CN114724871A - silver-Ti3SiC2Electric contact material and preparation method thereof - Google Patents
silver-Ti3SiC2Electric contact material and preparation method thereof Download PDFInfo
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- CN114724871A CN114724871A CN202210312764.9A CN202210312764A CN114724871A CN 114724871 A CN114724871 A CN 114724871A CN 202210312764 A CN202210312764 A CN 202210312764A CN 114724871 A CN114724871 A CN 114724871A
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- 239000000463 material Substances 0.000 title claims abstract description 185
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims abstract description 224
- 229910052709 silver Inorganic materials 0.000 claims abstract description 38
- 239000004332 silver Substances 0.000 claims abstract description 38
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000005452 bending Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims description 55
- 239000000843 powder Substances 0.000 claims description 37
- 238000002156 mixing Methods 0.000 claims description 17
- 238000000626 liquid-phase infiltration Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001764 infiltration Methods 0.000 claims description 10
- 230000008595 infiltration Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 22
- 238000000034 method Methods 0.000 description 15
- 230000003014 reinforcing effect Effects 0.000 description 15
- 229910052786 argon Inorganic materials 0.000 description 11
- 239000002131 composite material Substances 0.000 description 10
- 238000007731 hot pressing Methods 0.000 description 9
- 238000005520 cutting process Methods 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 7
- 239000011858 nanopowder Substances 0.000 description 7
- 230000001788 irregular Effects 0.000 description 6
- 238000004663 powder metallurgy Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 230000001419 dependent effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 238000001272 pressureless sintering Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 238000005096 rolling process Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0233—Composite material having a noble metal as the basic material and containing carbides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
- C04B35/5615—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium silicon carbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
Abstract
The invention relates to a silver-Ti3SiC2An electric contact material and a preparation method thereof relate to the technical field of silver-based electric contact materials. The main technical scheme adopted is as follows: silver-Ti3SiC2An electrical contact material of Ti3SiC2Is a framework, silver is infiltrated into Ti3SiC2Three-dimensional interpenetrating structure in the skeleton, and silver and Ti3SiC2The framework is a bicontinuous phase; wherein, in the silver-Ti3SiC2In the electric contact material, Ti3SiC2The volume fraction of (A) is 50-70%; wherein, the silver-Ti3SiC2The Vickers hardness of the electric contact material is more than 1.9GPa, preferably more than 2 GPa; the silver-Ti3SiC2The bending strength of the electric contact material is not less than 520MPa, preferably greater than 630 MPa; the silver-Ti3SiC2The electrical contact material has an electrical conductivity of more than 5MS/m, preferably more than 6.5 MS/m. The invention is mainly used for ensuring silver-Ti3SiC2On the basis of the electric conductivity of the electric contact material, silver-Ti3SiC2The electric contact material has better mechanical property.
Description
Technical Field
The invention relates to the field of silver-based electric contact materials, in particular to silver-Ti3SiC2An electric contact material and a preparation method thereof.
Background
The electric contact material is a key material for the contact parts of electric appliances (such as switches, relays, starters and the like) which bear on-off control and load current in a circuit. The silver-based electric contact material has the advantages of excellent conductivity and fusion welding resistance, small and stable contact resistance and the like, and is widely applied to circuit breakers and contactors in various light and heavy load high-low voltage household appliances, automobiles and aerospace electrical appliances.
The silver-MAX phase electrical contact material in the prior art is mainly a composite material prepared by a powder metallurgy method, such as:
the first prior art provides a Ti3SiC2The preparation method of the reinforced Ag-based electrical contact material mainly adopts the following scheme: mixing Ti3SiC2The powder and Ag powder are mixed according to a certain proportion, ball-milled, cold-pressed, made into blank and sintered at high temperature to prepare Ti with uniform structure, high density and excellent conductivity3SiC2A reinforced Ag-based electrical contact composite material.
The second prior art provides a preparation method of an Ag/MAX electric contact material, which mainly adopts the following scheme: the Ag/MAX phase electric contact material with the characteristics of Ag grain refinement, laminated MAX phase layering and directional arrangement, compactness and anisotropy is prepared by adopting a means of combining powder metallurgy with an equal channel corner extrusion method.
A third prior art provides an Ag/Ti alloy3SiC2The main scheme of the electric contact material is as follows: adding silver-plated Ti into silver matrix by adopting powder metallurgy method3SiC2And (3) preparing powder, namely preparing the silver-based electric contact material, and obtaining an actual product after hot extrusion molding, rolling or drawing processing and mechanical processing.
The composite material produced by the powder metallurgy method here: the MAX phase is typically dispersed as a reinforcing phase in the silver matrix without spatial interconnection, which results in no current conduction between the conductive MAX phases. The current path is mainly composed of two parts: firstly, a silver matrix; second is silver-MAX-silver. And the conduction of current at the interface results in an increase in the resistance of the material. In addition, the matrix metal silver provides high conductivity for the composite material, but the mechanical property is poor due to the soft quality of the composite material, the MAX reinforcing phase is used for improving the mechanical property of the composite material, but the conductivity of the reinforcing phase material is low, and the conductivity of the composite material is seriously influenced by the increase of the addition amount, so that the addition of the reinforcing phase is limited (the volume fraction of the reinforcing phase is low).
