CN112062155A - Ultra-thin two-dimensional material with limited growth and preparation method thereof - Google Patents
Ultra-thin two-dimensional material with limited growth and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of two-dimensional material preparation, and particularly relates to an ultrathin two-dimensional material with limited growth and a preparation method thereof. The method comprises the steps of uniformly dispersing a small-dose reactant A on the surface of another large-dose reactant crystal powder B to obtain a mixture; and then reacting the uniformly dispersed mixture by adopting a hydrothermal method to form a two-dimensional material with an ultrathin structure, namely the ultrathin two-dimensional material with limited growth. Compared with the prior similar technology for preparing two-dimensional materials by salt assistance, the method can be used for preparing ultrathin two-dimensional materials as long as the method meets the two points that A can be uniformly dispersed on the surface of B crystal grains and the B crystal grains are small enough to provide limited-area growth, and can be used for synthesizing different types of ultrathin two-dimensional materials by adjusting the types of A and B according to requirements. In addition, the thickness of the 2D material can be controlled by adjusting the ratio of a to B. The method is not available in other salt-assisted two-dimensional material preparation methods, and has wide applicability.
Description
Technical Field
The invention belongs to the technical field of two-dimensional material preparation, and particularly relates to an ultrathin two-dimensional material with limited growth and a preparation method thereof.
Background
Ultra-thin two-dimensional (2D) materials have been a hot area of material research since the 2004 successful separation of graphene by the geom group, resulting from its excellent optical, electrical, magnetic and structural properties. Its lateral dimensions are greater than 100nm or up to several microns or even more, but the thickness is only a single or a few atomic layers thick (typically less than 5 nm). The ultrathin thickness greatly increases the specific surface area and promotes the atom utilization rate, the ultrahigh specific surface area has huge application prospects in the aspects of catalysis, capacitors and the like, and the high utilization rate of surface atoms enables the material to be easier to optimize the properties and functions of the material in the modes of surface modification, doping and the like; secondly, the carrier migration and the heat diffusion of the ultrathin two-dimensional plane material are limited in the two-dimensional plane, so that the ultrathin two-dimensional plane material has unique electronic characteristics.
The synthesis process of two-dimensional materials can be divided into two types, namely top-down and bottom-up methods. Generally, lift-off is the most common top-down method to produce single or few layer 2D materials. Exfoliation can attenuate the interlayer van der waals forces of bulk materials having a layered crystal structure while maintaining covalent bonds in-plane to produce a monolayer or few layers of nanoplatelets. However, the top-down peeling method is not suitable for non-layered crystal materials and has limitations; the bottom-up approach is another efficient 2D material synthesis route. Unlike the lift-off process, the precursors used in the bottom-up process do not require a layered structure. Chemical Vapor Deposition (CVD) and wet chemical methods are typical bottom-up methods. CVD can be successfully carried out under gaseous atmosphere conditions on single crystal substrates (usually SiO)2Si, sapphire, mica and SrTiO3) A high quality single layer 2D material with large area and uniformity was synthesized. In this way, however, the substrate is, for example, SiO2the/Si, sapphire, mica and the like are difficult to remove, and therefore, removing the substrate in practical application increases the cost and the flow of preparing the two-dimensional material, and limits the wide application of the method. Wet chemical methods (e.g., water/solvothermal, sol-gel, and soft gel templating methods) generally have higher productivity due to the high availability of precursor atoms for liquid reaction systems. In such synthesis systems, surfactants or polymer monomers are typically introduced to induce the 2D morphology, but surfactant and polymer residues can affect the 2D materialChemical and physical properties, and thus it is difficult to achieve high quality two-dimensional materials using wet chemical methods.
Although most 2D materials with different structures and compositions can be synthesized using the above methods, there is still a lack of rapid, high-throughput, low-cost and simple synthesis methods to further explore the potential of 2D materials in different applications.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the primary object of the present invention is to provide a method for preparing a domain-limited growth ultrathin two-dimensional material.
The invention also aims to provide the ultra-thin two-dimensional material with limited growth domain prepared by the preparation method.
