CN112142472A - Cr (chromium)2AlC/MXene composite material and preparation method thereof - Google Patents

Cr (chromium)2AlC/MXene composite material and preparation method thereof Download PDF

Info

Publication number
CN112142472A
CN112142472A CN202011022145.3A CN202011022145A CN112142472A CN 112142472 A CN112142472 A CN 112142472A CN 202011022145 A CN202011022145 A CN 202011022145A CN 112142472 A CN112142472 A CN 112142472A
Authority
CN
China
Prior art keywords
alc
mxene
composite material
preparation
powder
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.)
Granted
Application number
CN202011022145.3A
Other languages
Chinese (zh)
Other versions
CN112142472B (en
Inventor
应国兵
胡聪
刘璐
吴毅然
张建新
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.)
Hohai University HHU
Original Assignee
Hohai University HHU
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 Hohai University HHU filed Critical Hohai University HHU
Priority to CN202011022145.3A priority Critical patent/CN112142472B/en
Publication of CN112142472A publication Critical patent/CN112142472A/en
Application granted granted Critical
Publication of CN112142472B publication Critical patent/CN112142472B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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
    • 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
    • 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
    • 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
    • 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
    • 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
    • C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
    • 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
    • C04B35/64—Burning or sintering processes
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—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
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3839—Refractory metal 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
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3839—Refractory metal carbides
    • C04B2235/3843—Titanium 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
    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/404—Refractory metals
    • 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
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • 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
    • C04B2235/65—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
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention relates to Cr2The preparation method of the AlC/MXene composite material comprises the following steps: (1) preparation of cermet MAX: mixing M, Al and C powder, and sintering at high temperature and no pressure to obtain a block, wherein M is a transition metal; (2) preparation of MXene: grinding the MAX blocks prepared in the step (1) into powder, corroding the MAX blocks by using a mixed solution of hydrochloric acid and lithium fluoride or hydrofluoric acid, washing a corrosion product by using clear water for multiple times, and then putting the MAX blocks into a vacuum drying oven to be dried into powder to obtain MXene powder; (3) cr (chromium) component2Preparing an AlC/MXene composite material: MXene powder and Cr prepared in the step (2)2Mixing AlC ceramic powder, placing into a ball milling tank, adding anhydrous ethanol, wet mixing, and mixingDrying the material by a rotary evaporator to obtain the product. The material is prepared by using multiple layers of MXene and Cr originally produced in water environment2Compounding AlC material to form Cr2AlC/Mxene composite material, Cr2The bending strength and the fracture toughness of the AlC/Mxene composite material are obviously improved, and the mechanical property is excellent.