In conclusion, the silver-MAX phase electrical contact material in the prior art has the problems of low strength and hardness due to low content of the ceramic in the enhanced phase in order to ensure the electrical conductivity.
Disclosure of Invention
In view of the above, the present invention provides a silver-Ti alloy3SiC2The main purpose of the electric contact material is to ensure the silver-Ti3SiC2On the basis of the conductivity of the electric contact material, silver-Ti3SiC2The electric contact material has better mechanical property.
In order to achieve the purpose, the invention mainly provides the following technical scheme:
in one aspect, embodiments of the present invention provide a silver-Ti alloy3SiC2An electrical contact material, wherein the silver-Ti3SiC2The electric contact material is Ti3SiC2For the skeleton, silver penetrating into said Ti3SiC2Three-dimensional interpenetrating structure in the skeleton, and silver and Ti3SiC2The framework is a bicontinuous phase; wherein, in the silver-Ti 3SiC2 electric contact material, the Ti3SiC2The volume fraction of (A) is 50-70%, and the rest is silver;
wherein, the silver-Ti3SiC2The Vickers hardness of the electric contact material is not less than 1.9GPa, and preferably more than 2 GPa; the silver-Ti3SiC2The bending strength of the electric contact material is more than 520MPa, preferably more than 630 MPa; the silver-Ti3SiC2The electrical contact material has an electrical conductivity of more than 5MS/m, preferably more than 6.5 MS/m.
Preferably, if Ti3SiC2The skeleton is composed of nano-scale Ti3SiC2Powder is prepared from the silver-Ti3SiC2In the electric contact material: ti3SiC259-67% by volume; if Ti3SiC2The skeleton is made of micron-sized Ti3SiC2Powder is prepared from the silver-Ti3SiC2In the electric contact material: ti3SiC2Is 59-70% by volume.
Preferably, the Ti is3SiC2The skeleton is composed of nano-scale Ti3SiC2Preparing powder; wherein, the nano-scale Ti3SiC2The particle size of the powder is 300-1600nm, preferably 600-940nm, and more preferably 700-730 nm. Preferably, the silver-Ti3SiC2The density of the electric contact material is 6.52-7.33g/cm3(ii) a And/or the silver-Ti3SiC2The Vickers hardness of the electric contact material is 2.06-3.36 GPa; and/or the silver-Ti3SiC2The bending strength of the electric contact material is 633-778 MPa; and/or the silver-Ti3SiC2Fracture toughness K of electric contact materialICThe value is 14-16 MPa.m1/2(ii) a And/or the silver-Ti3SiC2The electric conductivity of the electric contact material is 6.7-7.6 MS/m; and/or the silver-Ti3SiC2The friction coefficient of the electric contact material is 0.28-0.30; and/or the silver-Ti3SiC2The wear rate of the electric contact material is 7.6-17.5 × 10-6mm/(N·m)。
Preferably, the Ti3SiC2The skeleton is made of micron-sized Ti3SiC2Preparing powder; wherein the micron-sized Ti3SiC2The particle size of the powder is 5-66.5 microns, preferably 24-24.5 microns. Preferably, the silver-Ti3SiC2The density of the electric contact material is 6.35-6.97g/cm3(ii) a And/or the silver-Ti3SiC2The Vickers hardness of the electric contact material is 1.99GPa-2.93 GPa; and/or the silver-Ti3SiC2The bending strength of the electric contact material is 520-568 MPa; and/or the silver-Ti3SiC2Fracture toughness K of electric contact materialICThe value is 9.3-12.84 MPa.m1/2(ii) a And/or the silver-Ti3SiC2The electric conductivity of the electric contact material is 5.3-6.91 MS/m; and/or the silver-Ti3SiC2The friction coefficient of the electric contact material is 0.30-0.32; and/or the silver-Ti3SiC2The wear rate of the electric contact material is 3.4-16.7 × 10-6mm/(N·m)。
On the other hand, the embodiment of the invention also provides the silver-Ti of any one of the above3SiC2The preparation method of the electric contact material comprises the following steps:
preparation of Ti3SiC2A skeleton step: mixing Ti3SiC2Filling the powder into a mold, and sintering under a protective atmosphere or vacuum condition to obtain Ti3SiC2A framework;
and a melt infiltration treatment step: for Ti3SiC2The framework and the silver block are subjected to melt infiltration treatment, and after the set time, the silver-Ti is obtained3SiC2An electrical contact material.
Preferably, in said preparation of Ti3SiC2The skeleton step is as follows: the sintering treatment temperature is 800-1500 ℃, the sintering treatment pressure is 0-2t, and the sintering treatment time is 1-3 h.
