AU2020101306A4 - A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material And The Method For Preparing It - Google Patents

A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material And The Method For Preparing It Download PDF

Info

Publication number
AU2020101306A4
AU2020101306A4 AU2020101306A AU2020101306A AU2020101306A4 AU 2020101306 A4 AU2020101306 A4 AU 2020101306A4 AU 2020101306 A AU2020101306 A AU 2020101306A AU 2020101306 A AU2020101306 A AU 2020101306A AU 2020101306 A4 AU2020101306 A4 AU 2020101306A4
Authority
AU
Australia
Prior art keywords
max
mom
aon
electrical contact
core
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
AU2020101306A
Inventor
Jianxiang DING
Peiyan HUANG
Dongming Liu
Zhengming SUN
Dong Xu
Yuan Yang
Yuhui Zha
Shihong ZHANG
Xiao Zhang
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui University of Technology AHUT
Original Assignee
Anhui University of Technology AHUT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui University of Technology AHUT filed Critical Anhui University of Technology AHUT
Priority to AU2020101306A priority Critical patent/AU2020101306A4/en
Application granted granted Critical
Publication of AU2020101306A4 publication Critical patent/AU2020101306A4/en
Ceased legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • C04B35/5618—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 aluminium carbides
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C04B35/62615—High energy or reactive ball milling
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6265—Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • 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
    • H01H1/0237—Composite material having a noble metal as the basic material and containing oxides
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof

Abstract

of Description This invention discloses a core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material and the method for preparing it; the described MAX@MOm/AOn composite electrical contact reinforced phase material has a core-shell structure, the core is made of MAX phase material, and the shell is made up of oxide particles MOm and AO, or composite oxide layer MOm/AOn corresponding to the MAX phase material of the core; this invention also discloses the Ag/MAX@MOm/AO composite electrical contact material prepared by the above MAX@MOm/AOn material and the method for preparing it. After the MAX@MOm/AO composite electrical contact reinforced phase material prepared by this invention is compounded with the Ag matrix, the three-dimensional MAX plays the role of supporting the entire composite block structure, and the oxide particles MOm and AO, or the composite oxide layer MOm/AOn limits the interface diffusion between the Ag and MAX, maintains the conductivity of the composite material, and resists arc impact and absorbs arc energy to delay arc erosion damage in the process of electrical contact service. Drawings of Description Figure 1 -Ace V Spot Maqn Dot WDa 10 pmn 20 0 kV 3 0 3000x FE 7 ? Figure 2 1/1

