallic silver is infiltrated at a high temperature, so that the Ag-Ti 3SiC2 electric contact material with continuous two phases and high metallic silver content can be obtained, namely the electric contact material has the characteristics of fusion welding resistance, self lubrication resistance, arc erosion resistance and mechanical property and wear resistance on the premise of ensuring that the electric contact material has good electric conductivity and thermal conductivity.
The foregoing description is only an overview of the present invention, and is intended to provide a better understanding of the present invention, as it is embodied in the following description, with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is an XRD pattern of Ti 3SiC2 used in a method of modulating the composition of an infiltrated Ag-Ti 3SiC2 electrical contact material;
FIG. 2 is a macroscopic view of the composite porous Ti 3SiC2 -Ag skeleton prepared in example 1 of the present invention;
FIG. 3 is a microstructure of the Ti 3SiC2 -Ag composite porous matrix prepared in example 1 of the present invention;
FIG. 4 is a macroscopic photograph of the prepared Ag-Ti 3SiC2 electrical contact material according to example 1 of the present invention;
FIG. 5 is a microstructure chart of the Ag-Ti 3SiC2 electrical contact material prepared according to example 1 of the present invention (where the bright color is Ag and the dark color is Ti 3SiC2);
FIG. 6 is an in-situ fracture toughness force versus displacement curve for an Ag-Ti 3SiC2 electrical contact material prepared in accordance with example 1 of the present invention;
FIG. 7 is a stable crack deflection of the prepared Ag-Ti 3SiC2 electrical contact material according to example 1 of the present invention;
FIG. 8 is a microstructure chart of the Ag-Ti 3SiC2 electrical contact material prepared according to example 2 of the present invention (where the bright color is Ag and the dark color is Ti 3SiC2);
FIG. 9 is an in-situ fracture toughness force versus displacement curve for an Ag-Ti 3SiC2 electrical contact material prepared in accordance with example 2 of the present invention;
FIG. 10 is a stable crack deflection of the prepared Ag-Ti 3SiC2 electrical contact material according to example 2 of the present invention;
FIG. 11 is a microstructure chart of the prepared Ag-Ti 3SiC2 electrical contact material (where the bright color is Ag and the dark color is Ti 3SiC2) according to comparative example 3;
FIG. 12 is a plot of fracture toughness force versus displacement for the prepared Ag-Ti 3SiC2 electrical contact material according to comparative example 3;
Detailed Description
In order to further describe the technical means and effects adopted for achieving the preset aim of the invention, the following detailed description refers to the specific implementation, structure, characteristics and effects according to the application of the invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
The specific scheme of the invention is as follows:
The embodiment of the invention provides a component regulation and control method of an infiltration Ag-Ti 3SiC2 electric contact material. The electrical contact material is prepared by mixing micron-sized or nano-sized silver powder with ceramic powder Ti 3SiC2, obtaining a Ti 3SiC2 -Ag composite porous framework through a hot-pressing sintering process, and finally filling the composite porous framework through high-temperature infiltration silver to obtain the Ti 3SiC2 -Ag electrical contact material with a three-dimensional interpenetrating structure on a microcosmic scale; in the hot-press sintering process, corresponding hot-press sintering temperature is matched according to the addition amount of silver powder, so that not only is the silver powder contained in the mixed powder prevented from being extruded, but also the contact area between Ti 3SiC2 powder can be reduced by the added silver powder, and the Ti 3SiC2 phase in the Ti 3SiC2 -Ag composite porous skeleton is ensured to form a continuous three-dimensional interpenetrating structure. The preferable temperature is 600-900 ℃, the pressure applied to the raw material mixed powder is 0.1-40MPa, and the heat preservation and pressure maintaining time of sintering treatment is 0.5-3h; the volume fraction of silver is 40% -70%, preferably 45% -65%.
The invention is further illustrated below by means of specific experimental examples:
Examples 1-5 hot press sintering and high temperature infiltration were performed using the same furnace equipment with a graphite mold and graphite crucible having a diameter of 50 mm.
