CN111943207B - Method for preparing fluorine-free two-dimensional material MXene simply and in pollution-free manner - Google Patents
Method for preparing fluorine-free two-dimensional material MXene simply and in pollution-free manner Download PDFInfo
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Abstract
The invention provides a simple and pollution-free method for preparing a fluorine-free two-dimensional material MXene. The invention provides a simple and pollution-free method for preparing a two-dimensional material MXene, which is characterized in that the MXene is prepared by carrying out steam etching on a MAX two-dimensional material through an iodine co-solvent, the iodine co-solvent generates iodine steam after being heated, and the iodine steam and an A layer element are subjected to oxidation-reduction reaction etching at high temperature to obtain the MXene.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a simple and pollution-free method for preparing a fluorine-free two-dimensional material MXene.
Background
The two-dimensional material MXene is a novel carbon/nitride two-dimensional nano layered material prepared by etching an A atomic layer in a MAX phase by using a proper etchant and utilizing weak bonding force between the A sheet layer and the MX sheet layer in the MAX phase, has good conductivity and hydrophilicity, and contains M and X diatoms or polyatomic atoms with better stability in an MX structure compared with a monoatomic structure of graphene. In addition, C and C atoms in the graphene are bonded singly, and M-X is a mixed valence bond of a covalent bond, an ionic bond and a metal bond, which also indicates that the M-X two-dimensional material MXene has richer and more adjustable performance than the graphene, and shows great application prospects in the fields of environmental management, energy sources, composite materials and the like.
Currently, the MXene preparation method is mainly obtained by etching a weak a layer element in a MAX phase with a mixed solution of hydrofluoric acid, a fluoride salt and hydrochloric acid, or ammonium bifluoride. Although the method for preparing the MXene two-dimensional material by using the fluoride is relatively efficient, the preparation process has serious environmental pollution, and the application of the prepared MXene two-dimensional material in the field of energy storage is greatly limited by a large number of F-based terminal functional groups.
In order to solve the problems, a method for preparing an MXene two-dimensional material by etching an element in an A layer in a MAX phase without fluorine also appears on the market, for example, CN110540236A, the MXene two-dimensional material is prepared by using a high-temperature molten salt method (the MXene two-dimensional material taking Br/I as a surface group is prepared by using a transition metal bromide/transition metal iodide to react with MAX), but the preparation method is carried out under normal pressure, and the etching depth is shallow; and the product needs acid washing and drying to remove impurities, and the conditions are complex, so that the industrialization of MXene production is not facilitated.
Disclosure of Invention
In view of the above, the present invention provides a simple and pollution-free method for preparing fluorine-free two-dimensional material MXene, so as to overcome the deficiencies in the prior art.
Another object of the present invention is to provide MXene two-dimensional materials and uses of said two-dimensional materials.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a simple and pollution-free method for preparing fluorine-free MXene is characterized in that an iodine co-fusing agent and MAX are uniformly mixed, then the mixture is transferred into a sealed reaction bin, and is subjected to heating treatment in an inert environment, and after the reaction is finished, the fluorine-free MXene two-dimensional material is prepared.
Further, the iodine co-flux is a substance that can be decomposed into iodine vapor after heating, including but not limited to elemental iodine or triiodide salt.
Further, the mass ratio of the iodine co-flux to the MAX phase is 5-200.
Further, the inert environment includes, but is not limited to, argon, helium, nitrogen, or a vacuum environment.
Further, the temperature of the heating treatment is 100-1000 ℃.
Further, the reaction time of the heating treatment is 0.5h-72h.
Furthermore, the pressure range in the sealed reaction bin is-10 MPa to 100MPa.
Further, M in the MAX phase is a transition group metal element including, but not limited to, ti, zr, hf, V, nb, ta, cr, and/or Sc; a is Al or Si; x is C or N element.
Further, after the reaction is finished, circulating hot inert gas to the sealed reaction bin to remove impurities.
In another aspect of the present invention, the molecular formula of the MXene two-dimensional material is represented as M n+1 X n I 2 Wherein M is a transition group metal element including, but not limited to, ti, zr, hf, V, nb, ta, cr and/or Sc; x is C or N element, N is 1, 2, 3 or 4;
the fluorine-free MXene two-dimensional material is of a two-dimensional regular lamellar structure.
In another aspect of the invention, there is provided the use of an MXene two-dimensional material in the preparation of an energy storage material, a composite material, a lubricating material, an adsorbent material or a catalyst.
