CN109712769B - MXene-magnetic metal composite material and preparation method thereof - Google Patents
MXene-magnetic metal composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of preparation of nano magnetic composite materials, and discloses an MXene-magnetic metal composite material and a preparation method thereof. The magnetic nano-particles are composed of flake MXene and magnetic metal nano-particles uniformly loaded on the MXene. Dispersing MXene in a mixed solution composed of ethylene glycol and water, uniformly stirring, adding magnetic metal salt, stirring, adding NaOH to adjust the pH value of the system to 8-14, adding hydrazine hydrate, and uniformly stirring; heating to 60-120 ℃ and preserving heat for 0.2-8 h; and cooling, separating, washing and drying to obtain the MXene-magnetic metal composite material. The method comprises the steps of taking ethylene glycol and water as solvents, taking MXene as a carrier, selectively adsorbing the MXene on the surface through magnetic cations, heating at 60-120 ℃, and gradually reducing the magnetic cations into magnetic nanoparticles under the common reduction action of hydrazine hydrate and ethylene glycol, wherein the characteristics of the MXene and magnetic metal are combined with the characteristics of the MXene and the magnetic metal.
Description
Technical Field
The invention belongs to the field of preparation of nano magnetic composite materials, and particularly relates to an MXene-magnetic metal composite material and a preparation method thereof.
Background
MXene is a two-dimensional material synthesized by extracting the "a" layer from a lamellar carbide or carbonitride called the MAX phase. MAX phase has the general formula Mn + 1AXn(N =1, 2, 3), wherein M represents a transition metal element, a represents an IIIA or IVA element (e.g., Al, Ga, Si or Ge), and X represents C and/or N. MAX phase is etched into MXeneFunctional groups such as-O, -OH and-F are attached to the surface of MXene, and the presence of these functional groups also provides the possibility for the loading of other nanoparticles. MXene has excellent conductivity, and can be loaded with different particles to modify MXene according to requirements so as to improve the comprehensive performance. Patent CN108091862A discloses an MXene-metal composite material and a preparation method thereof, wherein the MXene-metal composite material is obtained by dispersing metal salt and MAX in HF, stirring, centrifuging and drying. The MXene-metal composite material has the advantages of simple preparation process, good performance when being applied to a lithium battery and high cycle rate.
The transition metal Ni and Co nano particles and the NiCo alloy particles thereof are typical magnetic materials and have wide application in the fields of catalysts, electromagnetic wave-absorbing materials, energy storage, functional coating materials, high-performance electronic materials and the like. However, since the magnetic materials Ni and Co have higher Snoek limit, agglomeration is easily caused to cause poor comprehensive performance of the materials. In combination with the above analysis, loading magnetic particles Ni and/or Co and/or NiCo alloy particles on MXene is a rational choice.
Disclosure of Invention
The invention aims to provide an MXene-magnetic metal composite material and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an MXene-magnetic metal composite material consists of flaky MXene and magnetic metal nanoparticles uniformly loaded on the MXene.
Preferably, the magnetic metal nanoparticles are Ni nanoparticles, Co nanoparticles or NiCo nanoparticles.
Preferably, the MXene is a lamellar structure with a thickness of less than 3nm and a number of layers < 5.
The preparation method comprises the following steps:
(1) dispersing MXene in a mixed solution composed of ethylene glycol and water, uniformly stirring, adding magnetic metal salt, stirring, adding NaOH to adjust the pH value of the system to 8-14, adding hydrazine hydrate, and uniformly stirring;
(2) heating the mixed solution obtained in the step (1) to 60-120 ℃, and preserving heat for 0.2-8 h;
(3) and (3) cooling, separating, washing and drying the solution obtained in the step (2) to obtain the MXene-magnetic metal composite material.
Preferably, in the step (1), the volume ratio of the ethylene glycol to the water is (1-40) to (1-9).
