CN109712769A - A kind of MXene- magnetic metal composite material and preparation method thereof - Google Patents
A kind of MXene- magnetic metal composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to nano magnetic composite materials preparation field, a kind of MXene- magnetic metal composite material and preparation method thereof is disclosed.It is made of the magnetic metal nano particle of sheet MXene and uniform load on MXene.MXene is dispersed in the mixed liquor being made of ethylene glycol and water and is stirred evenly, magnetic metal salt is then added and is stirred, NaOH regulation system pH value is subsequently added into 8 ~ 14, hydrazine hydrate is then added, stirs evenly；It is heated to 60 ~ 120 DEG C and keeps the temperature 0.2 ~ 8 h；Cooling, separation, washing, drying are to get MXene- magnetic metal composite material.The present invention is using ethylene glycol and water as solvent, using MXene as carrier, by magnetic cation selective absorption on the surface MXene, it is heated in 60 ~ 120 DEG C, under the common reduction of hydrazine hydrate and ethylene glycol, magnetic cation is gradually reduced into magnetic nanoparticle, and finally prepd MXene- magnetic metal composite material combines the characteristic of MXene and magnetic metal.
Description
Technical field
The invention belongs to nano magnetic composite materials preparation fields, and in particular to a kind of MXene- magnetic metal composite material
And preparation method thereof.
Background technique
MXene is the two-dimentional material synthesized and extracting " A " layer in the stratiform carbide or carbonitride from referred to as MAX phase
Material.MAX phase has formula M n + 1AXn (n=1,2,3), wherein M represents transition metal element, and A represents IIIA or IVA member
Plain (such as Al, Ga, Si or Ge), X represent C and/or N.MAX phase during being etched into MXene, such as-O ,-OH and-
The functional group of F is attached on the surface of MXene, and also provide for the load of other nano particles can for the presence of these functional groups
Energy.MXene has excellent electric conductivity, usually can according to need, and loads different particles and carries out the modification of MXene to improve
Comprehensive performance.Patent CN108091862A discloses a kind of MXene- metallic composite and preparation method thereof, by by metal
Salt and MAX, which are dispersed in HF, stirs, is centrifuged and is dried to obtain MXene- metallic composite.The system of MXene- metallic composite
Standby simple process, the performance applied to lithium battery is good, and cycling rate is high.
Transition metal Ni, Co nano particle and its NiCo alloying pellet are typical magnetic materials, in catalyst, electromagnetism
The fields such as absorbing material, energy storage, functional coating material and high-performance electronic material tool has a wide range of applications.But due to magnetism
Material Ni, Co the Snoek limit with higher easily cause reunion and cause the comprehensive performance of material bad.It is analyzed in conjunction with above,
Magnetic particle Ni and/or Co and/or NiCo alloying pellet is supported on MXene be a rationality selection.
Summary of the invention
The purpose of the present invention is intended to provide a kind of MXene- magnetic metal composite material and preparation method thereof.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of MXene- magnetic metal composite material, by the magnetic metal nanometer of sheet MXene and uniform load on MXene
Grain composition.
Preferably, magnetic metal nano particle is Ni nano particle, Co nano particle or NiCo nano particle.
Preferably, the MXene is thickness within 3 nm and the lamellar structure of the number of plies < 5 layer.
Preparation method includes the following steps:
(1) MXene is dispersed in the mixed liquor being made of ethylene glycol and water and is stirred evenly, magnetic metal salt is then added and stirred
It mixes, is subsequently added into NaOH regulation system pH value to 8 ~ 14, hydrazine hydrate is then added, stirs evenly；
(2) mixed solution obtained by step (1) is heated to 60 ~ 120 DEG C and keeps the temperature 0.2 ~ 8 h；
(3) step (2) acquired solution is cooling, separation, washing, drying are to get MXene- magnetic metal composite material.
Preferably, in step (1), the volume ratio of ethylene glycol and water is (1 ~ 40): (1 ~ 9).
Preferably, in step (1), the additive amount of magnetic metal salt guarantee the quality of its provided magnetic metal with
Ratio between the quality of MXene is (1 ~ 9): (1 ~ 30).
Preferably, in step (1), the magnetic metal salt be nickel chloride, cobalt chloride, nickel nitrate, cobalt nitrate, nickel sulfate,
One or more of cobaltous sulfate, nickel acetate, cobalt acetate.
Preferably, in step (1), the ratio between amount of substance of hydrazine hydrate and magnetic metal salt is (1 ~ 30): (1 ~ 3).