Example 1
The embodiment adopts a component regulation and control method of an infiltration Ag-Ti 3SiC2 electric contact material, which comprises the following preparation steps:
step 1, preparing Ti 3SiC2 -30vol% Ag mixed powder: weighing 36g of Ti 3SiC2 powder with the average particle size of 24 mu m and 35.7g of silver powder with the average particle size of 3 mu m, adding 100ml of alcohol and a small amount of zirconium balls, mixing for 48 hours on a rolling ball mill, pouring the mixed slurry into a beaker after mixing, precipitating the powder, removing upper alcohol, putting the powder into a fume hood or a 40 ℃ drying oven for low-temperature drying treatment, volatilizing the alcohol to obtain mixed powder;
Step 2, preparing the Ti 3SiC2 -Ag composite porous framework through hot-pressing sintering: adding the mixed and dried Ti 3SiC2 -Ag mixed powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, vacuumizing to 10 -3 Pa, closing vacuum, introducing flowing argon, heating under a protective atmosphere at a heating rate of 10 ℃/min, heating from room temperature to 750 ℃, preserving heat for 1h, heating while keeping the pressure from 0 to 10Mpa, keeping the pressure while cooling the furnace, and taking out after the furnace is cooled to room temperature to obtain the Ti 3SiC2 -Ag composite porous skeleton with certain strength;
Step 3, a high-temperature infiltration step: 90g of silver block was weighed. Then, placing the Ti 3SiC2 -Ag composite porous skeleton and silver blocks in a clean graphite crucible, placing the silver blocks on the Ti 3SiC2 -Ag composite porous skeleton, and placing the crucible in a furnace chamber of a heating furnace. Under the protection atmosphere, the temperature is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then raised to 1250 ℃ at the temperature raising speed of 5 ℃/min, the temperature is kept for 1h, and finally the furnace is cooled to the room temperature.
FIG. 1 is an XRD pattern of Ti 3SiC2 used; FIG. 3 is a microstructure of a porous skeleton of an Ag-Ti 3SiC2 electric contact material obtained in example 1 of the present invention, and FIG. 2 is a microstructure of a porous skeleton of an Ag-Ti 3SiC2 electric contact material obtained; FIG. 5 shows the microstructure of the Ag-Ti 3SiC2 electrical contact material according to example 1 of the present invention, and FIG. 4 shows the microstructure of the Ag-Ti 3SiC2 electrical contact material according to example 1 of the present invention, in which the metallic silver is sufficiently infiltrated, without defects, and the volume fraction of the base metallic silver is 55%; FIGS. 6 and 7 show the force versus displacement curve and stable crack deflection for the fracture toughness test of the Ag-Ti 3SiC2 electrical contact material obtained in example 1 of the present invention, which was calculated to have a fracture toughness K IC＝17.3±2MPa·m1/2, a flexural strength of 720.+ -. 10MPa, a conductivity of 21.+ -. 0.7MS/m, and a hardness of 1.17 G.+ -. 0.06Pa.
Example 2
A component regulation method of an infiltration Ag-Ti 3SiC2 electric contact material comprises the following preparation steps:
Step 1, preparing Ti 3SiC2 -20vol% Ag mixed powder: weighing 36g of Ti 3SiC2 powder with the average particle size of 24 mu m and 20.8g of silver powder with the average particle size of 3 mu m, adding 100ml of alcohol and a small amount of zirconium balls, mixing for 48 hours on a rolling ball mill, pouring the mixed slurry into a beaker after mixing, precipitating the powder, removing upper alcohol, putting the powder into a fume hood or a 40 ℃ drying oven for low-temperature drying treatment, volatilizing the alcohol to obtain mixed powder;
Step 2, preparing the Ti 3SiC2 -Ag composite porous framework through hot-pressing sintering: adding the mixed and dried Ti 3SiC2 -Ag mixed powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, vacuumizing to 10 -3 Pa, closing vacuum, introducing flowing argon, heating under a protective atmosphere at a heating rate of 10 ℃/min, heating from room temperature to 800 ℃, preserving heat for 1h, heating while keeping the pressure from 0 to 10Mpa, keeping the pressure while cooling the furnace, and taking out after the furnace is cooled to room temperature to obtain the Ti 3SiC2 -Ag composite porous skeleton with certain strength;
Step 3, a high-temperature infiltration step: 120g of silver block was weighed. Then, placing the Ti 3SiC2 -Ag composite porous skeleton and silver blocks in a clean graphite crucible, placing the silver blocks on the Ti 3SiC2 -Ag composite porous skeleton, and placing the crucible in a furnace chamber of a heating furnace. Under the protection atmosphere, the temperature is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then raised to 1250 ℃ at the temperature raising speed of 5 ℃/min, the temperature is kept for 1h, and finally the furnace is cooled to the room temperature.