Compared with the prior art, the invention has the following advantages:
(1) The invention creates the simple and pollution-free method for preparing the fluoride-free two-dimensional material MXene, the principle is that the two-dimensional material MXene is prepared by carrying out vapor etching on the MAX through an iodine co-solvent, the iodine co-solvent generates iodine vapor after being heated, and the iodine vapor and the layer A element are subjected to oxidation-reduction reaction etching at high temperature to obtain the MXene.
(2) The method for preparing the fluoride-free two-dimensional material MXene, which is simple and pollution-free, creatively uses the iodine simple substance as the etching agent, the iodine simple substance has the advantages of wide source, easiness in obtaining and low cost, other impurities cannot be introduced, and the purity of the product MXene is higher.
(3) The invention creates the simple and pollution-free method for preparing the fluoride-free two-dimensional material MXene, the reaction is carried out in the sealed reaction chamber, the etching depth can be improved by controlling the pressure of iodine vapor, the reaction time is shortened, and the MXene purity is improved; the reaction temperature can be controlled to provide enough reaction activation energy to enable the reaction to be continuously carried out; the purity of the etching can be increased by controlling the reaction time.
(4) According to the simple and pollution-free method for preparing the fluoride-free two-dimensional material MXene, after the heating reaction is completed, the impurity removal can be completed only by circulating hot inert gas to the sealed reaction bin, other treatment processes such as acid washing and the like are not needed, the product purity is high, impurities are not introduced, waste liquid is not generated, the operation is simple, the environment is friendly, and the large-scale production is facilitated.
(5) The fluorine-free MXene two-dimensional material provided by the invention has the advantages that the MXene material taking iodine as a surface group has better chemical stability and thermal stability than the traditional MXene taking fluorine as a surface group, has richer adjustable and controllable spaces in electrical properties, dielectric properties and the like, and has better application in the preparation of energy storage materials, composite materials, lubricating materials, adsorbing materials or catalysts and the like.
Drawings
FIG. 1 (a) is a MAX Scanning Electron Microscope (SEM) photograph based on the raw material in example 1;
fig. 1 (b) is a Scanning Electron Microscope (SEM) photograph of an MXene two-dimensional material prepared according to example 1;
FIG. 2 is an X-ray diffraction (XRD) spectrum based on MAX and MXene two-dimensional materials prepared in example 1;
fig. 3 is an energy dispersive X-ray (EDS) spectrum of an MXene two-dimensional material prepared based on example 1;
fig. 4 is a Scanning Electron Microscope (SEM) photograph of an MXene two-dimensional material prepared according to example 2;
fig. 5 is a Scanning Electron Microscope (SEM) photograph of an MXene two-dimensional material prepared according to example 3;
fig. 6 is a Scanning Electron Microscope (SEM) photograph of an MXene two-dimensional material prepared according to example 4;
fig. 7 is a Scanning Electron Microscope (SEM) photograph of MXene two-dimensional material prepared according to example 5.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
In view of the shortcomings in the prior art, the inventor of the present invention has made extensive studies and extensive practices to propose the technical solution of the present invention, and further explains the technical solution, the implementation process and principles thereof, and the like as follows.
In summary, the invention is a method for preparing a fluoride-free two-dimensional material MXene by iodine co-flux vapor etching MAX: uniformly mixing the iodine co-flux and the MAX, transferring the mixture into a sealed reaction chamber, heating the reaction chamber in an inert environment to generate iodine steam after the iodine co-flux is heated, carrying out oxidation-reduction reaction etching on the generated iodine steam and the layer A elements at a high temperature, circularly introducing hot inert gas to carry out purging and impurity removal after the reaction is finished, and naturally cooling to obtain the MXene two-dimensional material.
The inventor of the invention pays creative efforts, and the obtained technical scheme makes remarkable improvements on the prior art in the following aspects, and the improvements have obvious positive significance in reducing production cost, improving reaction efficiency and improving reaction effect. The specific description is as follows:
the preparation method of the MXene two-dimensional material creatively introduces iodine eutectic agent such as iodine simple substance or triiodide salt and the like as reactant, the iodine eutectic agent is utilized to generate iodine steam under heating reaction, and MAX phase is further etched to obtain the MXene two-dimensional material with iodine as surface group. In particular, the inventors of the present invention have creatively found that the etching reaction can be performed using only a common simple substance of iodine as an etchant. The iodine simple substance has the advantages of wide sources, easy obtainment and low cost, other impurities cannot be introduced, and the purity of the product MXene is higher.