Preferably, in the step (1), the addition amount of the magnetic metal salt ensures that the ratio of the mass of the provided magnetic metal to the mass of MXene is (1-9): (1-30).
Preferably, in the step (1), the magnetic metal salt is one or more of nickel chloride, cobalt chloride, nickel nitrate, cobalt nitrate, nickel sulfate, cobalt sulfate, nickel acetate and cobalt acetate.
Preferably, in the step (1), the ratio of the amounts of hydrazine hydrate and magnetic metal salt is (1-30) to (1-3).
Preferably, in step (1), the MXene is obtained by etching a MAX phase material, and the MAX phase material has a general formula: mn + 1AXnWherein M represents a transition metal element; a represents an IIIA or IVA element, X represents C and/or N, N =1, 2, or 3.
Preferably, the MAX phase material is Ti3AlC2、Ti2AlC、Ti3AlCN or Ti2And MAX phases such as SiC.
The formation principle of MXene-magnetic metal composite material: magnetic metal salt containing magnetic metal cations is uniformly dissolved in MXene dispersion liquid, and the magnetic metal cations are selectively adsorbed on the surface of the negative MXene under the drive of positive and negative electric adsorption; under a proper alkaline environment and temperature, magnetic metal cations are gradually reduced into magnetic metal simple substances by utilizing the reducibility of hydrazine hydrate, and the MXene-magnetic metal composite material is finally formed.
The invention has the beneficial effects that:
1. the method takes ethylene glycol and water as a solvent, MXene as a carrier, the MXene is selectively adsorbed on the surface of the MXene through magnetic cations, the MXene is heated at 60-120 ℃, the magnetic cations are gradually reduced into magnetic nanoparticles under the common reduction action of hydrazine hydrate and ethylene glycol, and the MXene-magnetic metal composite material prepared finally combines the characteristics of the MXene and magnetic metal, has good conductivity and magnetic performance, and can be widely applied to the fields of sensors, supercapacitors, energy storage, catalysts, electromagnetic wave absorption and shielding materials and the like.
2. The method has the advantages of less investment equipment, simple process, lower cost and the like, does not cause secondary pollution to the environment, can control the shape and the size of the magnetic nano-particles, and is suitable for large-scale preparation.
Drawings
FIG. 1: scanning electron micrographs of MXene-magnetic metal composite obtained in example 1.
FIG. 2: XRD patterns of MXene and MXene-magnetic metal composite obtained in example 1.
FIG. 3: electromagnetic wave shielding performance of MXene-magnetic metal composite obtained in example 1.
FIG. 4: scanning electron micrographs of MXene-magnetic metal composite obtained in example 2.
FIG. 5: scanning electron micrographs of MXene-magnetic metal composite obtained in example 4.
FIG. 6: scanning electron micrographs of MXene-magnetic metal composite obtained in example 5.
FIG. 7: scanning electron micrographs of MXene-magnetic metal composite obtained in example 6.
FIG. 8: scanning electron micrographs of MXene-magnetic metal composite obtained in comparative example 1.
FIG. 9: XRD pattern of MXene-magnetic metal composite obtained in comparative example 2.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following examples, but the scope of the present invention is not limited thereto.
Example 1
A preparation method of MXene-magnetic metal composite material comprises the following steps:
(1) 2 g of MAX phase material is put into 40 mL of mixed solution of hydrochloric acid (the mass concentration is 40%) and 2 g of lithium fluoride, etched for 24 h at 35 ℃, washed and dried to obtain MXene;
(2) dispersing 80 mg of MXene prepared in the step (1) in a mixed solution of 100 mL of ethylene glycol and 9 mL of deionized water, uniformly stirring, and adding 1.18 g of nickel chloride hexahydrate (NiCl)2·6H2O) and stirring, then adding NaOH to adjust the pH value of the system to 10, then adding 5 mL of hydrazine hydrate, and uniformly stirring;
(3) heating the mixed solution obtained in the step (2) to 80 ℃ and preserving heat for 1 h;
(4) and (4) cooling the solution obtained in the step (3), separating, washing with deionized water and ethanol for multiple times respectively, and drying to obtain the MXene-magnetic metal composite material (calculated as MXene-Ni).