Preferably, the preparation of Ti3SiC2The skeleton step is performed in a vacuum autoclave.
Preferably, the impregnation treatment step specifically includes: adding the Ti3SiC2The framework and the silver block are placed in a container; heating the container under the protective atmosphere or vacuum condition, raising the temperature to the infiltration treatment temperature, preserving the heat at the infiltration treatment temperature for a set time, and cooling to obtain the silver-Ti3SiC2An electrical contact material.
Preferably, the infiltration treatment temperature is 1000-1400 ℃, and preferably 1200 ℃; and/or
Preferably, the set time is 1-2h, preferably 2 h.
Compared with the prior art, the silver-Ti of the invention3SiC2The electric contact material and the preparation method thereof have at least the following beneficial effects:
in one aspect, the examples of the present invention provide silver-Ti3SiC2The electric contact material is Ti3SiC2Is a framework, silver is infiltrated into Ti3SiC2Three-dimensional interpenetrating structure in the skeleton, and silver and Ti3SiC2The framework is in a bicontinuous phase; wherein, in the silver-Ti3SiC2In the electric contact material, the Ti3SiC2The volume fraction is 50-70%; wherein, the silver-Ti3SiC2The Vickers hardness of the electric contact material is more than 2.2GPa, the bending strength is more than 500MPa, and the electric conductivity is more than 5 MS/m. Thus, the present invention provides silver-Ti3SiC2The electric contact material has excellent mechanical property on the basis of ensuring the conductivity. In addition, the silver-Ti provided by the embodiment of the invention3SiC2The electric contact material also has excellent wear resistance.
Further, Ti3SiC2The skeleton is made of nano-level powder or micron-level powder, in Ti3SiC2silver-Ti made from nano-grade powder under the condition of same content3SiC2The electric contact material has a finer and uniform structure, and has more excellent mechanical property, wear resistance and higher conductivity.
On the other hand, the embodiment of the invention also provides the silver-Ti3SiC2The preparation method of the electric contact material mainly comprises the steps of hot-pressing sintering and melt infiltration, wherein the porosity of the framework can be controlled and adjusted by controlling the sintering temperature of the framework, and the content of two phases in the composite material can be further controlled, so that the silver-Ti content can be adjusted3SiC2Mechanical property of the electric contact material. In addition, the preparation process is simple and can realize industrial production.
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 implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 shows a silver-Ti alloy according to an embodiment of the present invention3SiC2A preparation process flow chart of the electric contact material;
FIG. 2 shows Ag-Ti prepared in example 1 of the present invention3SiC2A sample macro topography of the electrical contact material;
FIG. 3 shows Ag-Ti prepared in example 1 of the present invention3SiC2A microstructure of the electrical contact material;
FIG. 4 shows Ag-Ti prepared in example 2 of the present invention3SiC2A microstructure of the electrical contact material;
FIG. 5 shows Ag-Ti prepared in example 3 of the present invention3SiC2A microstructure of the electrical contact material;
FIG. 6 shows Ag-Ti prepared in example 4 of the present invention3SiC2A microstructure of the electrical contact material;
FIG. 7 shows Ag-Ti prepared in example 5 of the present invention3SiC2A microstructure of the electrical contact material;
FIG. 8 shows Ag-Ti prepared in example 6 of the present invention3SiC2A microstructure of the electrical contact material;
FIG. 9 is silver-Ti3SiC2Hardness of electric contact material following Ti3SiC2The variation curve of the content;
FIG. 10 is a silver-Ti3SiC2Conductivity of the electrical contact material is dependent on Ti3SiC2The variation curve of the content;
FIG. 11 is silver-Ti3SiC2Bending strength of electric contact material following Ti3SiC2The variation curve of the content;
FIG. 12 is silver-Ti3SiC2Fracture toughness of electric contact material along with Ti3SiC2The variation curve of the content.
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.
Aiming at the problem of the prior art that the content of the reinforced phase ceramic is lower to ensure the conductivity, which results in silver-Ti3SiC2The electric contact material has the technical problems of low strength, low hardness and the like. The inventors of the present invention have desired to improve the electrical conductivity of the material without significantly reducing the electrical conductivity of the ceramic Ti by structural design3SiC2And the content of the active carbon is increased, so that the mechanical property of the material is improved.
The existing method for preparing silver-Ti mainly through powder metallurgy3SiC2Electric contact material of Ti3SiC2The phases are usually dispersed as a reinforcing phase in the silver matrix and do not spatially interact with each other, which results in conductive Ti3SiC2No current is conducted between the phases (the inventor finds that the current path of the material mainly consists of two parts, namely, a silver matrix and silver-Ti3SiC2-silver. And the conduction of current at the interface results in an increase in the resistance of the material). Here, the inventors found that by adding Ti3SiC2The phase is subjected to a three-dimensional interpenetrating structure design, so that the interfaces in the current conduction process of the material can be reduced, and the conductivity is improved; on the basis of properly increasing the content of the reinforcing phase, the conductivity can be ensured. In addition, the three-dimensional interpenetrating structure of the reinforcing phase can further improve the mechanical property of the composite material. The structural design can compensate the traditional silver-Ti3SiC2The electrical contact material has insufficient mechanical properties such as hardness and strength.