Description

Drawings of Description
Figure 1
-Ace V Spot Maqn Dot WDa 10 pmn 20 0 kV 3 0 3000x FE 7 ?
Figure 2
1/1
Description
A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material and the Method for Preparing it
Technical field This invention belongs to the technical field of composite electrical contact material, in particular relates to a core-shell structure MAX@MOm/AO composite electrical contact reinforced phase material and the method for preparing it as well as an Ag/MAX@MOm/AO composite electrical contact material prepared by using the above reinforced phase material and the method for preparing it.
Technical Background Low voltage electrical contact material is an important application field of electrical alloy material, which is widely used in the control switches such as relay, contactor, breaker and so on in low voltage distribution equipment. At present, Ag/CdO is the main material for making electrical contact for low-voltage switch. Although the arc extinguishing characteristics of Ag/CdO are outstanding, the Cd vapor produced in the service process of Ag/CdO is harmful to the environment and human body. With the increasingly strict global environmental protection policy, it is urgent to find alternative materials without Cd electrical contact. The existing Ag/SnO2, Ag/ZnO, Ag/Ni, Ag/C, Ag/W and other materials have their own advantages, but there are still a series of problems such as processing difficulties, structure agglomeration, high contact resistance, high temperature rise and so on, so their ability to replace Ag/CdO is limited.
In recent years, a new layered structure material MAX phase has attracted much attention. This material has low room-temperature resistivity (49.5-134x10-3 Q-m), high thermal conductivity (78~111 W/m-K), good high temperature resistance and corrosion resistance, excellent machinability, and Ag/MAX composite electrical contact material has the same excellent arc erosion resistance as Ag/CdO under severe acceleration conditions, so MAX phase has great potential as a silver based reinforced phase material. However, the Ag-MAX interface reaction damages the conductivity of Ag/MAX composite material and limits its industrialization. Therefore, how to develop new environmentally friendly composite electrical contact material with outstanding performance on the basis of Ag/MAX material for replacing Ag/CdO is the key technical problem to be solved.
Invention Summary The purpose of this invention is to solve the above technical problems, provide an electrical contact reinforced phase material MOm/AO@MAX which can completely replace the CdO reinforced phase and the method for preparing it as well as an Ag/MAX@MOm/AO composite electrical contact material and the method for preparing it.
The first technical proposal of this invention is to provide a core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material;
The second technical proposal of this invention is to provide a method for preparing the above core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material;
The third technical proposal of this invention is to provide a Ag/MAX@MOm/AOn composite electrical contact material;
The fourth technical proposal of this invention is to provide the method for preparing the above Ag/MAX@MOm/AOn composite electrical contact material.
The first technical proposal of this invention: to provide a core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material, which has a core-shell structure, including a core and a shell. The core is a three-dimensional material MAX phase, and the shell is the oxide particles MOm and AOn or composite oxide layer MOm/AOn corresponding to the core MAX phase material;
MAX@MOm/AOn powder has a multi-composite structure. MOm/AOn has a novel structure and is obtained by oxidizing the three-dimensional MAX phase. The single oxide particles MOm and AO, or composite oxide layer MOm/AOn is attached to or coated on the surface of MAX, which can effectively limit the interface diffusion between Ag and MAX and prevent the structural and performance defects caused by the composition of the single MAX phase and Ag. The high hardness of the three-dimensional structure MAX, as the core of the material, plays a good role of mechanical support for the whole composite material; while the effect of the oxide particles MOm and AO, or composite oxide layer MOm/AOn of the shell on increasing the strength of the material is more obvious. In addition, the shell plays an active role in limiting the interface diffusion and maintaining the good conductivity of the composite material. After the composite electrical contact reinforced phase with MAX phase as the core, the oxide particles MOm and AO, or composite oxide layer MOm/AOn as the shell is compounded with Ag matrix, its conductivity, processability and arc erosion resistance are all good, which overcomes the defects of the decreased conductivity caused by the interface diffusion when the MAX phase is used as the reinforced phase material and the great material loss caused by the electromagnetic impact damage of arc on the material in the later stage of discharge.
