CN115927900A - Ag-Ti 3 SiC 2 Component regulation and control method of electric contact material - Google Patents
Ag-Ti 3 SiC 2 Component regulation and control method of electric contact material Download PDFInfo
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- 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
- 238000001035 drying Methods 0.000 claims description 20
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Abstract
The invention belongs to the technical field of silver-based electric contact materials, and particularly relates to Ag-Ti 3 SiC 2 A component regulating method of an electric contact material. The method weighs silver powder and Ti 3 SiC 2 The powder is prepared into mixed powder, and the Ti-containing powder is prepared by matching the corresponding hot-pressing sintering temperature and pressure according to the addition amount of the silver powder 3 SiC 2 The mixed powder porous framework with the phase-continuous three-dimensional interpenetrating structure is infiltrated with the metallic silver at high temperature to obtain two phases of continuous Ag-Ti with high metallic silver content 3 SiC 2 An electrical contact material. Compared with the framework forming and high-temperature infiltration process, the method improves the proportion of the silver content in the electric contact material by a metal occupying method, is favorable for improving the electric conductivity of the electric contact material, and can reduce Ti 3 SiC 2 The closed pores formed by the powder are beneficial to improving the toughness of the electric contact material, and simultaneously, the electric contact material is ensured 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 has excellent electrical conductivity, thermal conductivity, good processability and good oxidation resistance, and is widely applied to electrical contact components of low-voltage electrical appliances, communication and aerospace as an electrical contact material. However, the silver contact has low hardness, low melting point, poor arc erosion resistance and poor abrasion resistance, and has great limitation on the application of the silver contact, and particularly, under the condition of long-term low voltage, the silver contact has no resistance to electrical abrasion, and is easy to generate arc erosion and fusion welding phenomena to influence the stable operation of a power circuit. Cermet of Ti 3 SiC 2 The ternary layered compound has excellent metal and ceramic performances, and has the characteristics of good metal conductivity, heat conductivity and machinability, high hardness, high melting point, high thermal stability, oxidation resistance, wear resistance and the like of ceramics. Ternary layered Ti 3 SiC 2 The cermet is used as a reinforcing phase, has good wettability with silver, and does not generate in-situ reaction. Compared with the conventional ceramic material, ti 3 SiC 2 The reinforced silver-based composite material is prepared on the premise of good electric conductivity, heat conductivity and high strengthThe electric arc erosion resistance, the fusion welding resistance, the mechanical property and the wear resistance are improved.
At present, it is about to impregnate Ag-Ti with an alloy 3 SiC 2 The component regulation and control method of the electric contact material comprises the following searched related technologies: (1) The invention discloses a silver-based electric contact material and a preparation method thereof, wherein the patent publication No. CN 110499435A discloses a silver-based electric contact material and a preparation method thereof; (2) The invention name of patent publication No. CN 101343700A is Ag/Ti 3 SiC 2 An electric contact material and a preparation process thereof; (3) Patent publication No. CN 102312150A invention name is Ag/Ti 3 SiC 2 A preparation method of the electric contact composite material. The preparation technology of the silver-based electric contact material is mainly a powder metallurgy process, and Ti is added 3 SiC 2 Powder or silver-plated Ti 3 SiC 2 The powder, silver powder or silver alloy powder and other additives are subjected to processes of ball milling, uniform mixing, sintering, hot extrusion treatment and the like to obtain Ti 3 SiC 2 A silver-based electrical contact material for the enhancement phase. By powder metallurgy process with Ti 3 SiC 2 Compared with the matrix, the silver-based electric contact material serving as the reinforcing phase has low addition content of the reinforcing phase, so that the reinforcing phase is unevenly and discontinuously distributed in the matrix, the mechanical property, the arc erosion resistance, the fusion welding resistance and the wear resistance of the silver-based electric contact material are seriously influenced, and particularly under the action of an electric arc, silver droplets are easily evaporated and splashed in a silver-rich area, so that a contact of the electric contact material fails.