The specific scheme of the invention is as follows:
the embodiment of the invention provides silver-Ti3SiC2An electrical contact material. Wherein, the silver-Ti3SiC2The electric contact material is micron-sized or nano-sized Ti3SiC2The ceramic powder is a framework, silver penetrates into a three-dimensional interpenetrating structure in the framework, and the silver and the Ti are mixed3SiC2The framework is a bicontinuous phase; wherein, the Ti3SiC2The volume fraction is 50-70%, preferably 53-69%, and the balance is silver.
Wherein the silver-Ti3SiC2The preparation method of the electric contact material (the specific preparation process is shown in figure 1) comprises the following steps:
1) preparation of Ti3SiC2A skeleton step: mixing Ti3SiC2Filling the powder into a mold, and sintering under a protective atmosphere or vacuum condition to obtain Ti3SiC2And (3) a framework.
In this step: the sintering treatment temperature is 800-1500 ℃, the sintering treatment pressure is 0-2t, and the sintering treatment time is 1-3 h.
2) And a melt infiltration treatment step: for Ti3SiC2The framework and the silver block are subjected to melt infiltration treatment, and after the set time, the silver-Ti is obtained3SiC2An electrical contact material.
The method comprises the following steps: mixing Ti3SiC2The framework and the silver block are placed in a container; heating the container under the protective atmosphere or vacuum condition, raising the temperature to the infiltration treatment temperature, preserving the heat at the infiltration treatment temperature for a set time, and cooling to obtain the silver-Ti3SiC2An electrical contact material.
Preferably, the impregnation treatment temperature is 1000-1400 ℃, preferably 1200 ℃; the set time is 1-2h, preferably 2 h.
The following is further illustrated by the specific examples:
example 1
This example prepares a silver-Ti3SiC2The electrical contact material comprises the following specific steps:
1) preparation of Ti3SiC2A skeleton step: about 85g of the powder with the particle sizeNano Ti of about 700nm3SiC2Filling powder into a die (the distance between the dies is 50mm), then placing the die into a hot-pressing sintering furnace, and sintering under the protection of argon to obtain Ti3SiC2And (3) a framework. Wherein the sintering treatment temperature is 900 ℃, the sintering treatment time is 1 hour, and the sintering treatment pressure is 2 t.
Here, it should be noted that: obtained Ti3SiC2The skeleton had a diameter of 49.8mm (shrinkage after sintering), a thickness of 27.2mm and a mass of 84.06 g.
Mixing Ti3SiC2The skeleton was cut into 8mm thick discs and then infiltrated (irregular shape of shrinkage, infiltrated after cutting to obtain the final silver-Ti3SiC2The electrical contact material sample may be more regular).
2) And a melt infiltration treatment step: mixing Ti3SiC2The skeleton, about 200g silver block was placed in a container; heating the container under the protection of pure argon or vacuum, heating to 1200 ℃, preserving heat for 2h at 1200 ℃, and cooling to obtain the silver-Ti3SiC2An electrical contact material.
In which, the silver-Ti prepared in this example3SiC2The macroscopic topography of the sample of electrical contact material is shown in fig. 2. As can be seen from fig. 2: silver-Ti3SiC2The surface of the electric contact material presents metallic luster and has no obvious defect; wherein, silver-Ti3SiC2The sample of electrical contact material was about 47mm in diameter.
Example 2
This example prepares a silver-Ti3SiC2The electrical contact material comprises the following specific steps:
1) preparation of Ti3SiC2A skeleton step: about 70g of nano Ti with the grain diameter of about 700nm3SiC2Filling the powder into a die (the diameter of the die is 50mm), then putting the die into a hot-pressing sintering furnace, and sintering under the protection of argon to obtain Ti3SiC2And (3) a framework. Wherein the sintering treatment temperature is 1200 ℃, the sintering treatment time is 1 hour, and the sintering treatment pressure is 2 t.
It should be noted here that: obtained Ti3SiC2The skeleton had a diameter of 46.8mm (shrinkage after sintering), a thickness of 20.0mm and a mass of 67.08 g.
Mixing Ti3SiC2Cutting the skeleton into 8mm thick wafers and infiltrating (irregular shape of shrinkage, infiltration after cutting to obtain final silver-Ti3SiC2The electrical contact material sample may be more regular).
2) And a melt infiltration treatment step: mixing Ti3SiC2The skeleton, about 200g silver block was placed in a container; heating the container under the protection of pure argon or vacuum, heating to 1200 ℃, keeping the temperature at 1200 ℃ for 2h, and cooling to obtain the silver-Ti3SiC2An electrical contact material.
Example 3
This example prepares a silver-Ti3SiC2The electrical contact material comprises the following specific steps:
1) preparation of Ti3SiC2A skeleton step: about 62g of nano Ti with the grain diameter of about 700nm3SiC2Filling the powder into a die (the diameter of the die is 50mm), then putting the die into a hot-pressing sintering furnace, and sintering under the protection of argon to obtain Ti3SiC2And (3) a framework. Wherein the sintering treatment temperature is 1400 ℃, the sintering treatment time is 1 hour, and the sintering treatment pressure is 2 t.
Here, it should be noted that: obtained Ti3SiC2The skeleton had a diameter of 40.7mm (shrinkage after sintering), a thickness of 16.4mm and a mass of 60.96 g.
Mixing Ti3SiC2The skeleton was cut into 8mm thick discs and then infiltrated (irregular shape of shrinkage, infiltrated after cutting to obtain the final silver-Ti3SiC2The electrical contact material sample may be more regular).
2) And a melt infiltration treatment step: mixing Ti3SiC2The skeleton, about 200g silver block was placed in a container; heating the container to 1200 deg.C under pure argon atmosphere or vacuum condition, and maintaining at 1200 deg.CThe temperature is kept for 2 hours, and silver-Ti is obtained after cooling3SiC2An electrical contact material.
Example 4
This example prepares a silver-Ti3SiC2The electrical contact material comprises the following specific steps:
1) preparation of Ti3SiC2A skeleton step: about 133g of Ti with a particle size of 24 microns3SiC2Filling the powder into a die (the diameter of the die is 50mm), then putting the die into a hot-pressing sintering furnace, and sintering under the protection of argon to obtain Ti3SiC2And (3) a framework. Wherein the sintering treatment temperature is 900 ℃, the sintering treatment time is 1 hour, and the sintering treatment pressure is 2 t.
Here, it should be noted that: obtained Ti3SiC2The skeleton had a diameter of 49.7mm (shrinkage after sintering), a thickness of 26.9mm and a mass of 131.42 g.
Mixing Ti3SiC2The skeleton was cut into 8mm thick discs and then infiltrated (irregular shape of shrinkage, infiltrated after cutting to obtain the final silver-Ti3SiC2The electrical contact material sample may be more regular).
2) And a melt infiltration treatment step: mixing Ti3SiC2The skeleton, about 200g silver block was placed in a container; heating the container under the protection of pure argon or vacuum, heating to 1200 ℃, preserving heat for 2h at 1200 ℃, and cooling to obtain the silver-Ti3SiC2An electrical contact material.
Example 5
This example prepares a silver-Ti3SiC2The electrical contact material comprises the following specific steps:
1) preparation of Ti3SiC2A skeleton step: about 140g of Ti with a particle size of 24 microns3SiC2Filling the powder into a die (the diameter of the die is 50mm), then putting the die into a hot-pressing sintering furnace, and sintering under the protection of argon to obtain Ti3SiC2And (3) a framework. Wherein the sintering treatment temperature is 1200 ℃, the sintering treatment time is 1 hour, and the sintering treatment pressure is 2 t.
Here, it should be noted that: obtained Ti3SiC2The skeleton had a diameter of 48.3mm (shrinkage after sintering), a thickness of 26.1mm and a mass of 137.53 g.
Mixing Ti3SiC2Cutting the skeleton into 8mm thick wafers and infiltrating (irregular shape of shrinkage, infiltration after cutting to obtain final silver-Ti3SiC2The electrical contact material sample may be more regular).
2) And a melt infiltration treatment step: mixing Ti3SiC2The skeleton, about 200g silver block was placed in a container; heating the container under the protection of pure argon or vacuum, heating to 1200 ℃, preserving heat for 2h at 1200 ℃, and cooling to obtain the silver-Ti3SiC2An electrical contact material.
Example 6
This example prepares a silver-Ti3SiC2The electric contact material comprises the following specific steps:
1) preparation of Ti3SiC2A skeleton step: about 170g of Ti with a particle size of 24 microns3SiC2Filling the powder into a die (the diameter of the die is 50mm), then putting the die into a hot-pressing sintering furnace, and sintering under the protection of argon to obtain Ti3SiC2And (3) a framework. Wherein the sintering treatment temperature is 1400 ℃, the sintering treatment time is 1 hour, and the sintering treatment pressure is 2 t.
It should be noted here that: obtained Ti3SiC2The skeleton had a diameter of 46.3mm (shrinkage after sintering), a thickness of 32.1mm and a mass of 167.7 g.
Mixing Ti3SiC2The skeleton was cut into 8mm thick discs and then infiltrated (irregular shape of shrinkage, infiltrated after cutting to obtain the final silver-Ti3SiC2The electrical contact material sample may be more regular).