FIG. 8 is a microstructure of the Ag-Ti 3SiC2 electrical contact material obtained in example 2 of the present invention, showing that the metallic silver is fully infiltrated, defect-free, and the volume fraction of the base metallic silver is 52%; FIGS. 9 and 10 are force versus displacement curves and stable crack deflection, respectively, for the Ag-Ti 3SiC2 electrical contact material prepared in example 2, which was calculated to have a fracture toughness K IC＝19.3±0.6MPa·m1/2, a flexural strength of 780+ -20 MPa, a conductivity of 17.8+ -0.5 MS/m, and a hardness value of 1.25+ -0.04 GPa.
Example 3
A component regulation method of an infiltration Ag-Ti 3SiC2 electric contact material comprises the following preparation steps:
Step 1, preparing Ti 3SiC2 -30vol% Ag mixed powder: weighing 35.7g of Ti 3SiC2 powder with the average particle size of 48 mu m and 20.8g of silver powder with the average particle size of 24 mu m, adding 100ml of alcohol and a small amount of zirconium balls, mixing for 48 hours on a rolling ball mill, pouring the mixed slurry into a beaker after mixing, precipitating the powder, removing upper alcohol, placing in a fume hood or a 40 ℃ drying oven for low-temperature drying treatment, volatilizing the alcohol to obtain mixed powder;
Step 2, preparing the Ti 3SiC2 -Ag composite porous framework through hot-pressing sintering: adding the mixed and dried Ti 3SiC2 -Ag mixed powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, vacuumizing to 10 -3 Pa, closing vacuum, introducing flowing argon, heating under a protective atmosphere at a heating rate of 10 ℃/min, heating from room temperature to 750 ℃, preserving heat for 1h, heating while keeping the pressure from 0 to 5Mpa, cooling the furnace to room temperature, and taking out to obtain the Ti 3SiC2 -Ag composite porous skeleton with certain strength;
Step 3, a high-temperature infiltration step: 90g of silver block was weighed. Then, placing the Ti 3SiC2 -Ag composite porous skeleton and silver blocks in a clean graphite crucible, placing the silver blocks on the Ti 3SiC2 -Ag composite porous skeleton, and placing the crucible in a furnace chamber of a heating furnace. Under the protection atmosphere, the temperature is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then is raised to 1150 ℃ at the temperature raising speed of 5 ℃/min, is kept for 1h, and finally is cooled to the room temperature.
Example 4
A component regulation method of an infiltration Ag-Ti 3SiC2 electric contact material comprises the following preparation steps:
Step 1, preparing Ti 3SiC2 -20vol% Ag mixed powder: weighing 36g of Ti 3SiC2 powder with the average particle size of 48 mu m and 20.84g of silver powder with the average particle size of 24 mu m, adding 100ml of alcohol and a small amount of zirconium balls, mixing for 48 hours on a rolling ball mill, pouring the mixed slurry into a beaker after mixing, precipitating the powder, removing upper alcohol, putting the powder into a fume hood or a 40 ℃ drying oven for low-temperature drying treatment, volatilizing the alcohol to obtain mixed powder;
Step 2, preparing the Ti 3SiC2 -Ag composite porous framework through hot-pressing sintering: adding the mixed and dried Ti 3SiC2 -Ag mixed powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, vacuumizing to 10 -3 Pa, closing vacuum, introducing flowing argon, heating under a protective atmosphere at a heating rate of 10 ℃/min, heating from room temperature to 800 ℃, preserving heat for 0.5h, starting heating, simultaneously, keeping the pressure from 0 to 10Mpa, keeping the pressure while cooling the furnace, and taking out after the furnace is cooled to room temperature to obtain the Ti 3SiC2 -Ag composite porous skeleton with certain strength;
Step 3, a high-temperature infiltration step: 120g of silver block was weighed. Then, placing the Ti 3SiC2 -Ag composite porous skeleton and silver blocks in a clean graphite crucible, placing the silver blocks on the Ti 3SiC2 -Ag composite porous skeleton, and placing the crucible in a furnace chamber of a heating furnace. Under the protection atmosphere, the temperature is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then raised to 1250 ℃ at the temperature raising speed of 5 ℃/min, the temperature is kept for 1h, and finally the furnace is cooled to the room temperature.