The scanning electron microscope image of the MXene-magnetic metal composite material prepared in this example is shown in fig. 1. As can be seen from fig. 1: ni particles are uniformly loaded on MXene, and the MXene is in a gauze shape, which shows that the MXene is successfully stripped; the results show that: the MXene-magnetic metal composite material is successfully prepared, and the Ni particle size is about 50-200 nm.
The XRD patterns of MXene and MXene-magnetic metal composite materials prepared in this example are shown in fig. 2. Fig. 2a shows the XRD pattern of MXene, knowing that: the XRD peak of the pure MXene of the product of the invention accords with the reported few-layer or single-layer MXene, reflects that the step (1) carried out by the invention is very successful, and is beneficial to the synthesis of MXene-magnetic metal composite materials. Fig. 2b shows the XRD pattern of MXene-magnetic metal composite, from which it can be found that: the peak of MXene does not change much, and meanwhile, the main diffraction peaks of metal Ni, including (111), (200) and (220) crystal faces and the like, can be found from the graph in FIG. 2 b; in addition, no other miscellaneous peaks appear, which indicates the purity compounding requirement of the product. The XRD results show that: MXene-magnetic metal composites can be easily prepared by the process of the present invention.
The MXene-magnetic metal composite material prepared in this example and paraffin wax were blended at a mass ratio of 3: 2, pressed into a ring shape having an inner diameter of 3.01 mm, an outer diameter of 7 mm and a thickness of 1.4 mm, and the electromagnetic wave shielding performance was measured with a network vector analyzer (VNA, Agilent N5234A), the results of which are shown in FIG. 3. The shielding performance of the MXene-magnetic metal composite material is maintained at 30dB in the frequency range of 2-18 GHz, which shows that the MXene-magnetic metal composite material prepared in the embodiment has excellent electromagnetic wave shielding performance.
Example 2
A preparation method of MXene-magnetic metal composite material comprises the following steps:
(1) putting 1 g of MAX phase material into a mixed solution of 20 mL of hydrochloric acid (the mass concentration is 40%) and 1 g of lithium fluoride, etching for 25 h at 35 ℃, washing and drying to obtain MXene;
(2) dispersing 50 mg of MXene prepared in the step (1) in a mixed solution of 48 mL of ethylene glycol and 6 mL of deionized water, uniformly stirring, and adding 0.59 g of nickel chloride hexahydrate (NiCl)2·6H2O) and stirring, then adding NaOH to adjust the pH value of the system to 11, then adding 2.5 mL of hydrazine hydrate, and stirring uniformly;
(3) heating the mixed solution obtained in the step (2) to 78 ℃ and preserving heat for 1 h;
(4) and (4) cooling the solution obtained in the step (3), separating, washing with deionized water and ethanol for multiple times respectively, and drying to obtain the MXene-magnetic metal composite material (calculated as MXene-Ni).
The scanning electron microscope image of the MXene-magnetic metal composite material prepared in this example is shown in fig. 4, and the result shows: magnetic metal Ni nanoparticles (diameter 100-300 nm) uniformly float on the MXene surface, and the SEM result proves the successful preparation of the MXene-magnetic metal composite material.
Example 3
A preparation method of MXene-magnetic metal composite material comprises the following steps:
(1) putting 1 g of MAX phase material into a mixed solution of 20 mL of hydrochloric acid (the mass concentration is 40%) and 1 g of lithium fluoride, etching for 25 h at 35 ℃, washing and drying to obtain MXene;
(2) dispersing 100 mg of MXene prepared in step (1) in a mixed solution of 51 mL of ethylene glycol and 5 mL of water, uniformly stirring, and adding 0.5 g of nickel nitrate hexahydrate(Ni(NO3)2·6H2O) and stirring, then adding NaOH to adjust the pH value of the system to 10, then adding 2 mL of hydrazine hydrate, and stirring uniformly;
(3) heating the mixed solution obtained in the step (2) to 78 ℃ and preserving heat for 1 h;
(4) and (4) cooling the solution obtained in the step (3), separating, washing with deionized water and ethanol for multiple times respectively, and drying to obtain the MXene-magnetic metal composite material (calculated as MXene-Ni).