2) And a melt infiltration treatment step: mixing Ti3SiC2The framework and the silver block are placed in a container; heating the container under the protection of pure argon gas or vacuum, heating to 1200 deg.C, maintaining the temperature at 1200 deg.C for 2 hr, cooling, and collecting the filtrateObtaining silver-Ti3SiC2An electrical contact material.
1. For silver-Ti prepared in examples 1-63SiC2The microstructure of the electrical contact material was characterized as follows:
silver-Ti prepared in example 13SiC2The microstructure of the electrical contact material is shown in fig. 3; silver-Ti prepared in example 23SiC2The microstructure of the electrical contact material is shown in fig. 4; silver-Ti prepared in example 33SiC2The microstructure of the electrical contact material is shown in fig. 5; silver-Ti prepared in example 43SiC2The microstructure of the electrical contact material is shown in fig. 6; silver-Ti prepared in example 53SiC2The microstructure of the electrical contact material is shown in fig. 7; silver-Ti prepared in example 63SiC2The microstructure of the electrical contact material is shown in fig. 8.
As can be seen from fig. 3-8: (1) silver-Ti prepared in examples 1-63SiC2Silver and Ti in electrical contact material3SiC2Are interpenetrating in three dimensions. (2) Under the same magnification, nano powder Ti is used3SiC2Prepared silver-Ti3SiC2The electric contact material has a finer microstructure, and the structure of the electric contact material is more uniform, and the corresponding mechanical property is improved more.
2. For the silver-Ti prepared in examples 1 to 63SiC2The electric contact material is subjected to performance test, and the test structure is shown in table 1 and table 2.
TABLE 1
| Example 1 | Example 2 | Example 3 | |
| Density of | 7.32 | 6.78 | 6.52 |
| Volume fraction% | 53.1 | 62.3 | 66.6 |
| Vickers hardness (GPa) | 2.41±0.02 | 2.9±0.04 | 3.16±0.04 |
| Flexural Strength (MPa) | 755.31±18.61 | 678.40±14.10 | 687.35±27.88 |
| Fracture toughness K1C value (MPa. m)1/2) | 15.14±0.68 | 14.99±0.94 | 14.64±0.15 |
| Conductivity (MS/m) | 7.41±0.11 | 7.28±0.22 | 6.95±0.22 |
| Coefficient of friction | 0.29 | 0.28 | 0.29 |
| Wear rate (mm/N. m) | 14.64±0.44×10-6 | 10.82±0.78×10-6 | 10.15±0.39×10-6 |
TABLE 2
| Example 4 | Example 5 | Example 6 | |
| Density of | 6.97 | 6.73 | 6.35 |
| Volume fraction% | 59.1 | 63.0 | 69.4 |
| Vickers hardness (GPa) | 2.35±0.06 | 2.52±0.05 | 2.61±0.10 |
| Flexural Strength (MPa) | 529.97±9.46 | 531.32±5.62 | 544.42±19.97 |
| Fracture toughness K1C value (MPa. m)1/2) | 11.68±1.00 | 11.24±0.73 | 10.59±1.25 |
| Conductivity (MS/m) | 6.58±0.20MS/m | 5.99±0.10 | 5.50±0.16 |
| Coefficient of friction | 0.31 | 0.30 | 0.32 |
| Wear rate (mm/N. m) | 5.00±0.28×10-6 | 8.67±0.87×10-6 | 11.07±1.41×10-6 |
Note: silver-Ti of this example was measured by Archimedes drainage method3SiC2Density of the electrical contact material, and then deducing silver-Ti according to the density3SiC2Ti in electric contact material3SiC2Volume fraction of (a). For silver-Ti3SiC2And (4) carrying out a three-point bending test on the electric contact material to test the bending strength. silver-Ti measurement by eddy current conductivity meter3SiC2Electrical conductivity of the electrical contact material. silver-Ti measured by friction and wear test3SiC2Coefficient of friction and wear rate of the electrical contact material.
3. FIG. 9 is silver-Ti3SiC2Hardness of electric contact material following Ti3SiC2The variation curve of the content. Wherein, the embodiment of the invention uses micron powder and nanometer powder Ti3SiC2Prepared silver-Ti3SiC2The hardness of the electric contact material is all changed with Ti3SiC2The increase in the content showed a tendency to rise. And in Ti3SiC2At the same content, the nano powder Ti is used3SiC2Prepared silver-Ti3SiC2The electrical contact material has a higher hardness.
In addition, other documents use processes such as pressureless sintering and spark plasma sintering. These two prepared silver-Ti3SiC2Ti in electric contact material3SiC2The content is generally lower, but in the higher part, the silver-Ti prepared by the process of the embodiment of the invention (sintering + melt infiltration)3SiC2The hardness of the electrical contact material is higher.