Preferably, in the above core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material, the core MAX phase material is one of Ti 3 SiC 2 , Ti 3 AlC 2 , Ti 2AlC, Ti2SnC, Ti 2 SiC, V 2AlC, Cr2AlC, Cr2GaC, Nb2 AlC, Ta 4AC3, NbAlC 3, TiAN, (Tio.,Nbo. 5) 2AlC, (Vo. 5 , Cro.5 )3AlC and (Nbo., Ti. 2 ) 4 AlC 3 . These MAX materials are spherical particles with high hardness (modulus of elasticity E: 228~414 GPa), good conductivity (resistivity p: 0.22~0.55 Q-m) and self-lubrication.
Preferably, the shell is the oxide particles MOm and AO, or composite oxide layer MOm/AOnmaterial, that is, one or more of Ti 2 , Si 2 , A1 2 0 3 , SnO2, V203, V20 4
, V20 5, Cr203, Ga203, Nb 2 0 5, NbAlO 4, Ta20s and TiNb 20 7 ; or the shell is MOm/AOn composite oxide layer, that is, one or more of TiO2/SiO 2 , TiO2/Al 20 3, TiO2/SnO2, V 2 0 3/Al 20 3, V 20 4/Al 20 3, V 205 /Al 20 3, Cr203/Al203, Cr203/Ga203, Nb 205 /Al 20 3
, NbAlO 4/Al 20 3 , Ta20 5/Al203, TiNb 20 7/Al 20 3 , TiO 2/NbAlO 4 , TiO 2/NbAlO 4/Al 20 3 TiO 2/TiNb 2 O7/Al2 0 3 , V203/Cr203/Al203, V20 4/Cr203/Al203 and V20/Cr203/Al203. , These MOm/AOn materials are granular or layered.
The second technical proposal of this invention: to provide the method for preparing the above core-shell structure MOm/AOn composite electrical contact reinforced phase material, in particular, the matrix MAX phase material is oxidized in the controlled atmosphere to generate oxide particles MOm and AO or composite oxide layer MOm/AOn by in-situ pre-oxidation on its surface and form the MAX@MOm/AOn;
The oxide particles MOm and AO, or composite oxide layer MOm/AOn can be generated in situ on the surface of the matrix MAX material by pre-oxidizing it to form the MAX@MOm/AOn. It has low requirements for equipment, good repeatability, simple technology, low cost and obvious value of practical application. Moreover, the integrated structure of the shell MOm/AOn and the core MAX has stronger binding force, stronger ability of blocking interface diffusion and better performance of the integrated composite material.
Preferably, the method for preparing the above core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material comprises the following steps:
Si: Weigh the MAX phase powder, place it in a high temperature tube furnace, and introduce different content of controlled atmosphere;
S2: Heat the MAX phase powder in Step Si in the tube furnace at a certain heating rate;
S3: Heat the MAX phase powder in Step S2 to the corresponding temperature in the tube furnace;
S4: Keep the MAX phase powder in Step S3 at the corresponding temperature for a certain period of time;
S5: Cool the MAX phase powder in Step S4 to room temperature in a tube furnace at a certain rate.
Preferably, in the above method for preparing the core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material, the described atmosphere is that the oxygen concentration in the mixture is 20-80 Vol%;
It is simple and fast to oxidize MAX in the atmosphere of the mixture of "oxygen + argon", and the oxide particles MOm and AO, or composite oxide layer MOm/AOn obtained by in-situ oxidation are complete and uniformly distributed with ideal effect. This simple, efficient, low-cost, pollution-free and in-situ preparation method is incomparable by the preparation of oxide or oxide layer by chemical reaction.
Preferably, in the above method for preparing the core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material, the heating rate of tube furnace in Step S2 is 2-10 °C/min, the heating temperature in Step S3 is 700-1200 °C, the holding time in Step S4 is 0.5-5 hours, and the cooling rate in Step S5 is 5-10 °C/min.
The third technical proposal of this invention: an Ag/MAX@MOm/AOn composite electrical contact material. The Ag/MOm/AO@MAX composite electrical contact material is prepared with the above core-shell structure MAX@MOm/AOn as the composite electrical contact reinforced phase material, in which the core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material accounts for 3~40% of the mass fraction of the integrated material, and Ag accounts for 60-97% of the mass fraction of the integrated material;
After the MAX@MOm/AO is compounded with the Ag matrix, the MAX phase coated with oxide particles or oxide layer, as the core support structure, effectively enhances the overall strength of the Ag matrix composite material and helps to resist the damage of arc impact and thermal stress; in addition, the oxide particles MOm and AO, or the composite oxide layer of MOm/AOn on the surface of MAX effectively limits the interface reaction between Ag and MAX, maintains the good conductivity and thermal conductivity of the composite material, thus prevents the defects of structure and performance caused by the single MAX phase reinforced Ag matrix, obviously improves the arc erosion resistance of the Ag matrix composite electrical contact material, and reduces the material loss.
The fourth technical proposal of this invention: a method for preparing the Ag/MAX@MOm/AOn composite electrical contact material, which comprises the following steps:
SI: Take ethanol as the ball-milling medium, and add MAX@MOm/AOn powder and Ag powder to the ball mill according to the mass ratio for ball milling for a certain period of time. After ball milling, take out the mixture and put it in a drying oven for drying for a certain time to obtain the mixture;
S2: Add the mixture in Si to the cold stamping die for pressurization, and keep it for a certain period of time until it is formed into the block material blank;
S3: Introduce protective atmosphere into the tube furnace, put the blank obtained in Step S2 into the tube furnace for high temperature sintering in the protective atmosphere for a certain period of time, and then cool it naturally in the furnace to obtain the Ag/MAX@MOm/AOn composite electrical contact material.
Preferably, the mass ratio of powder: ethanol: balls in the above Step Si is 1:(1-3):(2-6), the ball-milling time is 0.5-8 hours, and the drying time is 1-5 hours; the forming pressure in the described Step S2 is 50-900 MPa, and the holding time is 1-15 minutes; in the described Step S3, argon or nitrogen is used as the protective atmosphere composition, the heating rate is 2-16 °C/min, the sintering temperature is
500-900 °C, and the holding time is 0.5-8 hours.
This invention at least includes the following beneficial effects:
The MAX@MOm/AOn prepared by the method of pre-oxidation to generate oxide particles or oxide layer on the surface of MAX phase in this application has a multi-composite core-shell structure, of which the mechanical properties are enhanced, the ability of blocking the interface reaction between Ag and MAX is improved, and the in-situ pre-oxidation method is simple in technology, low in cost and good in practicability. The Ag/MAX@MOm/AOn composite electrical contact material prepared with the MAX@MOm/AOn prepared in this application as the reinforced phase has excellent conductivity (the resistivity is 1.9-2.4 Q-cm, which is close to 1.6 Q-cm of pure Ag), moderate hardness (HV6580) and good processability, can be processed into various shapes of electrical contact according to the actual requirements of application, has excellent arc erosion resistance (the material mass loss after 6000 discharges under the national standard is only 105.8~120.5 mg), and significant silver saving effect. The reinforced phase MAX content in the Ag matrix accounts for up to 40 wt% of the composite material. It has simple preparation process and good practicability, is suitable for large-scale production and low-voltage switchgear such as contactor, breaker, relay, and brings social and economic value.
Other advantages, objectives and characteristics of this invention will be partly embodied by the following description, and partly understood by those skilled in the art through research and practice of this invention.
Description of Drawings Figure 1 is the SEM image of the Ti 3 SiC 2 powder of the core before the in-situ oxidation in Embodiment 1.
Figure 2 is the SEM image of the core-shell structure Ti 3 SiC 2 @TiO 2 composite electrical contact reinforced phase powder prepared in Embodiment 1.
Detailed Description of the Presently Preferred Embodiments This invention will be further described in detail below, so that those skilled in the art can embody it with reference to the instructions.
In order to explain the technical proposal of this invention more clearly, specific embodiments will be further described.
Embodiment 1 Put 10 g of Ti 3 SiC 2 powder into the high temperature tube furnace, heat it to 1200 °C at a heating rate of 10 °C/min in the atmosphere of "oxygen + argon" with oxygen content of 20 vol%, keep it for 0.5 hours and cool it to room temperature at a cooling rate of 10 °C/min to obtain the Ti 3 SiC 2 @TiO 2 powder of the core-shell structure; wet mix the Ti 3 SiC 2 @TiO 2 powder, which accounts for 3% of the mass fraction of the integrated material, and Ag powder with a mass fraction of 97%, in the ball mill tank with ethanol medium for 0.5 hours (the mass ratio of powder: ethanol: balls is 1:1:2), and then dry it for 1 hour to obtain the mixed powder; press the mixed powder in a cold press at 900 MPa for 15 minutes; put the block sample in the tube furnace, heat it at a heating rate of 2 °C/min to 500 °C under the protection of Ar atmosphere and keep it for 8 hours to obtain the Ag/Ti3SiC 2 @TiO 2 composite electrical contact material.
Embodiment 2 Put 10 g of Ti 3 AlC 2 powder into the high temperature tube furnace, heat it to 700 °C at a heating rate of 2 °C/min in the atmosphere of "oxygen + argon" with oxygen content of 80 vol%, keep it for 5 hours and cool it to room temperature at a cooling rate of 5 °C/min to obtain the Ti 3AC 2@TiO 2/Al 20 3 powder of the core-shell structure; wet mix the Ti 3 AC 2 @TiO 2 /Al2 0 3 powder, which accounts for 40% of the mass fraction of the integrated material, and Ag powder with a mass fraction of 60%, in the ball mill tank with ethanol medium for 8 hours (the mass ratio of powder: ethanol: balls is 1:3:6), and then dry it for 5 hour to obtain the mixed powder; press the mixed powder in a cold press at 50 MPa for 1 minute; put the block sample in the tube furnace, heat it at a heating rate of 16 °C/min to 900 °C under the protection of Ar atmosphere and keep it for 0.5 hours to obtain the Ag/Ti 3AC 2@TiO 2/Al20 3 composite electrical contact material.
Embodiment 3 Put 10 g of (Tio.,Nbo. 5) 2AlC powder into the high temperature tube furnace, heat it to 950 °C at a heating rate of 5 °C/min in the atmosphere of "oxygen + argon" with oxygen content of 40 vol%, keep it for 2.5 hours and cool it to room temperature at a cooling rate of 6°C/min to obtain the (Tio.,Nbo. 5) 2AlC@TiO 2/NbAlO 4 powder of the core-shell structure; wet mix the (Tio.,Nbo. 5) 2AlC@TiO 2/NbAlO 4 powder, which accounts for 25% of the mass fraction of the integrated material, and Ag powder with a mass fraction of 75%, in the ball mill tank with ethanol medium for 2 hours (the mass ratio of powder: ethanol: balls is 1:2:2), and then dry it for 1.5 hours to obtain the mixed powder; press the mixed powder in a cold press at 450 MPa for 4 minutes; put the block sample in the tube furnace, heat it at a heating rate of 7 °C/min to 800 °C under the protection of N 2 atmosphere and keep it for 4.5 hours to obtain the
Ag/(Tio.,Nb. 5) 2AlC@TiO 2/NbAlO4 composite electrical contact material.
Embodiment 4 Put 10 g of (Nbo.,Tio.2) 4AlC 3 powder into the high temperature tube furnace, heat it to 1080 °C at a heating rate of 3 °C/min in the atmosphere of "oxygen + argon" with oxygen content of 28 vol%, keep it for 4.5 hours and cool it to room temperature at a cooling rate of 4 °C/min to obtain the (Nb. 8 ,io.2)4AlC 3 @TiO 2/ TiO 2/NbAlO 4/Al 20 3 powder of the core-shell structure; wet mix the (Nbo.8 ,Tio.2) 4AlC 3 @TiO 2
/ TiO2/NbAlO4/Al20 3 powder, which accounts for 37% of the mass fraction of the integrated material, and Ag powder with a mass fraction of 63%, in the ball mill tank with ethanol medium for 7.5 hours (the mass ratio of powder: ethanol: balls is 1:2:4), and then dry it for 4.5 hours to obtain the mixed powder; press the mixed powder in a cold press at 850 MPa for 13 minutes; put the block sample in the tube furnace, heat it at a heating rate of 14 °C/min to 880 °C under the protection of N 2 atmosphere and keep it for 7.5 hours to obtain the Ag/(Nbo.,Tio. 2) 4AlC 3@TiO 2/NbAlO 4/Al 20 3 composite electrical contact material.
Contrastive example 1 Wet mix the CdO powder, which accounts for 20% of the mass fraction of the integrated material, and Ag powder with a mass fraction of 80%, in the ball mill tank with medium for 3 hours (balls: alcohol: balls = 4.5:2.5:1), and other preparation steps are the same as those in Embodiment 5.
Test the performance of the electrical contact materials prepared from Embodiment 1-15 and Contrastive example 1 (under the national standard condition of 380V/50A/AC-3), and the test results are shown in Table 1;
Table 1 Performance test results of the composite electrical contact material of Embodiment 1-15 and Contrastive example 1 rformance Mass loss of Density Relative Resistivity Hardness 6000 arc (g/cm 3) density(%) ( -cm) (HV) discharges
Sample (mg)
Embodiment 8.47 98.5 2.1 65 120.5 1
Embodiment 8.65 98.8 2.4 67 117.2 2 Embodiment 8.49 99.1 2.2 70 112.8
Embodiment 8.62 99.4 1.9 80 105.8 4
Contrastive 8.97 99.2 2.0 92 120.9 example 1
It can be concluded from Table 1 that the performance test results of the Ag/MAX@MOm/AO composite electrical contact material prepared after reinforcing the Ag matrix with the MAX@MOm/AOn with a core-shell structure prepared by in-situ oxidation technology in this application as the reinforced phase material show that this composite electrical contact material has high density (8.48-8.58 g/cm 3), good conductivity (resistivity 1.9-2.4 Q-cm), moderate hardness (HV65-80) and excellent arc erosion resistance (the material mass loss after 6000 discharges is only 105.8~120.5 mg). The properties of the Ag/MAX@MOm/AOn composite electrical contact material prepared in this application are far superior to those of the Ag/CdO commercial composite electrical contact materials.
Although the embodiments of this invention have been disclosed as above, this invention is not limited to the application listed in the instructions and embodiments. It can be completely applied to various fields suitable for this invention. For those familiar with the art, additional modifications may be easily made. Therefore, without departing from the general concept defined by the claims and the equivalent range, this invention is not limited to specific details and the illustration herein.

Claims (8)

Claims
1. A core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material, characterized in that it has a core-shell structure, including a core and a shell. The described core is MAX phase. The described shell is oxide particles MOm and AO, or composite oxide layer MOm/AOn.
2. The core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material according to Claim 1 is characterized in that the core MAX phase material is one of Ti 3 SiC 2 , Ti 3 AC 2 , Ti 2AC, Ti2SnC, Ti2 SiC, V2AC, Cr2AC, Cr2GaC, Nb 2AlC, Ta 4AlC3, NbAC 3 , TiAN, (Tio.,Nb. 5) 2AlC, (Vo. 5 , Cro.5 )3AlC and (Nbo.8
, Ti. 2 ) 4 AlC 3 , the shell is the MOm/AOn oxide particles corresponding to the core MAX phase material, i.e. one or more of Ti 2, Si 2, A1 2 0 3 , Sn2, V203, V20 4 , V205 , Cr203, Ga203, Nb 2 0 5, NbAlO4 , Ta205 and TiNb 2 0 7; or the shell is MOm/AOn composite oxide layer, that is, one or more of Ti2/SiO 2 , TiO2/Al 2 0 3 , Ti2/SnO2, V 2 3/Al 2 0 3
, V 20 4/Al 20 3, V 20 5 /Al 20 3, Cr203/Al203, Cr203/Ga203, Nb 205 /Al 20 3 , NbAlO 4/Al 20 3
, Ta20 5 /Al203, TiNb 20 7/Al 20 3, TiO 2/NbAlO 4 , TiO 2/NbAlO 4/Al 20 3
, TiO 2/TiNb 2 O7/Al2 0 3 , V203/Cr203/Al203, V20 4/Cr203/Al203 and V20/Cr203/Al203.
3. A method for preparing the core-shell structure MAX@MOm/AO composite electrical contact reinforced phase material as described in Claim 1 or 2, characterized in that it comprises the following steps:
Si: Weigh the MAX phase powder, place it in a high temperature tube furnace, and introduce different content of controlled atmosphere;
S2: Heat the MAX phase powder in Step S Iin the tube furnace at a certain heating rate;
S3: Heat the MAX phase powder in Step S2 to the corresponding temperature in the tube furnace;
S4: Keep the MAX phase powder in Step S3 at the corresponding temperature for a certain period of time;
S5: Cool the MAX phase powder in Step S4 to room temperature in a tube furnace at a certain rate.
4. The method for preparing the core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material as described in Claim 3 is characterized in that the described controlled atmosphere is a mixture of "oxygen + argon", and the oxygen concentration in the described mixture is 20-80 Vol%.
5. The method for preparing the core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material as described in Claim 3 is characterized in that the heating rate of tube furnace in Step S2 is 2-10 °C/min, the heating temperature in Step S3 is 700-1200 °C, the holding time in Step S4 is 0.5-5 hours, and the cooling rate in Step S5 is 5-10 °C/min.
6. An Ag/MAX@MOm/AOn composite electrical contact material, characterized in that it comprises the core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material as described in any one of Claims 1-5, in which Ag accounts for 60-97% of the mass fraction of the integrated material, and the core-shell structure MAX@MOm/AOn composite electrical contact reinforced phase material accounts for 3-40% of the mass fraction of the integrated material.
7. A method for preparing the Ag/MAX@MOm/AOn composite electrical contact material as described in Claim 6, characterized in that it comprises the following steps:
Si: Take ethanol as the ball-milling medium, and add MAX@MOm/AOn powder and Ag powder to the ball mill according to the mass ratio for ball milling for a certain period of time. After ball milling, take out the mixture and put it in a drying oven for drying for a certain time to obtain the mixture;
S2: Add the mixture in S Ito the cold stamping die for pressurization, and keep it for a certain period of time until it is formed into the block material blank;
S3: Introduce protective atmosphere into the tube furnace, put the blank obtained in Step S2 into the tube furnace for high temperature sintering in the protective atmosphere for a certain period of time, and then cool it naturally in the furnace to obtain the Ag/MAX@MOm/AOn composite electrical contact material.
8. The method for preparing the Ag/MAX@MOm/AOn composite electrical contact material as described in Claim 7 is characterized in that the mass ratio of the powder, ethanol and balls in the described Step Sl is 1:(1-3):(2-6), the ball-milling time is 0.5-8 hours, and the drying time is 1-5 hours; the forming pressure in the described
Step S2 is 50-900 MPa, and the holding time is 1-15 minutes; in the described Step S3, argon or nitrogen is used as the protective atmosphere, the heating rate is 2-16 °C/min, the sintering temperature is 500-900 °C, and the holding time is 0.5-8 hours.
AU2020101306A 2020-07-09 2020-07-09 A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material And The Method For Preparing It Ceased AU2020101306A4 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2020101306A AU2020101306A4 (en) 2020-07-09 2020-07-09 A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material And The Method For Preparing It

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
AU2020101306A AU2020101306A4 (en) 2020-07-09 2020-07-09 A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material And The Method For Preparing It

Publications (1)

Publication Number Publication Date
AU2020101306A4 true AU2020101306A4 (en) 2020-08-13

Family

ID=71949519

Family Applications (1)

Application Number Title Priority Date Filing Date
AU2020101306A Ceased AU2020101306A4 (en) 2020-07-09 2020-07-09 A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material And The Method For Preparing It

Country Status (1)

Country Link
AU (1) AU2020101306A4 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114133273A (en) * 2021-12-06 2022-03-04 湖北大学 Preparation method of core-shell structure piezoelectric material and piezoelectric nano generator

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114133273A (en) * 2021-12-06 2022-03-04 湖北大学 Preparation method of core-shell structure piezoelectric material and piezoelectric nano generator

Similar Documents

Publication Publication Date Title
US6551374B2 (en) Method of controlling the microstructures of Cu-Cr-based contact materials for vacuum interrupters and contact materials manufactured by the method
Wei et al. Microstructure, corrosion resistance and oxidation behavior of Cr-coatings on Zircaloy-4 prepared by vacuum arc plasma deposition
Li et al. Material transfer behavior of AgTiB2 and AgSnO2 electrical contact materials under different currents
CN111834135B (en) MAX @ MOm/AOn electrical contact enhanced phase material, composite electrical contact material and preparation method
JP5419465B2 (en) Creep-resistant ferritic steel
AU2020101306A4 (en) A Core-shell Structure MAX@MOm/AOn Composite Electrical Contact Reinforced Phase Material And The Method For Preparing It
CN102426867B (en) Whisker reinforced copper-based electrical contact material and preparation method thereof
CN100588728C (en) Method for manufacturing CuWCr composite material by using WCr alloy powder
CN102290261A (en) Silver copper based metal oxide electrical contact material containing adding elements and preparation method thereof
AU2021354815A1 (en) Copper-tungsten alloy material, preparation method therefor, and application thereof
CN103509974A (en) Manufacturing method for precisely cast titanium alloy impeller
CN113707360B (en) Thick film resistor paste suitable for different types of stainless steel substrates
CN106319288A (en) Directly-introduced and in-situ generated TiC particle commonly-enhanced nickel-base composite and preparing method and application thereof
CN109859920A (en) A kind of highly resistance corrosion richness high abundance rare-earth permanent magnet and preparation method
CN112620640A (en) Preparation method of AgNi electrical contact material based on recycling of AgC scrap
EP0929088B1 (en) Contact material
Han et al. Interfacial thermal stress relief in Ag–SnO2 composites by in situ formation of CuO nanoparticles additive on SnO2
CN107299269A (en) A kind of W Cr Al composites of resistance to high temperature oxidation and preparation method thereof
CN114515829B (en) Preparation method of layered gradient W-Cu composite material
Li et al. Effect of short-time hot repressing on a Ag-SnO2 contact material containing CuO additive
CN109576537B (en) WC-Co nano reinforced high-silicon aluminum alloy for electric power connection hardware fitting and preparation method thereof
Wlodarczyk Porous composite for bipolar plate in low emission hydrogen fuel cells
KR100283207B1 (en) Metal Connecting Material for Solid Oxide Fuel Cell and Manufacturing Method Thereof
CN110735078A (en) CrFeMnMoSiZr high-entropy alloy porous material and preparation method thereof
Han et al. Arc erosion behaviors of the densified Ag-SnO2 contact materials containing sub-micron and nano In2O3 additives

Legal Events

Date Code Title Description
FGI Letters patent sealed or granted (innovation patent)
MK22 Patent ceased section 143a(d), or expired - non payment of renewal fee or expiry