Example 4
A preparation method of MXene-magnetic metal composite material comprises the following steps:
(1) 2 g of MAX phase material is put into 40 mL of mixed solution of hydrochloric acid (the mass concentration is 40%) and 2 g of lithium fluoride, etched for 24 h at 35 ℃, washed and dried to obtain MXene;
(2) MXene 80 mg prepared in step (1) was dispersed in a mixture of 100 mL of ethylene glycol and 9 mL of deionized water, and 1.18 g of cobalt chloride hexahydrate (CoCl) was added thereto2·6H2O) and stirring, then adding NaOH to adjust the pH value of the system to 10, then adding 5 mL of hydrazine hydrate, and uniformly stirring;
(3) heating the mixed solution obtained in the step (2) to 80 ℃ and preserving heat for 1 h;
(4) and (4) cooling the solution obtained in the step (3), separating, washing with deionized water and ethanol for multiple times respectively, and drying to obtain the MXene-magnetic metal composite material (calculated as MXene-Co).
The scanning electron microscope image of the MXene-magnetic metal composite material prepared in this example is shown in fig. 5, which reveals that Co nanoparticles are uniformly distributed on the surface of MXene, indicating that the MXene-Co composite material can be successfully prepared by the method of the present invention.
Example 5
A preparation method of MXene-magnetic metal composite material comprises the following steps:
(1) 2 g of MAX phase material is put into 40 mL of mixed solution of hydrochloric acid (the mass concentration is 40%) and 2 g of lithium fluoride, etched for 24 h at 35 ℃, washed and dried to obtain MXene;
（2）dispersing 80 mg of MXene prepared in step (1) in a mixed solution of 100 mL of ethylene glycol and 9 mL of deionized water, uniformly stirring, and adding 0.6g of cobalt chloride hexahydrate (CoCl)2·6H2O) and 0.6g of nickel chloride hexahydrate (NiCl)2·6H2O) and stirring, then adding NaOH to adjust the pH value of the system to 10, then adding 5 mL of hydrazine hydrate, and uniformly stirring;
(3) heating the mixed solution obtained in the step (2) to 80 ℃ and preserving heat for 1 h;
(4) and (4) cooling and separating the solution obtained in the step (3), washing with deionized water and ethanol for multiple times, and drying to obtain the MXene-magnetic metal composite material (calculated as MXene-NiCo).
The scanning electron microscope image of the MXene-magnetic metal composite material prepared in this example is shown in fig. 6, which reveals that NiCo nanoparticles are uniformly distributed on the surface of MXene, and thus the MXene-Co composite material can be successfully prepared by the method of the present invention.
Example 6
A preparation method of MXene-magnetic metal composite material comprises the following steps:
(1) 2 g of MAX phase material is put into 40 mL of mixed solution of hydrochloric acid (the mass concentration is 40%) and 2 g of lithium fluoride, etched for 24 h at 35 ℃, washed and dried to obtain MXene;
(2) dispersing 80 mg of MXene prepared in the step (1) in a mixed solution of 100 mL of ethylene glycol and 9 mL of deionized water, uniformly stirring, and adding 1 g of nickel chloride hexahydrate (NiCl)2·6H2O) and stirring, then adding NaOH to adjust the pH value of the system to 10, then adding 5 mL of hydrazine hydrate, and uniformly stirring;
(3) heating the mixed solution obtained in the step (2) to 80 ℃ and preserving heat for 1 h;
(4) and (4) cooling the solution obtained in the step (3), separating, washing with deionized water and ethanol for multiple times, and drying to obtain the MXene-magnetic metal composite material (calculated as MXene-Ni).