4. FIG. 10 is a silver-Ti3SiC2Conductivity of the electrical contact material is dependent on Ti3SiC2The variation curve of the content. Wherein, the embodiment of the invention uses micron powder and nanometer powder Ti3SiC2Prepared silver-Ti3SiC2The electrical conductivity of the electrical contact material follows that of Ti3SiC2The increase in the content shows a tendency to decrease, and is at Ti3SiC2At the same content, nano powder Ti is used3SiC2Prepared silver-Ti3SiC2The electrical contact material has a higher electrical conductivity.
In addition, other references use processes such as pressureless sintering processes and spark plasma sintering. silver-Ti prepared by the two processes3SiC2Ti in electric contact material3SiC2The content is generally lower, but in the higher part, the silver-Ti prepared by the process of the embodiment of the invention (sintering + melt infiltration)3SiC2The electrical contact material has a higher electrical conductivity.
5. FIG. 11 is silver-Ti3SiC2Bending strength of electric contact material following Ti3SiC2The variation curve of the content. Wherein, the embodiment of the invention uses nano powder Ti3SiC2Prepared silver-Ti3SiC2Bending strength of electric contact material following Ti3SiC2The content is increased and reduced, and micron powder Ti is used3SiC2Prepared silver-Ti3SiC2Bending strength of electric contact material following Ti3SiC2The content increases and shows an upward trend. And, in Ti3SiC2At the same content, nano powder Ti is used3SiC2Prepared silver-Ti3SiC2The bending strength of the electrical contact material is higher.
6. FIG. 12 is silver-Ti3SiC2Fracture toughness value of electric contact material is dependent on Ti3SiC2The variation curve of the content. Wherein, the embodiment of the invention uses micron powder and nanometer powder Ti3SiC2Prepared silver-Ti3SiC2Fracture toughness of electric contact material along with Ti3SiC2The content increases and the trend is reduced. And in Ti3SiC2At the same content, nano powder Ti is used3SiC2Prepared silver-Ti3SiC2The electrical contact material has a higher fracture toughness value.
Here, it should be noted that:
the sizes of the reinforcing phase particles used at the present stage are all in the micron level, but the embodiment of the invention provides that after the sizes of the reinforcing phase reach the nanometer level, the interface between the two phases becomes complex, so that the silver-Ti3SiC2The properties of the electrical contact material change and the dimensional effect further improves the performance of the material.
② traditional silver-Ti3SiC2In the electric contact material, the content of the reinforcing phase is often lower, and the reinforcing phase is randomly distributed in the silver matrix without mutual connection because the traditional preparation process is mainly based on powder metallurgy. It is proposed that the content of the reinforcing phase is increased, three-dimensional relation (design of three-dimensional interpenetrating structure) is established between the reinforcing phases, and the reinforcing phase Ti is added3SiC2The hot-pressing sintering can improve the comprehensive performance of the composite material.
The hot-pressing sintering and melt infiltration process provided by the embodiment of the invention can realize that the framework porosity of the material can be controlled and adjusted by controlling the framework sintering temperature, and further the silver-Ti content can be controlled3SiC2The contents of the two phases in the electric contact material are controlled, so that the mechanical property of the material is controlled.
silver-Ti prepared by the embodiment of the invention3SiC2The electrical contact material realizes the enhancement of the content of the enhanced phase, and Ti3SiC2The content reaches 50-70 vol.%. Same Ti as prepared by other processes3SiC2Compared with the content of the electric contact material, the silver-Ti prepared by the invention3SiC2The electric contact material has high conductivity, and the hardness and the mechanical property are greatly improved. silver-Ti prepared for the inventive examples3SiC2An electric contact material using nano-powder Ti3SiC2Prepared silver-Ti3SiC2The electric contact material is also superior to the micron powder Ti in performance3SiC2Prepared silver-Ti3SiC2An electrical contact material.
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. silver-Ti3SiC2An electrical contact material, characterized in that said silver-Ti3SiC2The electric contact material is Ti3SiC2Is a skeleton, silverIs infiltrated with the Ti3SiC2Three-dimensional interpenetrating structure in the skeleton, and silver and Ti3SiC2The framework is in a bicontinuous phase; wherein, in the silver-Ti3SiC2In the electric contact material, the Ti3SiC2The volume fraction of (A) is 50-70%, and the rest is silver;
wherein, the silver-Ti3SiC2The Vickers hardness of the electric contact material is more than 1.9GPa, preferably more than 2 GPa; the silver-Ti3SiC2The bending strength of the electric contact material is not less than 520MPa, preferably more than 630 MPa; the silver-Ti3SiC2The electrical contact material has an electrical conductivity of more than 5MS/m, preferably more than 6.5 MS/m.
2. silver-Ti according to claim 13SiC2An electrical contact material, characterized in that,
if Ti3SiC2The skeleton is composed of nano-scale Ti3SiC2Powder is prepared from the silver-Ti3SiC2In the electric contact material: ti3SiC259-67% by volume;
if Ti3SiC2The skeleton is made of micron-sized Ti3SiC2Powder is prepared from the silver-Ti3SiC2In the electric contact material: ti3SiC2Is 59-70% by volume.