Preferably, in step (1), the MXene is by the etched acquisition of MAX phase material, the general formula of MAX phase material are as follows:
Mn + 1AXn, wherein M represents transition metal element；A represents IIIA or IVA element, and X represents C and/or N, n=1,2 or 3.
Preferably, MAX phase material is Ti3AlC2、Ti2AlC、Ti3AlCN or Ti2The MAX phase such as SiC.
The formation basic theory of MXene- magnetic metal composite material: the magnetic metal salt of the cation containing magnetic metal is equably molten
Solution under the effect driving of positive and negative Electro Sorb, is adsorbed on elecrtonegativity to magnetic metal cation selective in MXene dispersion liquid
The surface MXene；Suitable alkaline environment and at a temperature of in, using the reproducibility of hydrazine hydrate, gradually by magnetic metal cation
It is reduced into magnetic metal simple substance, ultimately forms MXene- magnetic metal composite material, the weaker reduction of ethylene glycol during being somebody's turn to do
Property can with hydrazine hydrate formed collaborative SCM effect, facilitate the complete reduction of magnetic cation.
Beneficial effects of the present invention:
1, the present invention, using MXene as carrier, is existed using ethylene glycol and water as solvent by magnetic cation selective absorption
The surface MXene is heated in 60 ~ 120 DEG C, under the common reduction of hydrazine hydrate and ethylene glycol, magnetic cation gradually by
It is reduced into magnetic nanoparticle, finally prepd MXene- magnetic metal composite material combines the spy of MXene and magnetic metal
Property, satisfactory electrical conductivity and magnetic property are had both, can be widely applied to sensor, supercapacitor, energy storage, catalyst, electromagnetism
Wave absorbs and the fields such as shielding material.
2, the present invention has many advantages, such as that few investment goods, simple process, cost is relatively low, and will not cause to environment secondary
Pollution can carry out morphology and size control to magnetic nanoparticle, be suitable for being prepared on a large scale.
Detailed description of the invention
Fig. 1: the scanning electron microscope (SEM) photograph of 1 gained MXene- magnetic metal composite material of embodiment.
Fig. 2: the XRD diagram of 1 gained MXene and MXene- magnetic metal composite material of embodiment.
Fig. 3: the electromagnetic wave shielding performance figure of 1 gained MXene- magnetic metal composite material of embodiment.
Fig. 4: the scanning electron microscope (SEM) photograph of 2 gained MXene- magnetic metal composite material of embodiment.
Fig. 5: the scanning electron microscope (SEM) photograph of 4 gained MXene- magnetic metal composite material of embodiment.
Fig. 6: the scanning electron microscope (SEM) photograph of 5 gained MXene- magnetic metal composite material of embodiment.
Fig. 7: the scanning electron microscope (SEM) photograph of 6 gained MXene- magnetic metal composite material of embodiment.
Fig. 8: the scanning electron microscope (SEM) photograph of 1 gained MXene- magnetic metal composite material of reference examples.
Fig. 9: the XRD diagram of 2 gained MXene- magnetic metal composite material of reference examples.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of preparation method of MXene- magnetic metal composite material, steps are as follows:
(1) 2 g MAX phase materials are placed in 40 mL hydrochloric acid (mass concentration 40%) and 2 g lithium fluoride mixed liquors, at 35 DEG C
Etch 24 h, washing, dry, obtained MXene；
(2) 80 mg of MXene prepared by step (1) is dispersed in the mixed liquor of 9 mL of 100 mL of ethylene glycol and deionized water and is stirred
It mixes uniformly, 1.18 g Nickel dichloride hexahydrate (NiCl is added2·6H2O it) and stirs, being subsequently added into NaOH regulation system pH value is 10,
5 mL hydrazine hydrates are then added, stir evenly；
(3) mixed solution obtained by step (2) is heated to 80 DEG C and keeps the temperature 1 h；
(4) the resulting solution of step (3) is cooling, separation, deionized water washing and ethanol washing are multiple respectively, it is dry to get
MXene- magnetic metal composite material (is calculated as MXene-Ni).
The scanning electron microscope (SEM) photograph of MXene- magnetic metal composite material manufactured in the present embodiment is as shown in Figure 1.As shown in Figure 1:
Ni particle is equably supported on MXene, and MXene is in gauze-like, and it is very successful to illustrate that MXene is stripped；As the result is shown: institute
It obtains MXene- magnetic metal composite material successfully to be prepared, Ni granular size is about between 50 ~ 200 nm.