The scanning electron microscope image of the MXene-magnetic metal composite material prepared in this example is shown in fig. 7, and the MXene-magnetic metal composite material was also successfully prepared.
Example 7
A preparation method of MXene-magnetic metal composite material comprises the following steps:
(1) putting 1 g of MAX phase material into a mixed solution of 20 mL of hydrochloric acid (the mass concentration is 40%) and 1 g of lithium fluoride, etching for 24 h at 35 ℃, washing and drying to obtain MXene;
(2) dispersing 50 mg of MXene prepared in step (1) in a mixed solution of 48 mL of ethylene glycol and 6 mL of deionized water, uniformly stirring, and adding 0.3g of cobalt chloride hexahydrate (CoCl)2·6H2O) and 0.3g of nickel chloride hexahydrate (NiCl)2·6H2O) and stirring, then adding NaOH to adjust the pH value of the system to 12, then adding 2.5 mL of hydrazine hydrate, and stirring uniformly;
(3) heating the mixed solution obtained in the step (2) to 78 ℃ and preserving heat for 1 h;
(4) and (4) cooling and separating the solution obtained in the step (3), washing with deionized water and ethanol for multiple times, and drying to obtain the MXene-magnetic metal composite material (calculated as MXene-NiCo).
The invention utilizes the magnetic metal nano particles to modify MXene so as to improve the comprehensive performance of the MXene-magnetic metal composite material and expand the application range of the composite material. The key point of the technology is that the magnetic metal nanoparticles have uniform particle size, can be uniformly loaded on MXene, and can still ensure that MXene is not oxidized even under the action of high temperature due to the protection effect of hydrazine hydrate in the solution. However, MXene is difficult to load on magnetic metal nanoparticles, and the inventor creates the invention through continuous efforts, and finally obtains the key technology of the invention. Of course, such prepared examples are also numerous, according to the scope of adaptation of the invention.
Comparative example 1
The difference from example 1 is that: in the step (2), the using amount of the deionized water is 0 mL, namely the deionized water is not added; otherwise, the same procedure as in example 1 was repeated.
The scanning electron microscope image of the MXene-magnetic metal composite material prepared in the comparative example is shown in fig. 8, and the result shows: the Ni fiber coexisted with MXene, which was not successfully loaded with magnetic Ni nanoparticles uniformly. Ni fibers are abundant, and MXene also has an agglomeration phenomenon, so that the uniform loading of magnetic Ni nano particles on the MXene is not facilitated. By comparing example 1 with comparative example 1, it can be concluded that: the preparation scheme of the invention provides a good technology for uniformly loading MXene on the magnetic Ni nano particles, is simple to operate and low in cost, and is an invention with a good application prospect.
Comparative example 2
The difference from example 1 is that: in the step (2), the dosage of the glycol is 0 mL, namely the glycol is not added; otherwise, the same procedure as in example 1 was repeated.
MXene-magnetic Metal composite Material (calculated as MXene-Ni @ Ni (OH)) prepared in this comparative example2) The XRD pattern of fig. 9 shows that: the product contains Ni (OH)2Does not favor the reduction of Ni ions, but forms Ni (OH)2The precipitate is loaded on MXene, and uniform magnetic Ni nano-particles cannot be formed and loaded on MXene uniformly. By comparing example 1 with comparative example 2, it can be concluded that: under certain alkaline conditions, the existence of ethylene glycol needs to be provided, and the mixture of the ethylene glycol and deionized water needs to be mixed and dissolved, so that Ni ions can be completely converted into magnetic Ni nano particles.