3. silver-Ti according to claim 23SiC2An electrical contact material, characterized in that said Ti3SiC2The skeleton is composed of nano-scale Ti3SiC2Preparing powder; wherein, the nano-scale Ti3SiC2The particle size of the powder is 300-1600nm, preferably 600-940nm, and more preferably 700-730 nm.
4. silver-Ti according to claim 33SiC2An electrical contact material, characterized in that,
the silver-Ti3SiC2The density of the electric contact material is 6.52-7.33g/cm3(ii) a And/or
The silver-Ti3SiC2The Vickers hardness of the electric contact material is 2.06-3.36 GPa; and/or
The silver-Ti3SiC2The bending strength of the electric contact material is 633-778 MPa; and/or
The silver-Ti3SiC2Fracture toughness K of electric contact materialICThe value is 14-16 MPa.m1/2(ii) a And/or
The silver-Ti3SiC2The electric conductivity of the electric contact material is 6.7-7.6 MS/m; and/or
The silver-Ti3SiC2The friction coefficient of the electric contact material is 0.28-0.30; and/or
The silver-Ti3SiC2The wear rate of the electric contact material is 7.6-17.5 × 10-6mm/N·m。
5. silver-Ti according to claim 13SiC2An electrical contact material, characterized in that said Ti3SiC2The skeleton is made of micron-sized Ti3SiC2Preparing powder; wherein the micron-sized Ti3SiC2The particle size of the powder is 5-66.5 microns, preferably 24-24.5 microns;
preferably, the silver-Ti3SiC2The density of the electric contact material is 6.35-6.97g/cm3；
Preferably, the silver-Ti3SiC2The Vickers hardness of the electric contact material is 1.99GPa-2.93 GPa;
preferably, the silver-Ti3SiC2The bending strength of the electric contact material is 520-568 MPa; and/or
Preferably, the silver-Ti3SiC2Fracture toughness K of electric contact materialICThe value is 9.3-12.84 MPa.m1/2；
Preferably, the silver-Ti3SiC2The electric conductivity of the electric contact material is 5.3-6.91 MS/m;
preferably, the silver-Ti3SiC2Tribological system of electrical contact materialThe number is 0.30-0.32;
preferably, the silver-Ti3SiC2The wear rate of the electric contact material is 3.4-16.7 × 10-6mm/N·m。
6. silver-Ti according to any one of claims 1 to 53SiC2The preparation method of the electric contact material is characterized by comprising the following steps:
preparation of Ti3SiC2A skeleton step: mixing Ti3SiC2Filling the powder into a mold, and sintering under a protective atmosphere or vacuum condition to obtain Ti3SiC2A framework;
and a melt infiltration treatment step: for Ti3SiC2The framework and the silver block are processed by melt infiltration treatment, and after the set time, the silver-Ti is obtained3SiC2An electrical contact material.
7. silver-Ti according to claim 63SiC2The preparation method of the electric contact material is characterized in that the Ti is prepared3SiC2The skeleton step is as follows:
the sintering treatment temperature is 800-1500 ℃, the sintering treatment pressure is 0-2t, and the sintering treatment time is 1-3 h.
8. silver-Ti according to claim 73SiC2The preparation method of the electric contact material is characterized in that the preparation method of Ti3SiC2The skeleton step is performed in a vacuum autoclave.
9. silver-Ti according to claim 63SiC2The preparation method of the electric contact material is characterized by comprising the following steps of:
adding the Ti3SiC2The framework and the silver block are placed in a container; heating the container under the protective atmosphere or vacuum condition, raising the temperature to the infiltration treatment temperature, preserving the heat at the infiltration treatment temperature for a set time, and cooling to obtain the silver-Ti3SiC2An electrical contact material.
10. silver-Ti according to claim 6 or 93SiC2The preparation method of the electric contact material is characterized in that the infiltration treatment temperature is 1000-1400 ℃, preferably 1200 ℃; and/or
The set time is 1-2h, preferably 2 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115927900A (en) * | 2022-11-17 | 2023-04-07 | 东北大学 | Ag-Ti 3 SiC 2 Component regulation and control method of electric contact material |
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| CN112974774A (en) * | 2021-02-07 | 2021-06-18 | 中国科学院金属研究所 | Silver-based composite material and preparation method thereof |
| CN114005572A (en) * | 2021-10-19 | 2022-02-01 | 中国科学院金属研究所 | Silver-nickel bicontinuous phase material and preparation method thereof |
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| AT286423B (en) * | 1969-01-27 | 1970-12-10 | Plansee Metallwerk | Electric contact |
| JPS56146839A (en) * | 1980-04-12 | 1981-11-14 | Matsushita Electric Works Ltd | Manufacture of electrical contact material |
| CN101343700A (en) * | 2008-08-25 | 2009-01-14 | 倪树春 | Ag/Ti3SiC2 electric contact material and manufacturing process |
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