The XRD diagram of MXene and MXene- magnetic metal composite material manufactured in the present embodiment is as shown in Figure 2.Fig. 2 a is shown
Be MXene XRD diagram, it is known that: the peak XRD of the pure MXene of product of the present invention meets the MXene of reported few layer or single layer,
It is very successful to reflect the step of present invention is carried out (1), facilitates the synthesis of MXene- magnetic metal composite material.Fig. 2 b is shown
Be MXene- magnetic metal composite material XRD diagram, from figure it can be found that: the peak of MXene is there is no too big variation, together
When, it has also been found that the main diffraction peak, including (111), (200) and (220) crystal face etc. of W metal from Fig. 2 b；In addition, nothing
The appearance of other miscellaneous peaks illustrates the degree of purity composite demand of product.XRD the result shows that: MXene- magnetic metal composite material warp
The method of the present invention can easily be prepared.
MXene- magnetic metal composite material manufactured in the present embodiment and paraffin in mass ratio 3: 2 are blended, internal diameter is pressed into
It is 7 mm for 3.01 mm, outer diameter, the ring-type of 1.4 mm of thickness, with network vector analyzer (VNA, Agilent N5234A)
Its electromagnetic wave shielding performance is tested, as a result as shown in Figure 3.In 2-18 gigahertz frequency range, shielding properties maintains 30
DB illustrates that the electromagnetic wave shielding performance of MXene- magnetic metal composite material manufactured in the present embodiment is excellent.
Embodiment 2
A kind of preparation method of MXene- magnetic metal composite material, steps are as follows:
(1) 1 g MAX phase material is placed in 20 mL hydrochloric acid (mass concentration 40%) and 1 g lithium fluoride mixed liquor, at 35 DEG C
Etch 25 h, washing, dry, obtained MXene；
(2) 50 mg of MXene prepared by step (1) is dispersed in the mixed liquor of 6 mL of 48 mL of ethylene glycol and deionized water and is stirred
It mixes uniformly, 0.59 g Nickel dichloride hexahydrate (NiCl is added2·6H2O it) and stirs, being subsequently added into NaOH regulation system pH value is 11,
2.5 mL hydrazine hydrates are then added, stir evenly；
(3) mixed solution obtained by step (2) is heated to 78 DEG C and keeps the temperature 1 h；
(4) the resulting solution of step (3) is cooling, separation, deionized water washing and ethanol washing are multiple respectively, it is dry to get
MXene- magnetic metal composite material (is calculated as MXene-Ni).
The scanning electron microscope (SEM) photograph of MXene- magnetic metal composite material manufactured in the present embodiment is as shown in figure 4, as the result is shown: magnetic
Property W metal nano particle (diameter 100-300 nm) equably float on the surface MXene, SEM result confirms MXene- magnetic metal
The successful preparation of composite material.
Embodiment 3
A kind of preparation method of MXene- magnetic metal composite material, steps are as follows:
(1) 1 g MAX phase material is placed in 20 mL hydrochloric acid (mass concentration 40%) and 1 g lithium fluoride mixed liquor, at 35 DEG C
Etch 25 h, washing, dry, obtained MXene；
(2) 100 mg of MXene prepared by step (1) is dispersed in the mixed liquor of 5 mL of 51 mL of ethylene glycol and water and is stirred
It is even, 0.5 g Nickelous nitrate hexahydrate (Ni (NO is added3)2·6H2O it) and stirs, being subsequently added into NaOH regulation system pH value is 10, with
After 2 mL hydrazine hydrates are added, stir evenly；
(3) mixed solution obtained by step (2) is heated to 78 DEG C and keeps the temperature 1 h；
(4) the resulting solution of step (3) is cooling, separation, deionized water washing and ethanol washing are multiple respectively, it is dry to get
MXene- magnetic metal composite material (is calculated as MXene-Ni).
Embodiment 4
A kind of preparation method of MXene- magnetic metal composite material, steps are as follows:
(1) 2 g MAX phase materials are placed in 40 mL hydrochloric acid (mass concentration 40%) and 2 g lithium fluoride mixed liquors, at 35 DEG C
Etch 24 h, washing, dry, obtained MXene；
(2) 80 mg of MXene prepared by step (1) is dispersed in the mixed liquor of 9 mL of 100 mL of ethylene glycol and deionized water and is stirred
It mixes uniformly, 1.18 g cobalt chloride hexahydrate (CoCl is added2·6H2O it) and stirs, being subsequently added into NaOH regulation system pH value is 10,
5 mL hydrazine hydrates are then added, stir evenly；
(3) mixed solution obtained by step (2) is heated to 80 DEG C and keeps the temperature 1 h；
(4) the resulting solution of step (3) is cooling, separation, deionized water washing and ethanol washing are multiple respectively, it is dry to get
MXene- magnetic metal composite material (is calculated as MXene-Co).
The scanning electron microscope (SEM) photograph of MXene- magnetic metal composite material manufactured in the present embodiment is as shown in figure 5, disclose Co in figure
Nanoparticle is uniformly distributed in the surface MXene, illustrates that MXene-Co composite material can successfully be prepared using the method for the present invention.
Embodiment 5
A kind of preparation method of MXene- magnetic metal composite material, steps are as follows:
(1) 2 g MAX phase materials are placed in 40 mL hydrochloric acid (mass concentration 40%) and 2 g lithium fluoride mixed liquors, at 35 DEG C
Etch 24 h, washing, dry, obtained MXene；
(2) 80 mg of MXene prepared by step (1) is dispersed in the mixed liquor of 9 mL of 100 mL of ethylene glycol and deionized water and is stirred
It mixes uniformly, 0.6 g cobalt chloride hexahydrate (CoCl is added2·6H2) and 0.6g Nickel dichloride hexahydrate (NiCl O2·6H2O it) and stirs
It mixes, being subsequently added into NaOH regulation system pH value is 10, and 5 mL hydrazine hydrates are then added, stir evenly；
(3) mixed solution obtained by step (2) is heated to 80 DEG C and keeps the temperature 1 h；
(4) the resulting solution of step (3) is cooling, separation, carries out deionized water washing and ethanol washing is multiple, it is dry to get
MXene- magnetic metal composite material (is calculated as MXene-NiCo).
The scanning electron microscope (SEM) photograph of MXene- magnetic metal composite material manufactured in the present embodiment in figure as shown in fig. 6, disclose
NiCo nanoparticle is uniformly distributed in the surface MXene, illustrates that MXene-Co composite material can successfully be made using the method for the present invention
It is standby.
Embodiment 6
A kind of preparation method of MXene- magnetic metal composite material, steps are as follows:
(1) 2 g MAX phase materials are placed in 40 mL hydrochloric acid (mass concentration 40%) and 2 g lithium fluoride mixed liquors, at 35 DEG C
Etch 24 h, washing, dry, obtained MXene；
(2) 80 mg of MXene prepared by step (1) is dispersed in the mixed liquor of 9 mL of 100 mL of ethylene glycol and deionized water and is stirred
It mixes uniformly, 1 g Nickel dichloride hexahydrate (NiCl is added2·6H2O it) and stirs, being subsequently added into NaOH regulation system pH value is 10, with
After 5 mL hydrazine hydrates are added, stir evenly；
(3) mixed solution obtained by step (2) is heated to 80 DEG C and keeps the temperature 1 h；
(4) the resulting solution of step (3) is cooling, separation, carries out deionized water washing and ethanol washing is multiple, it is dry to get
MXene- magnetic metal composite material (is calculated as MXene-Ni).
The scanning electron microscope (SEM) photograph of MXene- magnetic metal composite material manufactured in the present embodiment is as shown in fig. 7, MXene- is magnetic
Metallic composite is also successfully prepared.
Embodiment 7
A kind of preparation method of MXene- magnetic metal composite material, steps are as follows:
(1) 1 g MAX phase material is placed in 20 mL hydrochloric acid (mass concentration 40%) and 1 g lithium fluoride mixed liquor, at 35 DEG C
Etch 24 h, washing, dry, obtained MXene；
(2) 50 mg of MXene prepared by step (1) is dispersed in the mixed liquor of 6 mL of 48 mL of ethylene glycol and deionized water and is stirred
It mixes uniformly, 0.3 g cobalt chloride hexahydrate (CoCl is added2·6H2) and 0.3g Nickel dichloride hexahydrate (NiCl O2·6H2O it) and stirs
It mixes, being subsequently added into NaOH regulation system pH value is 12, and 2.5 mL hydrazine hydrates are then added, stir evenly；
(3) mixed solution obtained by step (2) is heated to 78 DEG C and keeps the temperature 1 h；
(4) the resulting solution of step (3) is cooling, separation carries out deionized water washing and ethanol washing is multiple, it is dry to get
MXene- magnetic metal composite material (is calculated as MXene-NiCo).
The present invention is to be modified using magnetic metal nano particle to MXene, compound to improve MXene- magnetic metal
The comprehensive performance of material expands the application range of composite material.The key of technology is that the partial size of magnetic metal nano particle is equal
It is even, magnetic metal nano particle can uniform load on MXene, furthermore MXene due to there is the protection of hydrazine hydrate in the solution
Effect, even if still ensuring that its is not oxidized under high temperature action.It however is ten for magnetic metal nano particle load MXene
Divide difficulty, inventor has finally just obtained key technology of the invention by unremitting effort, creativity and innovation.Certainly, according to
Adaptation range of the invention, the example of this preparation are also too numerous to enumerate.