Example 5
A component regulation method of an infiltration Ag-Ti 3SiC2 electric contact material comprises the following preparation steps:
Step 1, preparing Ti 3SiC2 -20vol% Ag mixed powder: weighing 36g of Ti 3SiC2 powder with the average particle size of 0.7 mu m and 20.84g of silver powder with the average particle size of 3 mu m, adding 100ml of alcohol and a small amount of zirconium balls, mixing for 48 hours on a rolling ball mill, pouring the mixed slurry into a beaker after mixing, precipitating the powder, removing upper alcohol, placing in a fume hood or a 40 ℃ drying oven for low-temperature drying treatment, volatilizing the alcohol to obtain mixed powder;
Step 2, preparing the Ti 3SiC2 -Ag composite porous framework through hot-pressing sintering: adding the mixed and dried Ti 3SiC2 -Ag mixed powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, vacuumizing to 10 -3 Pa, closing vacuum, introducing flowing argon, heating under a protective atmosphere at a heating rate of 10 ℃/min, heating from room temperature to 800 ℃, preserving heat for 1h, heating while keeping the pressure from 0 to 5Mpa, cooling the furnace to room temperature, and taking out to obtain the Ti 3SiC2 -Ag composite porous skeleton with certain strength;
Step 3, a high-temperature infiltration step: 120g of silver block was weighed. Then, placing the Ti 3SiC2 -Ag composite porous skeleton and silver blocks in a clean graphite crucible, placing the silver blocks on the Ti 3SiC2 -Ag composite porous skeleton, and placing the crucible in a furnace chamber of a heating furnace. Under the protection atmosphere, the temperature is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then raised to 1200 ℃ at the temperature raising speed of 5 ℃/min, the heat is preserved for 1h, and finally the furnace is cooled to the room temperature.
Comparative example
This example is a comparative example, in which a Ti 3SiC2 -Ag composite porous matrix was infiltrated with metallic silver to prepare an Ag-Ti 3SiC2 electrical contact material. Wherein the adopted raw materials comprise Ti 3SiC2 powder with an average particle size of 24 mu m and pure silver blocks.
The preparation method comprises the following preparation steps:
step 1, preparing a Ti 3SiC2 -Ag composite porous framework by hot-pressing sintering: weighing 36g of Ti 3SiC2 powder, adding the powder into a graphite mold, placing the graphite mold into a hot-pressing sintering furnace, vacuumizing to a vacuum degree of 10 -3 Pa, closing the vacuum, introducing flowing argon, heating under a protective atmosphere, heating at a heating rate of 10 ℃/min from room temperature to 800 ℃, preserving heat for 1h, heating while starting to heat, keeping the pressure from 0 to 10Mpa, keeping the pressure while cooling the furnace, and taking out the furnace after the furnace is cooled to the room temperature to obtain the Ti 3SiC2 -Ag composite porous skeleton with certain strength;
Step 2, a high-temperature infiltration step: 150g of silver block was weighed. Then, placing the Ti 3SiC2 -Ag composite porous skeleton and silver blocks in a clean graphite crucible, placing the silver blocks on the Ti 3SiC2 -Ag composite porous skeleton, and placing the crucible in a furnace chamber of a heating furnace. Under the protection atmosphere, the temperature is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then raised to 1250 ℃ at the temperature raising speed of 5 ℃/min, the temperature is kept for 1h, and finally the furnace is cooled to the room temperature.