It is a further object of the present invention to provide the use of the above-described ultra-thin two-dimensional materials grown in confined areas.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an ultrathin two-dimensional material with limited growth comprises the following steps:
uniformly dispersing a small amount of reactant A on the surface of another large amount of reactant crystal powder B to obtain a mixture; then reacting the uniformly dispersed mixture by adopting a hydrothermal method to form a two-dimensional material with an ultrathin structure, namely the ultrathin two-dimensional material with limited growth; wherein the reactant crystal powder B is used as a template, and the particle size of the reactant crystal powder B is 10-50 μm;
the mass ratio of the reactant crystal powder B to the reactant A is preferably not less than 15: 1;
the preparation method of the ultra-thin two-dimensional material with limited growth preferably comprises the following steps:
(1) thinning the reactant crystal powder B to a particle size of 10-50 μm;
(2) adding the reactant A into a solvent to prepare a precursor solution; wherein, the reactant A is soluble in the solvent, and the reactant B is insoluble or slightly soluble in the solvent;
(3) adding the reactant crystal powder B subjected to the grain refinement treatment in the step (1) into the precursor solution prepared in the step (2), and stirring until the system is pasty to obtain a mixture;
(4) uniformly coating the mixture prepared in the step (3) on a carrier, then placing the carrier in a reaction system, and carrying out hydrothermal reaction to obtain a first reaction product;
(5) carrying out suction filtration and drying on the first reaction product prepared in the step (4) to obtain an ultrathin two-dimensional material with limited-area growth;
the reactant crystal powder B in the step (1) is preferably NaCl, MnSO4And CaCl2At least one of;
the reactant A in the step (2) is preferably VO (acac)2(vanadium bis (acetylacetonate) oxide);
the solvent in the step (2) is preferably absolute ethyl alcohol;
the concentration of the precursor solution of the reactant A in the step (2) is preferably 0.05 mol/L;
the mass volume ratio of the reactant crystal powder B to the precursor solution in the step (3) is preferably (2-3) g: (5-10) mL;
the carrier in the step (4) is preferably a polytetrafluoroethylene sheet or a carbon cloth;
the temperature of the hydrothermal reaction in the step (4) is preferably 150-180 ℃;
the time of the hydrothermal reaction in the step (4) is preferably 120-180 min;
the drying in the step (5) is preferably vacuum drying;
the temperature for drying in the step (5) is preferably 60 ℃;
an ultrathin two-dimensional material with limited growth is prepared by the preparation method;
the ultra-thin two-dimensional material with limited growth is applied to the fields of catalysis, electrochemical energy storage and the like;
uniformly dispersing a small-dose reactant A on the surface of another large-dose reactant crystal powder B (serving as a template and having a particle size of 10-50 mu m) to obtain a mixture; and then reacting the uniformly dispersed mixture by a hydrothermal method to form the two-dimensional material with the ultrathin structure. The specific principle is as follows: a small amount of reactant A precursor solution is uniformly coated on the surface of a large amount of reactant crystal particles B, so that the precursor grows in a limited space on the surface of the crystal particles B, the transverse growth is guided by the geometrical shape of the crystal particles B, and the growth vertical to the surface of the crystal particles B is limited by the limited space and the amount of the precursor, so that the precursor can form an ultrathin two-dimensional material on the surface of a microcrystal B.
In the hydrothermal reaction process, the crystal powder B can play a role of both a reactant and a template source; the small size of the crystalline powder B allows the reactant a to be uniformly dispersed on its surface and provides a limited area for the first reaction product to form an ultra-thin two-dimensional material. Experimental detection shows that the two-dimensional material with the ultrathin structure is successfully prepared by the technical scheme.
Compared with the prior art, the invention has the following advantages and effects:
(1) the invention is different from similar salt-assisted methods, is not limited to the preparation of two-dimensional materials by using salt as a template, and does not participate in reactions and the like.
(2) The method can be used for preparing ultrathin two-dimensional materials as long as the condition that A can be uniformly dispersed on the surface of B crystal grains and the condition that B crystal grains are small enough to provide limited growth is met, and different types of bimetal oxide two-dimensional materials are synthesized by adjusting the types of precursors and salt microcrystals according to requirements; controlling the total amount of the synthesized two-dimensional material according to the total amount of the mixture ratio of the A and the B; in addition, the thickness of the 2D material can be easily controlled by adjusting the ratio of segments a and B.
(3) The method belongs to low-temperature growth, and reactants serving as templates can participate in the reaction, so that the universality is stronger; and the reaction condition is mild, and the yield is high.
Drawings
FIG. 1 shows a domain-limited growth of an ultrathin two-dimensional sodium vanadate material (reactant A-vanadyl acetylacetonate VO (acac))2Reactant B-NaCl).
FIG. 2 is an XRD representation of the domain-limited growth sodium vanadate ultrathin two-dimensional material prepared in example 1.