Reference examples 1
The difference from embodiment 1 is that: in step (2), the dosage of deionized water is 0 mL, i.e., does not add deionized water；It is other
With embodiment 1.
The scanning electron microscope (SEM) photograph of the MXene- magnetic metal composite material of this reference examples preparation is as shown in figure 8, as the result is shown: Ni
Fiber coexists with MXene, and MXene is upper, and there is no by successful equably carried magnetic Ni nano particle.Ni fiber is in the majority, MXene
Also there is agglomeration, be unfavorable for magnetic Ni nano particle uniform load on MXene.Pass through 1 phase of embodiment 1 and reference examples
Comparison, it can be deduced that conclusion: preparation method of the invention equably loads MXene for magnetism Ni nano particle and provides well
Technology, it is easy to operate at low cost, it is a kind of very with the invention of application prospect.
Reference examples 2
The difference from embodiment 1 is that: in step (2), the dosage of ethylene glycol is 0 mL, i.e., does not add ethylene glycol；It is other same
Embodiment 1.
The MXene- magnetic metal composite material of this reference examples preparation (is calculated as MXene-Ni@Ni (OH)2) XRD diagram such as
Shown in Fig. 9, as the result is shown: having Ni (OH) in product2Presence, be unfavorable for the reduction of Ni ion, but form Ni (OH)2Precipitating
It is supported on MXene, uniform magnetism Ni nano particle uniform load can not be formed on MXene.By embodiment 1 and right
2 compare as usual, it can be deduced that conclusion: under certain alkaline condition, it is desirable to provide the presence of ethylene glycol and deionized water into
Row is miscible, and Ni ion could be fully converted to magnetic Ni nano particle.
Claims (10)
1. a kind of MXene- magnetic metal composite material, it is characterised in that: MXene- magnetic metal composite material is by sheet MXene
With magnetic metal nano particle composition of the uniform load on MXene.
2. MXene- magnetic metal composite material as described in claim 1, it is characterised in that: magnetic metal nano particle is Ni
Nano particle, Co nano particle or NiCo nano particle.
3. MXene- magnetic metal composite material as described in claim 1, it is characterised in that: the MXene is thickness 3
The lamellar structure of within the nm and number of plies < 5 layer.
4. a kind of preparation method of the MXene- magnetic metal composite material as described in claim 1 ~ 3 is any, which is characterized in that
Include the following steps:
(1) MXene is dispersed in the mixed liquor being made of ethylene glycol and water and is stirred evenly, magnetic metal salt is then added and stirred
It mixes, is subsequently added into NaOH regulation system pH value to 8 ~ 14, hydrazine hydrate is then added, stirs evenly；
(2) mixed solution obtained by step (1) is heated to 60 ~ 120 DEG C and keeps the temperature 0.2 ~ 8 h；
(3) step (2) acquired solution is cooling, separation, washing, drying are to get MXene- magnetic metal composite material.
5. the preparation method of MXene- magnetic metal composite material as claimed in claim 4, it is characterised in that: in step (1),
The volume ratio of ethylene glycol and water is (1 ~ 40): (1 ~ 9).
6. the preparation method of MXene- magnetic metal composite material as claimed in claim 4, it is characterised in that: in step (1),
The additive amount of magnetic metal salt guarantees that the ratio between the quality of its provided magnetic metal and the quality of MXene is (1 ~ 9):
(1 ~ 30).
7. the preparation method of MXene- magnetic metal composite material as claimed in claim 4, it is characterised in that: in step (1),
The magnetic metal salt is nickel chloride, cobalt chloride, nickel nitrate, cobalt nitrate, nickel sulfate, cobaltous sulfate, nickel acetate, one in cobalt acetate
Kind is several.
8. the preparation method of MXene- magnetic metal composite material as claimed in claim 4, it is characterised in that: in step (1),
The ratio between amount of substance of hydrazine hydrate and magnetic metal salt is (1 ~ 30): (1 ~ 3).
9. the preparation method of MXene- magnetic metal composite material as claimed in claim 4, it is characterised in that: in step (1),
The MXene is by the etched acquisition of MAX phase material, the general formula of MAX phase material are as follows: Mn + 1AXn, wherein M represents transition metal member
Element；A represents IIIA or IVA element, and X represents C and/or N, n=1,2 or 3.
10. the preparation method of MXene- magnetic metal composite material as claimed in claim 9, it is characterised in that: MAX phase material
For Ti3AlC2、Ti2AlC、Ti3AlCN or Ti2The MAX phase such as SiC.
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