The further improvement is that according to the requirement, the invention can even directly introduce iodine vapor into the closed reaction container, and directly use the iodine vapor to etch the MAX phase to obtain the MXene two-dimensional material with iodine as the surface group. By the technical means, the production flow is further simplified, and the reaction efficiency and the product purity are improved.
Compared with the reaction for preparing the MXene two-dimensional material by using the fluorine-containing etching agent in the prior art, the reaction method adopts the iodine cosolvent or the iodine steam which can generate iodine steam under the heating condition as the reactant, the reactant has low toxicity and is more environment-friendly, the chemical stability and the thermal stability of the reactant are superior to those of MXene taking the traditional fluorine as a surface group, and the electrical property, the dielectric property and the like of the reactant have richer adjustable space.
In the technical scheme of the invention, the etching depth is improved and the reaction time is reduced by simply controlling the iodine vapor pressure, and the reaction is continuously carried out by controlling the reaction temperature; compared with solution etching, the reaction process is simpler and controllable, and the reaction efficiency is further improved.
In the technical scheme of the invention, the reaction temperature can be far lower than that of a high-temperature molten salt method. It can be understood by those skilled in the art that the technical scheme of the invention only needs to supply less heat to enable the iodine simple substance or the triiodide salt to form iodine vapor. The high temperature molten salt method must be above 400-500 ℃ to form molten salt in the reaction system, and further, the smooth proceeding of the etching reaction can be ensured. This is never disclosed or disclosed in the prior art, and is one of the outstanding advantages of the solution of the present invention.
Further, compared with high-temperature molten salt etching in the prior art, the method provided by the invention does not need to use acid to wash the product for removing impurities, only needs inert gas to circularly sweep, does not introduce impurities, has high product purity, is simple and efficient in operation process, does not generate waste liquid, and is environment-friendly.
The invention is described in detail below with reference to embodiments and the accompanying drawings.
The first embodiment is as follows:
as shown in FIG. 1, 10g of elemental iodine and 0.1g of Ti were weighed 3 Mixing AlC uniformly, transferring into a tube furnace, treating at 500 deg.C under 10Mpa in Ar atmosphere for 6 hr, introducing Ar circulation gas at 300 deg.C for 2 hr after reaction is completed, removing AlI 3 And iodine vapor, and then naturally cooled. Namely the MXene two-dimensional material nanosheet.
FIG. 1 is Ti in example 1 3 And the shape and size characteristics of the AlC (a) and the prepared MXene two-dimensional material (b) are determined by a Scanning Electron Microscope (SEM). As shown in fig. 1 (a), MAX exhibits a massive structure with a bulk thickness of about 1 μm. High temperature iodine vapor selective redox etching of Ti 3 The intermediate phase Al layer of AlC makes the layered structure stripped. As shown in fig. 1 (b), MXene prepared exhibits an ultra-thin lamellar structure with a monolayer lamellar thickness of about 10nm.
FIG. 2 is Ti of example 1 3 And X-ray diffraction (XRD) spectra of the AlC and the prepared MXene two-dimensional material. As shown in FIG. 2, after high temperature iodine vapor etching, the original Ti 3 The characteristic AlC diffraction peak disappears and the MXene phase with high purity is transformed.
Fig. 3 is an energy dispersive X-ray (EDS) spectrum of an MXene two-dimensional material prepared in example 1. As shown in FIG. 3, the element contents of carbon, aluminum, titanium and iodine of the prepared MXene two-dimensional material are 53%,14%,7% and 26%, respectively, and no fluorine element exists. This result is a good demonstration that MXene is prepared as a two-dimensional material with I as the surface group.
The second embodiment:
5g of iodine and 0.1g of V are weighed 2 Mixing AlC uniformly, transferring into a tube furnace, treating at 200 deg.C under 2Mpa and He atmosphere for 24h, introducing He circulation gas at 200 deg.C for 2h after reaction is completed, and removing AlI 3 And iodine vapor, and then naturally cooled. Namely the MXene two-dimensional material nanosheet. Fig. 4 is a Scanning Electron Microscope (SEM) topographic dimension feature of the MXene two-dimensional material prepared in example 2. The prepared MXene has an ultrathin lamellar structure.
Example three:
weigh 17g of BI 3 And 0.1g of Ti 2 AlN is evenly mixed and then is transferred into a tube furnace, the mixture is treated for 4 hours under the pressure of 5Mpa and the temperature of 800 ℃ in vacuum atmosphere, after the reaction is completed, the mixture is continuously vacuumized for 2 hours under the temperature of 900 ℃, and the AlI is removed 3 And iodine vapor, and then naturally cooled. Namely the MXene two-dimensional material nanosheet. Fig. 5 is a Scanning Electron Microscope (SEM) topographic dimension feature of the MXene two-dimensional material prepared in example 3. The prepared MXene has an ultrathin lamellar structure.