Description

Cr (chromium)2AlC/MXene composite material and preparation method thereof
Technical Field
The invention relates to a composite material, in particular to Cr2AlC/MXene composite material and a preparation method thereof.
Background
In recent years, with the discovery of graphene and its unique physical and chemical properties, the research heat of two-dimensional crystals is raised. The two-dimensional layered nano compound is a material with a graphene-like structure, has various excellent performances due to the characteristic of high specific surface area, and comprises transition metal disulfides, metal oxides and the like besides graphene. In recent years, barsum and the like selectively etches away Al atoms in a three-dimensional layered compound MAX by using hydrofluoric acid to obtain a two-dimensional crystal compound with a graphene-like structure, and the two-dimensional crystal compound is named as MXene. Having the chemical formula Mn+1XnN =1, 2, 3, M is an early transition metal element, and X is a carbon/nitrogen element. The MXene precursor is MAX which is a ternary layered structure with the excellent properties of metal and ceramic, M, X, n is the same as the above, A is a main group element, more than 60 MAX phases are known at present, and a large amount of MXene with special properties can be prepared by etching, which is of great significance for the preparation and research of two-dimensional crystal materials.
Ternary laminated ceramic Mn+1AXn(wherein M is a transition group element, A is a IIIA or IVA group element, X is C or N, N =1, 2, 3; MAX for short) is a series of novel machinable ceramic materials, has the advantages of metal and ceramic, not only has the characteristics of high temperature resistance, oxidation resistance and high strength of the ceramic materials, but also has the characteristics of high electrical conductivity, heat conduction, easy processing, plasticity and the like of the metal, and thus has wide application prospect. With the development of aviation and aerospace industries, the development of novel functional and structural ceramics under special conditions is particularly urgent. The ternary layered ceramic has special properties of metal and ceramic, and the composite material has wide application prospect, so that the development and preparation of the novel ternary layered ceramic composite material have extremely important significance.
The MXene is prepared in a water environment at the present stage, and the MXene is difficult to store for a long time due to extremely high chemical activity of the surface of the MXene.
Disclosure of Invention
The invention aims to provide a ternary layered ceramic composite material with excellent mechanical property, which is prepared by using multiple layers of MXene and Cr originally produced in water environment2Compounding AlC material to form Cr2AlC/Mxene composite material, Cr2The bending strength and the fracture toughness of the AlC/Mxene composite material are obviously improved, and the mechanical property is excellent.
The technical scheme adopted by the invention is as follows: cr (chromium)2The preparation method of the AlC/MXene composite material comprises the following steps
(1) Preparation of cermet MAX: mixing M, Al and C powder, and sintering at high temperature and no pressure to obtain a block, wherein M is a transition metal;
(2) preparation of MXene: grinding the MAX blocks prepared in the step (1) into powder, corroding the MAX blocks by using a mixed solution of hydrochloric acid and lithium fluoride or hydrofluoric acid, washing a corrosion product by using clear water for multiple times, and then putting the MAX blocks into a vacuum drying oven to be dried into powder to obtain MXene powder;
（3）Cr2preparing an AlC/MXene composite material: MXene powder and Cr prepared in the step (2)2Mixing AlC ceramic powder, putting into a ball milling tank, adding absolute ethyl alcohol for wet mixing, and drying the mixed material by adopting a rotary evaporator to obtain the product.
Further, M is one or more of Ti, Nb, V, Cr or Ta.
Furthermore, the quality of MXene is MXene and Cr2The mass sum of AlC is 0-10%.
Further, MXene and Cr2And placing AlC in a ball milling tank for ball milling, wherein the ball-to-material ratio is 5: 1.
further, the ball milling and mixing time is 8-12 h.
Furthermore, the sintering temperature is 1350-1450 ℃.
Further, the sintering method is selected to be spark plasma sintering.
Hair brushThe invention also relates to Cr prepared by the preparation method2AlC/MXene composite material.
The beneficial effects produced by the invention comprise: (1) the invention effectively leads the multilayer MXene and Cr originally produced in the water environment2Compounding AlC material to form Cr2The preparation method of the AlC/Mxene composite material has the advantages of simple process, short time, high efficiency and low cost.
(2) The method has easily controlled conditions, can accurately quantify the addition amount of the multiple layers of MXene, and can prepare the composite materials with different MXene addition ratios.
(3) Cr prepared by the method2The bending strength and the fracture toughness of the AlC/Mxene composite material are obviously improved, and the mechanical property is excellent.
Drawings
FIG. 1 shows Cr obtained in example 1 of the present invention2Cr in AlC/MXene composite material2AlC/Ti3C2The bending strength of (a);
FIG. 2 shows Cr obtained in example 3 of the present invention2Cr in AlC/MXene composite material2AlC/Ti3C2Fracture toughness of the composite.
Detailed Description
The invention is explained in further detail below with reference to the figures and the embodiments, but it should be understood that the scope of protection of the invention is not limited to the embodiments.
Example 1
Cr2The preparation method of the AlC/Mxene composite material comprises the following steps:
firstly, preparing MXene:
(1) uniformly mixing Ti, Al and C powder according to the molar ratio of 3:1.2:2, and preparing high-purity ternary layered Ti at 1500 ℃ by a pressureless sintering process3AlC2Ceramic bulk material, Ti to be produced3AlC2Drilling powder by a drilling machine to obtain Ti3AlC2Ceramic powder. Prepared Ti3AlC2Sieving the ceramic powder with a 200-mesh sieve;
(2) 3g of prepared Ti3AlC2Adding ceramic powder into 30ml of mixed solution of 12mol/ml hydrochloric acid and 3g of lithium fluoride, adding a magnetic rotor, stirring for 48 hours in an oil bath environment at 40 ℃, and corroding Ti3AlC2An Al atomic layer;
(3) washing the corroded suspension of the mixture with 80ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6;
