CN112142472B - Cr (chromium)2AlC/MXene composite material and preparation method thereof - Google Patents

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

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CN112142472B
CN112142472B CN202011022145.3A CN202011022145A CN112142472B CN 112142472 B CN112142472 B CN 112142472B CN 202011022145 A CN202011022145 A CN 202011022145A CN 112142472 B CN112142472 B CN 112142472B
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mxene
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应国兵
胡聪
刘璐
吴毅然
张建新
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Hohai University HHU
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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, 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. 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 originally in a water environmentMulti-layer MXene and Cr produced in the process2Compounding 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.
The 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 Cr2Preparation of AlC/Mxene composite materialThe method 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 ceramic block 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 prepared230ml of hydrochloric acid with the concentration of 10mol/ml and 3g of lithium fluoride are added into the AlC ceramic powder to be mixedAdding a magnetic rotor into the mixed solution, 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) uniformly mixing Ta, Al and C powder according to the molar ratio of 2:1.2:1, and preparing high-purity ternary layered Ta at 1200 ℃ by a pressureless sintering process2AlC 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 30ml of water solution with HF content of 50% into AlC ceramic powderAdding magnetic rotor into the solution, stirring for 72h in 50 deg.C oil bath environment, 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 (4)

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 preparing a block by high-temperature pressureless sintering, wherein the selected sintering method is spark plasma sintering, the sintering temperature is 1350-1450 ℃, and M is 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, wherein the mass of MXene is less than that of MXene and Cr210% of the sum of the mass of AlC; putting the mixture into a ball milling tank for ball milling, wherein the ball material ratio is 5: 1, adding absolute ethyl alcohol for wet mixing, and drying the mixed material by adopting a rotary evaporator to obtain the composite material.
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 ball milling and mixing time is 8-12 h.
4. Cr prepared by the preparation method of any one of claims 1 to 32AlC/MXene composite material.
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