Fig. 11 is a microstructure chart of the comparative example preparation Ti 3SiC2 -Ag electrical contact material, the volume fraction of the base metal silver is 45%, it can be seen that the ratio of the base metal silver is lower than that of examples 1 and 2, and fig. 12 is a force versus displacement curve of the fracture toughness test of the comparative example 3 preparation Ti 3SiC2 -Ag electrical contact material, it can be judged that brittle fracture occurs in the comparative example preparation Ti 3SiC2 -Ag electrical contact material due to the low content of the metal silver. The bending strength of the Ti 3SiC2 -Ag electric contact material is 850Mpa, the electric conductivity is 15.5+/-0.5 MS/m, and the hardness value is 1.4+/-0.05 Gpa.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (4)
1. A component regulation and control method of an Ag-Ti 3SiC2 electric contact material comprises the following steps:
Step 1, preparing mixed powder: filling Ti 3SiC2 powder and silver powder into a container with alcohol according to a certain proportion, fully immersing the mixed powder with alcohol, filling zirconium balls, performing wet ball milling, pouring the mixed slurry into the container after the mixing is completed, performing powder precipitation, removing upper alcohol, and drying until the alcohol volatilizes to obtain Ti 3SiC2 -Ag mixed powder;
Step 2, preparing a Ti 3SiC2 -Ag composite porous framework: placing Ti 3SiC2 -Ag mixed powder into a mould, placing the mould into a hot-pressing sintering furnace, matching corresponding hot-pressing sintering temperature and pressure according to the addition amount of silver powder, and then sintering under the protection atmosphere and/or vacuum condition to obtain a Ti 3SiC2 -Ag composite porous skeleton;
Step 3, a high-temperature infiltration step: putting a silver block and Ti 3SiC2 -Ag composite porous skeleton into a container, wherein the adding amount of the silver block is enough to fill a skeleton gap, putting the container into a furnace chamber of a heating furnace, and carrying out high-temperature infiltration treatment under vacuum and/or protective atmosphere to finally obtain an Ag-Ti 3SiC2 electric contact material; the temperature of the high-temperature infiltration treatment is higher than the melting point of silver;
in the step 1, the ball milling mixing time is at least 48 hours, and drying treatment is carried out in a fume hood or a drying oven at 40 ℃;
In the step 1, the size of Ti 3SiC2 powder is 0.5-50 mu m, the size of silver powder is 3-25 mu m, the volume fraction of the silver powder is 20% -30%, and the volume fraction of Ti 3SiC2 powder is 70% -80%;
In the step 2, hot-pressing sintering is performed at a heating rate of 10 ℃/min, the temperature is raised to 750-800 ℃ from room temperature, the pressure is increased from 0 to 5-10 MPa while heating is started, the heat preservation and pressure maintaining time of sintering treatment is 0.5-1 h, furnace cooling and pressure maintaining are carried out, and the mold is taken out after the furnace cooling is carried out to room temperature, wherein the material of the mold is graphite;
in the step3, silver blocks are placed on the Ti 3SiC2 -Ag composite porous framework up and down;
The bending strength of the Ag-Ti 3SiC2 electric contact material is 700-900 MPa, the fracture toughness value is 15-20 MPa ∙ m 1/2, the hardness is 1.2-1.5 gpa, and the conductivity is 15.5-21.7 MS/m;
the volume fraction of silver in the Ag-Ti 3SiC2 electric contact material is 40% -70%, and the balance is Ti 3SiC2.
2. The method for controlling the composition of an Ag-Ti 3SiC2 electrical contact material according to claim 1, wherein in the step 2, the vacuum degree is 10 -3 Pa, and the protective atmosphere is argon.
3. The method for regulating and controlling the composition of the Ag-Ti 3SiC2 electric contact material according to claim 1, wherein in the step 2, the porosity of the Ti 3SiC2 -Ag composite porous skeleton is 25-50%.
4. The method for controlling the composition of an ag—ti 3SiC2 electrical contact material according to claim 1, wherein in the step 3, the temperature in the furnace chamber of the heating furnace is raised from room temperature to 1000 ℃ at a rate of 10 ℃/min, then raised to the infiltration treatment temperature of 1100-1300 ℃ at a rate of 5 ℃/min, the heat preservation time is at least 1h, and finally the furnace is cooled to room temperature, and the container is a graphite crucible.
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