(4) and putting the obtained precipitate into a vacuum drying oven for drying for 10-48 h.
II, Cr2Preparation of AlC/MXene composite material
(1) Weighing the mass of the taken multi-layer MXene powder;
(2) prepared Cr2The mass of AlC is 100g, and the mass fractions of MXene planned to be added are 1%, 2% and 4%, so that 1g, 2g and 4g of multi-layer MXene powder are required;
(3) respectively putting the weighed powder into a ball milling tank, and controlling the ball-material ratio to be 5: 1;
(4) adding 50ml of absolute ethyl alcohol into each ball milling tank;
(5) placing the mixture on a ball mill for wet mixing for 10 hours, and drying the mixture by adopting a vacuum pump and a rotary evaporator;
(6) sintering the dried powder by adopting a discharge plasma technology, wherein the sintering temperature is 1350 ℃.
FIG. 1 shows Cr obtained in example 1 of the present invention2Cr in AlC/MXene composite material2AlC/Ti3C2Bending strength of (2), wherein 0wt.% corresponds to pure Cr2AlC material, Cr, depending on the amount of MXene added (1wt.%, 2wt.% and 4wt.%)2The bending strength of the AlC/MXene composite material can be changed.
Example 2
Cr2The preparation method of the AlC/MXene composite material comprises the following steps:
firstly, preparing MXene:
(1) uniformly mixing V powder, Al powder and C powder according to the molar ratio of 2:1.3:1, and preparing the high-purity ternary laminar V through a pressureless sintering process at 1500 DEG C2AlC potteryCeramic bulk material, V to be prepared2Drilling powder for an AlC ceramic material by using a drilling machine to obtain V2AlC ceramic powder. Prepared V2Sieving AlC ceramic powder with 325 mesh sieve;
(2) two portions are prepared, each portion using 3g of V prepared2Adding AlC ceramic powder into a mixed solution of 30ml of hydrochloric acid with the concentration of 10mol/ml and 3g of lithium fluoride, adding a magnetic rotor, stirring for 72 hours in an oil bath environment at 50 ℃, and corroding V2An Al atomic layer in AlC;
(3) washing the corroded suspension of the mixture with 45ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6;
(4) transferring the two precipitates into a centrifuge tube, washing with 45ml of absolute ethyl alcohol and centrifuging, pouring out the supernatant, and repeating for 2 times;
(5) and (3) putting the obtained precipitate into a vacuum drying oven for drying for 10-48h to obtain multi-layer MXene powder.
II, Cr2Preparation of AlC/MXene composite material
(1) Weighing the mass of the multi-layer MXene powder by using an electronic scale;
(2) prepared Cr2The mass of the AlC is 100g, and the mass fractions of the MXene planned to be added are 1%, 2% and 4%, so that the MXene colloidal solution needs 1g, 2g and 4g respectively;
(3) respectively putting the weighed powder into a ball milling tank, and controlling the ball-material ratio to be 5: 1;
(4) adding 50ml of absolute ethyl alcohol into each ball milling tank;
(5) placing the mixture on a ball mill for wet mixing for 12 hours, and drying the mixture by adopting a vacuum pump and a rotary evaporator;
(6) sintering the dried powder by adopting a discharge plasma technology, wherein the sintering temperature is 1400 ℃.
Example 3
Cr2The preparation method of the AlC/MXene composite material comprises the following steps:
firstly, preparing MXene:
(1) mixing Ta, Al and C powder in the molar ratio of 2 to 1.2 to 1, and pressureless sintering at 1200 deg.cPreparation of high-purity ternary layered Ta2AlC ceramic block material, Ta to be prepared2Drilling powder for an AlC ceramic material by a drilling machine to obtain Ta2AlC ceramic powder. Prepared Ta2Sieving AlC ceramic powder with 200 mesh sieve;
(2) 3g of prepared Ta2Adding AlC ceramic powder into 30ml of aqueous solution with HF content of 50%, adding a magnetic rotor, stirring for 72h in an oil bath environment at 50 ℃, and corroding Ta2An Al atomic layer in AlC;
(3) washing the corroded suspension of the mixture with 40ml of deionized water, centrifuging, pouring out the supernatant, and repeating the steps until the pH value of the supernatant is more than or equal to 6;
(4) washing with 40ml of absolute ethanol, centrifuging, pouring out the supernatant, and repeating for 2 times;
(5) and (4) putting the obtained precipitate into a vacuum drying oven for drying for 36h to obtain multi-layer MXene powder.
II, Cr2Preparation of AlC/MXene composite material
(1) Weighing the mass of the multi-layer MXene powder by using an electronic scale;
(2) prepared Cr2The mass of the AlC is 100g, and the mass fractions of the MXene planned to be added are 1%, 2% and 4%, so that the MXene colloidal solution needs 1g, 2g and 4g respectively;
(3) respectively putting the weighed powder into a ball milling tank, and controlling the ball-material ratio to be 5: 1;
(4) adding 50ml of absolute ethyl alcohol into each ball milling tank;
(5) placing the mixture on a ball mill for wet mixing for 8 hours, and drying the mixture by adopting a vacuum pump and a rotary evaporator;
(6) sintering the dried powder by adopting a discharge plasma technology, wherein the sintering temperature is 1450 ℃.
FIG. 2 shows Cr obtained in example 3 of the present invention2Cr in AlC/MXene composite material2AlC/Ti3C2Fracture toughness of the composite, wherein 0wt.% corresponds to pure Cr2AlC material, Cr, depending on the amount of MXene added (1wt.%, 2wt.% and 4wt.%)2The fracture toughness of the AlC/MXene composite material can change.
On one hand, the ternary layered ceramic matrix composite prepared by the method can make up for certain defects of ternary ceramics, such as relatively low strength and hardness; on the other hand, the good high-temperature oxidation resistance, high heat conduction, electric conduction and other properties of the ternary ceramic can be kept, and other function strengthening phases are continuously added to obtain a composite material with higher structural or functional properties, such as continuous increase of electric conduction, heat conduction and other properties.
In the description of the present application, it is to be understood that the terms "central," "longitudinal," "lateral," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings for the convenience of description and simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be considered limiting of the claimed invention.
The above description is only a preferred embodiment of the present invention, and the present invention is not limited to the content of the embodiment. It will be apparent to those skilled in the art that various changes and modifications can be made within the technical scope of the present invention, and any changes and modifications made are within the protective scope of the present invention.