Claims (9)
1. The preparation method of the MXene-magnetic metal composite material is characterized in that the MXene-magnetic metal composite material consists of flaky MXene and magnetic metal nanoparticles uniformly loaded on the MXene, wherein the magnetic metal nanoparticles are Ni nanoparticles, Co nanoparticles or NiCo nanoparticles; the preparation method of the MXene-magnetic metal composite material comprises the following steps:
(1) dispersing MXene in a mixed solution composed of ethylene glycol and water, uniformly stirring, adding magnetic metal salt, stirring, adding NaOH to adjust the pH value of the system to 8-14, adding hydrazine hydrate, and uniformly stirring;
(2) heating the mixed solution obtained in the step (1) to 60-120 ℃, and preserving heat for 0.2-8 h;
(3) and (3) cooling, separating, washing and drying the solution obtained in the step (2) to obtain the MXene-magnetic metal composite material.
2. The method of preparing the MXene-magnetic metal composite of claim 1, wherein: in the step (1), the volume ratio of the ethylene glycol to the water is (1-40) to (1-9).
3. The method of preparing the MXene-magnetic metal composite of claim 1, wherein: in the step (1), the addition amount of the magnetic metal salt ensures that the ratio of the mass of the provided magnetic metal to the mass of MXene is (1-9): (1-30).
4. The method of preparing the MXene-magnetic metal composite of claim 1, wherein: in the step (1), the magnetic metal salt is one or more of nickel chloride, cobalt chloride, nickel nitrate, cobalt nitrate, nickel sulfate, cobalt sulfate, nickel acetate and cobalt acetate.
5. The method of preparing the MXene-magnetic metal composite of claim 1, wherein: in the step (1), the ratio of the hydrazine hydrate to the magnetic metal salt is (1-30) to (1-3).
6. The method of preparing the MXene-magnetic metal composite of claim 1, wherein: in the step (1), the MXene is obtained by etching a MAX phase material, and the general formula of the MAX phase material is as follows: mn + 1AXnWherein M represents a transition metal element; a represents an IIIA or IVA element, X represents C and/or N, N =1, 2, or 3.
7. The method of preparing the MXene-magnetic metal composite of claim 6, wherein: MAX phase material is Ti3AlC2、Ti2AlC、Ti3AlCN or Ti2SiC。
8. An MXene-magnetic metal composite prepared by the preparation method according to any one of claims 1 to 7, characterized in that: the MXene-magnetic metal composite material consists of flaky MXene and magnetic metal nanoparticles uniformly loaded on the MXene, wherein the magnetic metal nanoparticles are Ni nanoparticles, Co nanoparticles or NiCo nanoparticles.
9. The MXene-magnetic metal composite of claim 8, wherein: the MXene is a lamellar structure with the thickness within 3nm and the number of layers less than 5.
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| CN110283570B (en) * | 2019-07-17 | 2022-03-25 | 湖南工程学院 | FeCo @ MXene core-shell structure composite wave-absorbing material and preparation method thereof |
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| CN112961723B (en) * | 2021-02-26 | 2022-07-01 | 陕西科技大学 | MXene @ COFs/liquid metal-based lubricating additive, and preparation method, application and composite material thereof |
| CN113380945B (en) * | 2021-05-21 | 2022-10-14 | 电子科技大学 | Magnetic heterostructure based on electric field regulation and control and preparation method thereof |
| CN113316379B (en) * | 2021-05-26 | 2022-09-02 | 湖南工程学院 | Nano composite structure wave absorber material, preparation method and application |
| CN113429820B (en) * | 2021-06-25 | 2022-04-26 | 西安热工研究院有限公司 | Oriented Mxene/Co conductive filler for anti-corrosion coating and preparation method thereof |
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| CN113462367B (en) * | 2021-07-23 | 2023-03-21 | 苏州双碳新材料有限公司 | Optical energy and magnetic energy dual-drive composite phase change material |
| CN114478148B (en) * | 2022-01-10 | 2022-07-19 | 北京理工大学 | Blasting multi-mechanism coupling type energetic electromagnetic damage cloud cluster and preparation method and application thereof |
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