FIG. 3 is an SEM representation of the domain-limited growth sodium vanadate ultrathin two-dimensional material prepared in example 1.
FIG. 4 is a TEM representation of the domain-limited grown sodium vanadate ultrathin two-dimensional material prepared in example 1.
FIG. 5 shows a limited-area growth manganese vanadate ultrathin two-dimensional material (reactant A-VO (acac))2Reactant B-MnSO4) SEM characterization of (d).
FIG. 6 shows a domain-limited growth calcium vanadate ultrathin two-dimensional material (reactant A-VO (acac))2Reaction B-CaCl2) SEM characterization of (d).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
The embodiment provides a preparation method of a sodium vanadate ultrathin two-dimensional material with limited growth, which comprises the following reaction raw materials: reactant A-VO (acac)2Reactant B-NaCl and solvent-absolute ethyl alcohol. As shown in the preparation flow chart of fig. 1, the method comprises the following steps:
(1) weighing 2g of NaCl particles, and thinning the NaCl particles until the particle size is 10-50 mu m, wherein the specific method comprises the following steps: dissolving NaCl in deionized water, then quickly freezing by adopting liquid nitrogen, and freeze-drying by using a freeze dryer;
(2) weighing 0.19887g of VO (acac)2Added to 15mL of absolute ethanol and magnetically stirred until VO (acac)2Complete dissolution to obtain VO (acac)2The ethanol solution is a precursor solution, and the concentration is 0.05 mol/L;
(3) adding NaCl after the particle refining treatment in the step (1) into 10mL of VO (acac) prepared in the step (2)2Magnetically stirring until the ethanol is volatilized to form paste, and obtaining a mixture of NaCl and vanadyl acetylacetonate; wherein, a little absolute ethyl alcohol in the mixture can be left, and the mixture absorbs a little water;
(4) mixing NaCl prepared in the step (3) and VO (acac)2The mixture is evenly coated on a carrier carbon cloth in a thin layer, and then the carbon cloth is suspendedPutting the reaction kettle into a drying box in the reaction kettle, setting the heat preservation temperature to be 180 ℃, and preserving the heat for 180min to obtain a first reaction product;
(5) after the reaction is finished, taking out the first reaction product in the reaction kettle, carrying out suction filtration on the reaction product by using ethanol, then carrying out suction filtration by using deionized water, and carrying out vacuum drying on the residual product after suction filtration at 60 ℃ to obtain a sodium vanadate ultrathin two-dimensional material with limited growth; wherein, the first reaction product is filtered and dried, and residual NaCl and VO (acac) in the reaction product can be removed2；
The sodium vanadate ultrathin two-dimensional material with limited growth prepared in the embodiment is subjected to X-ray diffraction, scanning electron microscope scanning and transmission electron microscope scanning in sequence, and the result is shown in FIGS. 2-4. As can be seen from FIG. 2, NaCl can not only be used as a template for generating a two-dimensional material, but also participate in a reaction. In the scanning electron microscope and transmission electron microscope images, it can be seen that NaCl participates in the reaction to generate an ultrathin two-dimensional structure.
Example 2
The embodiment provides a preparation method of a manganese vanadate ultrathin two-dimensional material with limited growth. The reaction raw materials are as follows: reactant A-VO (acac)2Reactant B-MnSO4Solvent-absolute ethyl alcohol. As shown in the preparation flow chart of fig. 1, the method comprises the following steps:
(1) weighing 2g of MnSO4The method comprises the following steps of carrying out particle refinement treatment until the particle size is 10-50 mu m: mixing MnSO4Dissolving in deionized water, quickly freezing by adopting liquid nitrogen, and freeze-drying by using a freeze dryer;
(2) weighing 0.19887g of VO (acac)2Added to 15mL of absolute ethanol and magnetically stirred until VO (acac)2Complete dissolution to obtain VO (acac)2The ethanol solution is a precursor solution, and the concentration is 0.05 mol/L;
(3) MnSO treated by the grain refinement treatment in the step (1)4Adding 10mL of VO (acac) prepared in the step (2)2Magnetically stirring until the ethanol volatilizes to form paste to obtain MnSO4And VO (acac)2A mixture of (a); wherein in the mixtureA little of the absolute ethyl alcohol can be left, and the mixture has little water absorption;
(4) MnSO prepared in the step (3)4And VO (acac)2The mixture is evenly smeared on a carrier carbon cloth in a thin mode, then the carbon cloth is hung in a reaction kettle, the reaction kettle is placed in a drying box, the heat preservation temperature is set to be 150 ℃, the heat preservation time is set to be 120min, and a first reaction product is obtained;
(5) after the reaction is finished, taking out the first reaction product in the reaction kettle, carrying out suction filtration on the reaction product by using ethanol, then carrying out suction filtration by using deionized water, and carrying out vacuum drying on the residual product after the suction filtration at 60 ℃ to obtain a limited-area-grown manganese vanadate ultrathin two-dimensional material; wherein the first reaction product is filtered and dried to remove the residual MnSO in the reaction product4And VO (acac)2；
Scanning electron microscope scanning is performed on the material prepared in the embodiment, and the obtained result is shown in fig. 5, and the material is an ultrathin two-dimensional structure with limited growth.
Example 3
The embodiment provides a preparation method of a calcium vanadate ultrathin two-dimensional material with limited growth. The reaction raw materials are as follows: reactant A-VO (acac)2And the reactant B-CaCl2Solvent-absolute ethyl alcohol. As shown in the preparation flow chart of fig. 1, the method comprises the following steps:
(1) weighing 3g of CaCl2The method comprises the following steps of carrying out particle refinement treatment until the particle size is 10-50 mu m: adding CaCl2Dissolving in deionized water, quickly freezing by adopting liquid nitrogen, and freeze-drying by using a freeze dryer;
(2) weighing 0.19887g of VO (acac)2Added to 15mL of absolute ethanol and magnetically stirred until VO (acac)2Complete dissolution to obtain VO (acac)2The ethanol solution is a precursor solution, and the concentration is 0.05 mol/L;
(3) the CaCl after the particle refining treatment in the step (1)2Adding 10mL of VO (acac) prepared in the step (2)2Magnetically stirring until the ethanol is volatilized to form paste to obtain CaCl2And VO (acac)2A mixture of (a); wherein the content of the first and second substances,a little absolute ethyl alcohol in the mixture can remain, and the mixture absorbs a little water;
(4) CaCl prepared in the step (3)2And VO (acac)2The mixture is evenly smeared on a carrier carbon cloth in a thin mode, then the carbon cloth is hung in a reaction kettle, the reaction kettle is placed in a drying box, the heat preservation temperature is set to be 170 ℃, the heat preservation time is set to be 160min, and a first reaction product is obtained;
(5) after the reaction is finished, taking out the first reaction product in the reaction kettle, carrying out suction filtration on the reaction product by using ethanol, then carrying out suction filtration by using deionized water, and carrying out vacuum drying on the residual product after the suction filtration at 60 ℃ to obtain a calcium vanadate ultrathin two-dimensional material with limited growth; wherein the first reaction product is filtered and dried to remove the remaining CaCl in the reaction product2And VO (acac)2。
Scanning electron microscope scanning is performed on the material prepared in the embodiment, and the obtained result is shown in fig. 6, and the material is an ultrathin two-dimensional material with limited growth.
Comparative example 1
Reference to this comparative example: hu, Z, Xiao, X, Jin, h.et al. rapid mass production of two-dimensional oxides and hydroxides via the mol present method, com 8,15630(2017), the specific preparation process is as follows:
(1) 5g of nitrate powder was added to the crucible;
(2) the crucible was heated to 350 ℃ (NaNO for sodium nitrate)3) Or 380 deg.C (KNO for potassium nitrate)3) Then transferring the mixture into a muffle furnace for about 10 minutes;
(3) when the nitrate was molten, 0.2g of manganese sulfate (MnSO) was added to the molten salt4) Powder for about 1 minute;
(4) the product was removed from the muffle and cooled to room temperature under ambient conditions;
(5) the product was washed with deionized water to remove NaNO3Or KNO3Then dried to obtain Na0.55Mn2O4·1.5H2O or K0.27MnO2·0.54H2O ultrathin two-dimensional material.
The process of the invention was compared with comparative example 1: comparative example 1 use of molten salt for two-dimensional material formation assistance, reaction at higher temperature was required, and nitrate was likely to produce NO when molten2And the like, and limits the application of the method to a certain extent. The method can be used for reaction at a relatively low temperature, has low energy consumption, is safe and convenient, can be used for preparing a large amount of two-dimensional materials, and has higher universality.
Comparative example 2
Reference to this comparative example: xiao, x, Song, h, Lin, s.et al. scalable salt-mapped synthesis of two-dimensional transformation metals.nat Commun 7,11296 (2016.) specific preparation process is as follows:
(1) mn (CH) amounting to 0.5g3COO)2·4H2O was dispersed in 25ml of ethanol and stirred for 5 minutes to obtain MnO precursor solution;
(2) mixing the MnO precursor solution with 400g potassium chloride powder and drying at 70 ℃ under stirring;
(3) the dried mixture was heated at 2 ℃ for min under Ar atmosphere-1Further annealing at 400 ℃ for 1 h;
(4) cooling after annealing, washing the product with deionized water to remove a KCl template, and drying to obtain an ultrathin two-dimensional MnO material;
the process of the invention was compared with comparative example 2: the comparative example 2 is similar to the method of the invention, the comparative example 2 is beneficial to the crystal salt powder to generate the two-dimensional material in an auxiliary way, the small-dose precursor is uniformly dispersed on the surface of the salt particle to achieve the purpose of growing the two-dimensional material in a limited area, but high-temperature annealing is needed, the template does not participate in the reaction, and the subsequent washing and removal are needed. But the method is not limited to the use of salt for assistance any more, and the two-dimensional material can be synthesized by compounding the conditions of the method; and the substance serving as the template can also be used for reaction, and a proper reactant is selected to achieve the aim of modifying the two-dimensional material, so that the step of preparing the high-performance two-dimensional material is simplified, and the superiority of the method is revealed.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of an ultrathin two-dimensional material with limited growth is characterized by comprising the following steps:
uniformly dispersing a small amount of reactant A on the surface of another large amount of reactant crystal powder B to obtain a mixture; then reacting the uniformly dispersed mixture by adopting a hydrothermal method to form a two-dimensional material with an ultrathin structure, namely the ultrathin two-dimensional material with limited growth; wherein the reactant crystal powder B is used as a template, and the particle size of the reactant crystal powder B is 10-50 μm;
the mass ratio of the reactant crystal powder B to the reactant A is not less than 15: 1.
2. The method for preparing the ultra-thin two-dimensional material with limited domain growth of claim 1, which is characterized by comprising the following steps:
(1) thinning the reactant crystal powder B to a particle size of 10-50 μm;
(2) adding the reactant A into a solvent to prepare a precursor solution; wherein, the reactant A is soluble in the solvent, and the reactant B is insoluble or slightly soluble in the solvent;
(3) adding the reactant crystal powder B subjected to the grain refinement treatment in the step (1) into the precursor solution prepared in the step (2), and stirring until the system is pasty to obtain a mixture;
(4) uniformly coating the mixture prepared in the step (3) on a carrier, then placing the carrier in a reaction system, and carrying out hydrothermal reaction to obtain a first reaction product;
(5) and (4) carrying out suction filtration and drying on the first reaction product prepared in the step (4) to obtain the ultra-thin two-dimensional material with limited-area growth.
3. The method for preparing the ultra-thin two-dimensional material with limited growth according to claim 2, wherein the method comprises the following steps:
the reactant crystal powder B in the step (1) is NaCl and MnSO4And CaCl2At least one of (1).
4. The method for preparing the ultra-thin two-dimensional material with limited growth according to claim 2, wherein the method comprises the following steps:
the reactant A in the step (2) is VO (acac)2。
5. The method for preparing the ultra-thin two-dimensional material with limited growth according to claim 2, wherein the method comprises the following steps:
the solvent in the step (2) is absolute ethyl alcohol.
6. The method for preparing the ultra-thin two-dimensional material with limited growth according to claim 2, wherein the method comprises the following steps:
the concentration of the precursor solution of the reactant A in the step (2) is 0.05 mol/L;
the mass-to-volume ratio of the reactant crystal powder B to the precursor solution in the step (3) is (2-3) g: (5-10) mL.
7. The method for preparing the ultra-thin two-dimensional material with limited growth according to claim 2, wherein the method comprises the following steps:
the carrier in the step (4) is a polytetrafluoroethylene sheet or carbon cloth.
8. The method for preparing the ultra-thin two-dimensional material with limited growth according to claim 2, wherein the method comprises the following steps:
the temperature of the hydrothermal reaction in the step (4) is 150-180 ℃;
the hydrothermal reaction time in the step (4) is 120-180 min.
9. An ultrathin two-dimensional material with limited growth is characterized by being prepared by the preparation method of any one of claims 1-8.
10. Use of the domain-limited grown ultrathin two-dimensional material of claim 9 in the fields of catalysis and electrochemical energy storage.
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