Claims (8)

1. Cr (chromium)2The preparation method of the AlC/MXene composite material is characterized by comprising the following steps: comprises the following steps
(1) Preparation of cermet MAX: mixing M, Al and C powder, and sintering at high temperature and no pressure to obtain a block, wherein M is a transition metal;
(2) preparation of MXene: grinding the MAX blocks prepared in the step (1) into powder, corroding the MAX blocks by using a mixed solution of hydrochloric acid and lithium fluoride or hydrofluoric acid, washing a corrosion product by using clear water for multiple times, and then putting the MAX blocks into a vacuum drying oven to be dried into powder to obtain MXene powder;
（3）Cr2preparing an AlC/MXene composite material: MXene powder and Cr prepared in the step (2)2Mixing AlC ceramic powder, and placing into a ball milling tankAdding absolute ethyl alcohol, wet mixing, and drying the mixed material by using a rotary evaporator to obtain the finished product.
2. The Cr of claim 12The preparation method of the AlC/MXene composite material is characterized by comprising the following steps: and M is one or more of Ti, Nb, V, Cr or Ta.
3. The Cr of claim 12The preparation method of the AlC/MXene composite material is characterized by comprising the following steps: the quality of MXene is MXene and Cr2The mass sum of AlC is 0-10%.
4. The Cr of claim 12The preparation method of the AlC/MXene composite material is characterized by comprising the following steps: the MXene and Cr2And placing AlC in a ball milling tank for ball milling, wherein the ball-to-material ratio is 5: 1.
5. the Cr of claim 12The preparation method of the AlC/MXene composite material is characterized by comprising the following steps: the ball milling and mixing time is 8-12 h.
6. The Cr of claim 12The preparation method of the AlC/MXene composite material is characterized by comprising the following steps: the sintering temperature is 1350-1450 ℃.
7. The Cr of claim 12The preparation method of the AlC/MXene composite material is characterized by comprising the following steps: the sintering method chosen is spark plasma sintering.
8. Cr prepared by the preparation method of any one of claims 1 to 72AlC/MXene composite material.
CN202011022145.3A 2020-09-25 2020-09-25 Cr (chromium)2AlC/MXene composite material and preparation method thereof Active CN112142472B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011022145.3A CN112142472B (en) 2020-09-25 2020-09-25 Cr (chromium)2AlC/MXene composite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011022145.3A CN112142472B (en) 2020-09-25 2020-09-25 Cr (chromium)2AlC/MXene composite material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112142472A true CN112142472A (en) 2020-12-29
CN112142472B CN112142472B (en) 2021-10-15