Example four:
weigh 20g of BI 3 And 0.1g of Ti 3 SiC 2 Mixing, transferring into a tube furnace, treating at 10Mpa under vacuum at 1000 deg.C for 1 hr, cooling to 300 deg.C after reaction, vacuumizing at 300 deg.C for 2 hr, and removing SiI 4 And iodine vapor, and then naturally cooled. Namely the MXene two-dimensional material nanosheet. Fig. 6 is a Scanning Electron Microscope (SEM) topographical dimensional feature of the MXene two-dimensional material prepared in example 4. The prepared MXene has an ultrathin lamellar structure.
EXAMPLE five
Weigh 10g of BI 3 And 0.1g of Ti 3 SnC 2 Mixing, transferring into a tube furnace, treating at 50Mpa at 600 deg.C for 10 hr, reacting completely, vacuumizing at 600 deg.C for 2 hr, and removing SnI 4 And iodine vapor, and then naturally cooled. Namely the MXene two-dimensional material nanosheet. Fig. 7 is a Scanning Electron Microscope (SEM) topographic dimensional feature of the MXene two-dimensional material prepared in example 5. The prepared MXene has an ultrathin lamellar structure.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the invention, so that any modifications, equivalents, improvements and the like, which are within the spirit and principle of the present invention, should be included in the scope of the present invention.
Claims (7)
1. A method for preparing fluoride-free two-dimensional material MXene simply and in a pollution-free manner is characterized by comprising the following steps: uniformly mixing the iodine eutectic agent and the MAX phase, transferring the mixture into a sealed reaction chamber, heating the mixture in an inert environment or a vacuum environment, and obtaining the MXene two-dimensional material after the reaction is finished, wherein: the iodine co-flux is a substance which can be decomposed into iodine steam after being heated, and comprises an iodine simple substance or triiodide salt; m in the MAX phase is a transition metal element, and comprises Ti, zr, hf, V, nb, ta, cr and/or Sc; a is a third or fourth main group element; x is C or N element.
2. The simple and pollution-free preparation method of the fluorine-free two-dimensional material MXene according to claim 1, wherein: the mass ratio of the iodine eutectic agent to the MAX phase is 5-200.
3. The simple and pollution-free preparation method of the fluorine-free two-dimensional material MXene according to claim 1, wherein: the inert environment comprises argon, helium or nitrogen.
4. The simple and pollution-free method for preparing the fluorine-free two-dimensional material MXene according to claim 1, wherein the method comprises the following steps: the temperature of the heating treatment is 100-1000 ℃, and the reaction time of the heating treatment is 0.5-72 h.
5. The simple and pollution-free preparation method of the fluorine-free two-dimensional material MXene according to claim 1, wherein: the pressure range in the sealed reaction bin is 2MPa to 100MPa.
6. The simple and pollution-free preparation method of the fluorine-free two-dimensional material MXene according to claim 1, wherein: and after the reaction is finished, circularly introducing hot inert gas into the sealed reaction bin to carry out purging and impurity removal.
7. A simple and pollution-free method for preparing a fluorine-free two-dimensional material MXene is characterized by comprising the following steps: introducing iodine steam into a sealed reaction chamber filled with MAX phase, heating in inert environment or vacuum environment, and obtaining MXene two-dimensional material after reaction; m in the MAX phase is a transition metal element, and comprises Ti, zr, hf, V, nb, ta, cr and/or Sc; a is a third or fourth main group element; x is C or N element.
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| EP3957601A1 (en) | 2020-08-19 | 2022-02-23 | Technische Universität Dresden | Method for the synthesis of mxenes, mxene nanosheets and their use |
| WO2022153889A1 (en) * | 2021-01-13 | 2022-07-21 | 株式会社村田製作所 | Adsorption element, method for manufacturing same, adsorption sheet, separation film, and artificial dialysis equipment |
| CN112794329B (en) * | 2021-02-26 | 2023-12-19 | 山东大学 | Green preparation method and application of MXene material |
| CN115367754B (en) * | 2021-05-21 | 2023-11-14 | 北京航空航天大学 | Method for preparing MAX phase material by MXene conversion and application |
| CN114031078B (en) * | 2021-11-19 | 2024-04-12 | 徐州纳烯新材料研究院有限公司 | Preparation method of fluorine-free MXene two-dimensional nanosheets |
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