By preparing ceramic Ti 3 SiC 2 The process of skeleton and re-infiltration of metal is found in patent application No. 202210312764.9 entitled silver-Ti 3 SiC 2 The electric contact material and its preparation process adopts hot pressing sintering of pure Ti 3 SiC 2 Powder preparation of porous Ti 3 SiC 2 Skeleton, and finally, carrying out high-temperature infiltration on metallic silver to obtain Ti 3 SiC 2 The hot-pressing sintering temperature of the framework of the reinforced silver-based electric contact material is not lower than 900 ℃, the process is favorable for improving the strength of the silver-based electric contact material, the bending strength is not lower than 520MPa, and the reinforced silver-based electric contact material also has good arc erosion resistance and wear resistance. However, the process is subjected to hot-pressing sintering temperatureAnd the porosity of the framework cannot be further improved due to the influence of pressure, so that the content of metallic silver in the prepared electric contact material cannot be improved, which is the reason of poor electric conductivity of the electric contact material, and the electric conductivity is not higher than 7.5MS/m; second, ti 3 SiC 2 The powder generates closed pores in a framework due to the arch bridge effect at higher hot-pressing sintering temperatures of 1200 ℃ and 1400 ℃, so that molten silver cannot fill the pores to cause defects, the occupation ratio and the connectivity of metallic silver in the silver-based electric contact material are seriously influenced, and the silver-based electric contact material has low conductivity and poor toughness and is easy to cause brittle fracture.
Therefore, this patent developed an infiltration Ag-Ti 3 SiC 2 The component regulating and controlling method of the electric contact material has important significance for improving the performance and service reliability of the electric contact material, and is expected to be used as a novel silver-based electric contact material to replace the existing oxide and carbide enhanced silver-based electric contact material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides Ag-Ti 3 SiC 2 The component regulating and controlling method of the electric contact material mainly aims to prepare the silver-based electric contact material with excellent electric and thermal conductivity, high strength and wear resistance by a simple process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
Ag-Ti 3 SiC 2 The component regulating and controlling method of the electric contact material comprises the following steps:
In the step 1, the ball milling mixing time is at least 48 hours.
In the step 1, drying treatment is carried out in a fume hood or a drying oven at 40 ℃.
In the step 1, the raw material powder is Ti 3 SiC 2 Powder and silver powder, wherein Ti 3 SiC 2 The powder size is 0.5-50 μm, the silver powder size is 3-25 μm, the volume fraction of the silver powder is 20-30%, and the Ti content 3 SiC 2 The volume fraction of the powder is 70-80%.
In the step 2, the hot-pressing sintering is carried out at the heating rate of 10 ℃/min, the temperature is increased from the room temperature to 750-800 ℃, the pressure is increased from 0 to 5-10 MPa while heating is carried out, furnace cooling and pressure maintaining are carried out all the time, the furnace is taken out after being cooled to the room temperature, and the heat preservation and pressure maintaining time of the sintering treatment is 0.5-1 h.
In the step 2, the vacuum degree is 10 -3 Pa, and the protective atmosphere is argon.
In said step 2, ti 3 SiC 2 The porosity of the-Ag composite porous framework is 25-50%.
In the step 3, the silver blocks are 90-120 g.
In the step 3, the temperature in the furnace cavity of the heating furnace is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then raised to the infiltration treatment temperature of 1100-1300 ℃ at the heating rate of 5 ℃/min, the heat preservation time is at least 1h, and finally the furnace is cooled to the room temperature; the temperature of the high-temperature infiltration treatment is higher than the melting point of silver.
In the step 3, the silver block is Ti 3 SiC 2 the-Ag composite porous framework is placed up and down.
In the step 2 and the step 3, the crucible and the mold are made of graphite.
In the method, ag-Ti 3 SiC 2 The volume fraction of silver in the electric contact material is 40-70%, preferably 45-65%, and the rest is Ti 3 SiC 2 。
Preferably, the Ag-Ti 3 SiC 2 The bending strength of the electric contact material is 700-900 Mpa.
Preferably, the Ag-Ti 3 SiC 2 The fracture toughness value of the electric contact material is 15-20 MPa.m 1/2 。
Preferably, the Ag-Ti 3 SiC 2 The hardness of the electric contact material is 1.2-1.5 GPa.
Preferably, the Ag-Ti 3 SiC 2 The electric conductivity of the electric contact material is 15.5-21.7 MS/m.
Compared with the prior art, the Ag-Ti of the invention 3 SiC 2 The component regulating and controlling method of the electric contact material has the following beneficial effects:
the invention provides an infiltration Ag-Ti 3 SiC 2 The component regulating and controlling method of electric contact material adopts metal occupying method to mix silver powder and Ti in a certain proportion 3 SiC 2 Preparing mixed powder by wet mixing, and preparing Ti by selecting matched hot-pressing sintering temperature and pressure according to the amount of the added silver powder 3 SiC 2 And (4) carrying out Ag composite porous framework, and finally infiltrating 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 melting the silver powder by infiltration. The composite material prepared by mixing silver powder and other powder and through a powder metallurgy process has the problems that impurities such as an oxide film of the silver powder are difficult to avoid being introduced in the process, and the impurities can be reduced to a great extent by adopting infiltration block silverAnd (4) quality. Compared with a powder metallurgy process and a skeleton infiltration method, the regulation and control method can effectively regulate and control the content of silver in the electric contact material, wherein the regulation and control method can match corresponding hot-pressing sintering temperature and pressure according to the addition amount of the silver powder, so that the silver powder contained in the mixed powder is prevented from being extruded, and the added silver powder can reduce Ti 3 SiC 2 The contact area between the powders is ensured and Ti is ensured 3 SiC 2 Ti in-Ag composite porous skeleton 3 SiC 2 The phases form a continuous three-dimensional interpenetrating structure, and then the metal silver is infiltrated at high temperature to obtain two phases of continuous Ag-Ti with high metal silver content 3 SiC 2 The electric contact material has the characteristics of fusion welding resistance, self lubrication resistance, arc erosion resistance, mechanical property improvement and wear resistance on the premise of ensuring good electric conduction and heat conductivity of the electric contact material.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to make the technical solutions of the present invention practical in accordance with the contents of the specification, the following detailed description is given of preferred embodiments of the present invention with reference to the accompanying drawings.
Drawings
FIG. 1 is an infiltration Ag-Ti 3 SiC 2 Ti used in method for regulating composition of electric contact material 3 SiC 2 XRD pattern of (a);
FIG. 2 is a schematic representation of example 1 of the present invention, ti being prepared 3 SiC 2 -a macroscopic view of the Ag composite porous framework;
FIG. 3 is Ti prepared according to example 1 of the present invention 3 SiC 2 -microstructure of Ag composite porous skeleton;
FIG. 4 shows Ag-Ti prepared according to example 1 of the present invention 3 SiC 2 A macroscopic photograph of the electrical contact material;
FIG. 5 shows Ag-Ti prepared according to example 1 of the present invention 3 SiC 2 Microstructure diagram of electric contact material (wherein the light color is Ag and the dark color is Ti) 3 SiC 2 )；
FIG. 6 shows Ag-Ti prepared according to example 1 of the present invention 3 SiC 2 The in-situ fracture toughness force and displacement curve of the electric contact material;
FIG. 7 shows Ag-Ti prepared according to example 1 of the present invention 3 SiC 2 Stable crack deflection of the electrical contact material;
FIG. 8 is a photograph of Ag-Ti films prepared according to example 2 of the present invention 3 SiC 2 Microstructure diagram of electric contact material (wherein the light color is Ag and the dark color is Ti) 3 SiC 2 )；
FIG. 9 shows Ag-Ti prepared according to example 2 of the present invention 3 SiC 2 The in-situ fracture toughness force and displacement curve of the electric contact material;
FIG. 10 shows Ag-Ti alloys prepared according to example 2 of the present invention 3 SiC 2 Stable crack deflection of the electrical contact material;
FIG. 11 is a comparative example 3, ag-Ti prepared 3 SiC 2 Microstructure diagram of electric contact material (wherein the light color is Ag and the dark color is Ti) 3 SiC 2 )；
FIG. 12 is a comparative example 3, ag-Ti 3 SiC 2 Fracture toughness force versus displacement curve of the electrical contact material;
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined object, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The specific scheme of the invention is as follows:
the embodiment of the invention provides infiltration Ag-Ti 3 SiC 2 A component regulating method of an electric contact material. Wherein the electric contact material is prepared from micron-sized or nano-sized silver powder and ceramic powder Ti 3 SiC 2 Mixing, and hot-pressing sintering to obtain Ti 3 SiC 2 The composite porous framework is filled with silver by high-temperature infiltration to obtain the material with a microscopic three-dimensional interpenetrating structureTi 3 SiC 2 -Ag electrical contact material; wherein, in the hot-pressing sintering process, the corresponding hot-pressing sintering temperature is matched according to the addition amount of the silver powder, so that the silver powder contained in the mixed powder is not only prevented from being extruded, but also the added silver powder can reduce Ti 3 SiC 2 The contact area between the powders is ensured and Ti is ensured 3 SiC 2 Ti in-Ag composite porous skeleton 3 SiC 2 The phases form a continuous three-dimensional interpenetrating structure. The preferred 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 between 40% and 70%, preferably between 45% and 65%.
The invention is further illustrated by the following specific experimental examples:
in examples 1 to 5, the same heating furnace equipment, a graphite mold having a diameter of 50mm and a graphite crucible were used for hot-press sintering and high-temperature infiltration.
Example 1
This example uses an infiltration Ag-Ti 3 SiC 2 The component regulation and control method of the electric contact material comprises the following preparation steps:
FIG. 1 shows Ti used 3 SiC 2 XRD pattern of (a); FIG. 3 shows Ag-Ti obtained in example 1 of the present invention 3 SiC 2 The microstructure of the porous skeleton of the electrical contact material, FIG. 2 shows the resulting Ag-Ti 3 SiC 2 A macrostructure of a porous skeleton of the electrical contact material; FIG. 5 shows Ag-Ti obtained in example 1 of the present invention 3 SiC 2 The microstructure of the electrical contact material, FIG. 4 is Ag-Ti obtained in example 1 of the present invention 3 SiC 2 The macroscopic structure of the electric contact material shows that the metal silver is fully infiltrated and has no defects, and the volume fraction of the matrix metal silver is 55 percent; FIGS. 6 and 7 show Ag-Ti obtained in example 1 of the present invention 3 SiC 2 The force-displacement curve and stable crack deflection of the fracture toughness test of the electric contact material are calculated, and the fracture toughness K of the electric contact material is known IC ＝17.3±2MPa·m 1/2 The bending strength is 720 +/-10 MPa, the electric conductivity is 21 +/-0.7 MS/m, and the hardness value is 1.17G +/-0.06 Pa.
Example 2
Infiltration Ag-Ti 3 SiC 2 The component regulation and control method of the electric contact material comprises the following preparation steps:
FIG. 8 shows Ag-Ti obtained in example 2 of the present invention 3 SiC 2 The microstructure of the electric contact material shows that the metallic silver is fully infiltrated and has no defect, and the volume fraction of the matrix metallic silver is 52 percent; FIGS. 9 and 10 are Ag-Ti prepared in example 2, respectively 3 SiC 2 The force-displacement curve and stable crack deflection of the fracture toughness test of the electric contact material are calculated, and the fracture toughness K of the electric contact material is known IC ＝19.3±0.6MPa·m 1/2 The bending strength is 780 +/-20 Mpa, the electric conductivity is 17.8 +/-0.5 MS/m, and the hardness value is 1.25 +/-0.04 GPa.
Example 3
Infiltration Ag-Ti 3 SiC 2 The component regulation and control method of the electric contact material comprises the following preparation steps:
Example 4
Infiltration Ag-Ti 3 SiC 2 The component regulating and controlling method of the electric contact material comprises the following preparation steps:
Example 5
Infiltration Ag-Ti 3 SiC 2 The component regulating and controlling method of the electric contact material comprises the following preparation steps:
Comparative example
This example is a comparative example, with Ti 3 SiC 2 Infiltrating metal silver into-Ag composite porous framework to prepare Ag-Ti 3 SiC 2 An electrical contact material. Wherein the raw material comprises Ti with an average particle size of 24 μm 3 SiC 2 Powder and pure silver blocks.
The preparation method comprises the following preparation steps:
FIG. 11 shows comparative example preparation of Ti 3 SiC 2 Microstructure of Ag electric contact material, the volume fraction of matrix metal silver is 45%, it can be seen that the proportion of matrix silver is lower than that of examples 1 and 2, and FIG. 12 is Ti prepared in comparative example 3 3 SiC 2 The force and displacement curve of the fracture toughness test of Ag electrical contact material can judge Ti prepared by the comparative example 3 SiC 2 Brittle fracture of Ag electrical contact material occurs due to the low content of metallic silver. The Ti 3 SiC 2 The bending strength of the-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 a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. Ag-Ti 3 SiC 2 The component regulating and controlling method of the electric contact material comprises the following steps:
step 1, preparing mixed powder: mixing Ti 3 SiC 2 Putting the powder and silver powder into a container with alcohol according to a certain proportion, completely immersing the mixed powder in alcohol, filling zirconium balls, carrying out wet ball milling, pouring the mixed slurry into the container after mixing, carrying out powder precipitation, removing upper-layer alcohol, drying until the alcohol is volatilized to prepare Ti 3 SiC 2 -Ag mixed powder;
step 2, preparing Ti 3 SiC 2 -Ag composite porous skeleton step: mixing Ti 3 SiC 2 Putting the Ag mixed powder into a mould, putting the mould into a hot-pressing sintering furnace, matching the corresponding hot-pressing sintering temperature and pressure according to the addition amount of the silver powder, and then putting the mould into a protective atmosphereOr sintering under vacuum condition to obtain Ti 3 SiC 2 -an Ag composite porous skeleton;
step 3, high-temperature infiltration: mixing silver block and Ti 3 SiC 2 Putting the Ag-Ti composite porous skeleton into a container, adding silver blocks in an amount enough to fill the gaps of the skeleton, putting the container into a furnace cavity of a heating furnace, and performing high-temperature infiltration treatment under vacuum and/or protective atmosphere to finally obtain Ag-Ti 3 SiC 2 An electrical contact material.
2. Ag-Ti according to claim 1 3 SiC 2 The method for regulating and controlling the components of the electric contact material is characterized in that in the step 1, the ball milling and mixing time is at least 48 hours, and the drying treatment is carried out in a fume hood or a drying oven at 40 ℃.
3. Ag-Ti according to claim 1 3 SiC 2 The component regulation and control method of the electric contact material is characterized in that in the step 1, ti 3 SiC 2 The powder size is 0.5-50 μm, the silver powder size is 3-25 μm, the volume fraction of the silver powder is 20-30%, and the Ti content 3 SiC 2 The volume fraction of the powder is 70-80%.
4. Ag-Ti according to claim 1 3 SiC 2 The method for regulating and controlling the components of the electric contact material is characterized in that in the step 2, the temperature rise rate of hot-pressing sintering is 10 ℃/min, the temperature rises from room temperature to 750-800 ℃, 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 and is accompanied with furnace cooling and pressure maintaining all the time, the electric contact material is taken out after the furnace is cooled to room temperature, and the material of the mold is graphite.
5. Ag-Ti according to claim 1 3 SiC 2 The component regulation and control method of the electric contact material is characterized in that in the step 2, the vacuum degree is 10 -3 Pa, and the protective atmosphere is argon.
6. Ag-Ti according to claim 1 3 SiC 2 The component regulation and control method of the electric contact material is characterized in that in the step 2, ti 3 SiC 2 The porosity of the-Ag composite porous framework is 25-50%.
7. Ag-Ti according to claim 1 3 SiC 2 The component regulation and control method of the electric contact material is characterized in that in the step 3, the temperature in the furnace cavity of the heating furnace is raised to 1000 ℃ from the room temperature at the speed of 10 ℃/min, then 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 temperature of the high-temperature infiltration treatment is higher than the melting point of silver, and the container is a graphite crucible.
8. Ag-Ti according to claim 1 3 SiC 2 The component regulation and control method of the electric contact material is characterized in that in the step 3, the silver block accounts for 90-120 g, and the silver block is in Ti 3 SiC 2 the-Ag composite porous framework is placed up and down.
9. Ag-Ti according to claim 1 3 SiC 2 The component regulation and control method of the electric contact material is characterized in that the Ag-Ti 3 SiC 2 The volume fraction of silver in the electric contact material is 40-70%, and the rest is Ti 3 SiC 2 。
10. Ag-Ti according to claim 1 3 SiC 2 The component regulation and control method of the electric contact material is characterized in that the Ag-Ti 3 SiC 2 The bending strength of the electric contact material is 700-900 Mpa, and 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.
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