Family

ID=73897095

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011022145.3A Active CN112142472B (en) 2020-09-25 2020-09-25 Cr (chromium)2AlC/MXene composite material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112142472B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113480313A (en) * 2021-08-06 2021-10-08 航天特种材料及工艺技术研究所 MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170088429A1 (en) * 2015-09-24 2017-03-30 Samsung Electronics Co., Ltd. Mxene nanosheet and manufacturing method thereof
CN109880290A (en) * 2019-01-17 2019-06-14 河海大学 A kind of preparation method of epoxy resin/MXene composite material
CN110433834A (en) * 2019-08-30 2019-11-12 福建工程学院 A kind of MXene/TiO of two-dimensional slice material modification2The preparation and application of composite material
CN110699568A (en) * 2019-09-12 2020-01-17 安徽工业大学 Shell-core structure MXene @ MAX composite contact reinforcing phase material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170088429A1 (en) * 2015-09-24 2017-03-30 Samsung Electronics Co., Ltd. Mxene nanosheet and manufacturing method thereof
CN109880290A (en) * 2019-01-17 2019-06-14 河海大学 A kind of preparation method of epoxy resin/MXene composite material
CN110433834A (en) * 2019-08-30 2019-11-12 福建工程学院 A kind of MXene/TiO of two-dimensional slice material modification2The preparation and application of composite material
CN110699568A (en) * 2019-09-12 2020-01-17 安徽工业大学 Shell-core structure MXene @ MAX composite contact reinforcing phase material and preparation method thereof

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
GUOBING YING ET.AL: "Synthesis and mechanical properties of nano-layered composite", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
冯爱虎 等: "Cr2AlC陶瓷的无压合成及氢氟酸腐蚀行为研究", 《硅酸盐通报》 *
李勉 等: "三元层状碳氮化合物(MAX 相)及其衍生二维纳米材料(MXene)研究趋势与展望", 《无机材料学报》 *
淳道勇: "新型MXene 复合吸波材料研究进展", 《广州化工》 *
王一博 等: "二维材料MXene制备及其在电催化领域的研究进展", 《电源技术》 *
田宝娜 等: "三元纳米层状Ta2AlC原位合成机制", 《人工晶体学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113480313A (en) * 2021-08-06 2021-10-08 航天特种材料及工艺技术研究所 MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof
CN113480313B (en) * 2021-08-06 2022-06-10 航天特种材料及工艺技术研究所 MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof

Also Published As

Publication number Publication date
CN112142472B (en) 2021-10-15

Similar Documents

Publication Publication Date Title
Fu et al. MAX phases as nanolaminate materials: chemical composition, microstructure, synthesis, properties, and applications
Luo et al. Flexible MXene‐Based Composite Films: Synthesis, Modification, and Applications as Electrodes of Supercapacitors
CN100363303C (en) Silicon carbide base multiphase composite ceramic and its preparation method
CN112142472B (en) Cr (chromium)2AlC/MXene composite material and preparation method thereof
CN109650391B (en) Preparation method of two-dimensional vanadium carbide MXene
CN106477578A (en) A kind of MXene two-dimensional material preparation method based on acid deep co-melting solvent
Chen et al. From high-yield Ti3AlCN ceramics to high-quality Ti3CNTx MXenes through eliminating Al segregation
CN114180969B (en) Preparation method and application of nitrogen-containing high-entropy MAX phase material and two-dimensional material
CN112226644B (en) MXene reinforced copper-based composite material and preparation method thereof
CN104725049B (en) A kind of preparation method of aluminium nitride/boron nitride composite ceramic powder
CN112592183B (en) Preparation method of Zr-Al-C series MAX phase ceramic powder product
CN100532319C (en) Mo-corundum ceramic material and low-temperature sintering method
CN102659106A (en) Pressureless sintering method for synthesizing high-purity Ti3SiC2 powder
CN110105069A (en) A kind of new MAX phase lamellar compound and preparation method thereof
Liang et al. Fabrication of in-situ Ti-Cx-N1− x phase enhanced porous Si3N4 absorbing composites by gel casting
CN1498876A (en) Method for preparing composite engineering ceramics material of nano ZrO2 (Y2O3)/A12O3/Cu
CN100509692C (en) Tungsten corundum ceramic material and low temperature sintering method
WO2015173188A1 (en) MAX PHASE MATERIALS FREE OF THE ELEMENTS Al AND Si
CN111041314B (en) High-strength molybdenum alloy rod and preparation method thereof
WO2008059864A1 (en) Method for producing magnesium diboride superconductor
CN111763089A (en) Preparation method of ternary boride ceramic material with laminated structure and product thereof
CN1286774C (en) Niobate leadless piezoelectric material material and preparation method thereof
CN114108069B (en) Preparation method and application of organic-inorganic hybrid lead-free piezoelectric crystal
Liao et al. First-principles study of oxygen incorporation and migration mechanisms in Ti2AlC
CN115159519A (en) Method for purifying natural graphite by pressurization electrolysis

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant