CN112591718A - Two-dimensional material Fe3GeTe2Preparation method of nanosheet - Google Patents
Two-dimensional material Fe3GeTe2Preparation method of nanosheet Download PDFInfo
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Abstract
The invention relates to a two-dimensional material Fe3GeTe2A preparation method of the nano-sheet. The method comprises the following steps: 1) fe3GeTe2Grinding the crystals in a liquid medium; 2) transferring the ground mixture into a certain amount of same liquid phase medium, heating and stirring; 3) subjecting the stirred mixture to ultrasonic treatment; 4) centrifugal classification to obtain Fe3GeTe2A two-dimensional nanosheet dispersion; 5) freeze drying to obtain Fe3GeTe2Two-dimensional nanosheet powder. The method of the invention has the following advantages: 1) the process is simple, and the preparation period is short; 2) macro preparation can be realized; 3) can prepare Fe with controllable thickness3GeTe2Nanosheets, mainly concentrated in single, few and multi-layer ranges; 4) can prepare Fe with controllable size3GeTe2Nanosheets, having a size in the range of nanometers to micrometers; 5) preparation of the resulting Fe3GeTe2Nanosheet segmentThe defect is less, and the crystal structure is kept complete. The method is simple and feasible, and can greatly promote Fe3GeTe2Research and application of materials.
Description
Technical Field
The invention relates to a two-dimensional material Fe3GeTe2A preparation method of a nano sheet, in particular to a method capable of preparing Fe in a macroscopic quantity3GeTe2A liquid phase stripping method of two-dimensional nanosheets. Grinding for thinning, intercalating solvent molecules, and performing ultrasonic treatmentStripping and centrifugal classification to obtain single-layer, few-layer and multi-layer high-quality Fe with controllable thickness and size3GeTe2Two-dimensional nanosheets.
Background
Novel two-dimensional magnetic material Fe3GeTe2The Van der Waals metal compound with the ferromagnetic order is different from a general two-dimensional material, and due to the unique spintronics, the Van der Waals metal compound has a series of quantum physical mechanical properties, such as Hall effect, giant magnetoresistance effect, electronic coupling effect, magnetocaloric effect and the like, which plays a revolutionary promotion role in the development of quantum spin devices.
Existing two-dimensional magnetic material Fe3GeTe2The preparation method mainly adopts two methods of mechanical stripping and chemical vapor transport, and the obtained nano-sheet has complete structure and few defects; but the disadvantages are also very obvious, such as low yield, difficult control of conditions and unsuitability for large-scale production.
Chinese patent CN111593402A discloses a two-dimensional ferromagnetic material Fe3GeTe2And Fe doped with Co3-xCoxGeTe2Method of growing single crystal, wherein Fe is obtained3GeTe2The monocrystalline block has uniform components, the size of the nanosheet obtained by mechanical stripping is in the order of mum, and the thickness is in the order of nm.
CN110255549A discloses a preparation method of graphene and a stripping method of two-dimensional nano material, wherein the method relates to two-dimensional material Fe3GeTe2. The method comprises the following steps: mixing and reacting an alkali solution dispersed with a two-dimensional material with a soluble salt to obtain a mixed solution containing a grinding aid, wherein the grinding aid is in a supersaturated state in the mixed solution, and stirring the mixed solution dispersed with the two-dimensional material and solid particles precipitated by the grinding aid. According to the stripping method, under the stirring effect, solid particles can uniformly enter between two-dimensional materials to efficiently strip the two-dimensional materials, but a large amount of alkali and a large amount of soluble salt grinding aid are used, and post-treatment is needed, so that the preparation process is complex, the energy consumption is high, and the preparation efficiency is low.
In summary, the two-dimensional magnetic material Fe3GeTe2Of (2) peeling offThe mechanical stripping process is time-consuming, labor-consuming and incapable of mass production. Therefore, it is urgently needed to develop a method for preparing Fe with simple process and high quality3GeTe2A method of two-dimensional nanoplatelets.
Disclosure of Invention
The invention aims to provide a two-dimensional material Fe3GeTe2A method for producing a nanosheet, which enables Fe to be produced in large quantities3GeTe2The liquid phase stripping method of the two-dimensional nanosheet can overcome the problems of low yield, complex process and the like, and the liquid phase stripping method based on ultrasonic assistance does not introduce chemical reaction, so that the obtained nanosheet is high in quality, good in performance and controllable in thickness and size. The invention is expected to realize high-quality two-dimensional Fe3GeTe2The macro preparation of the nano sheet material promotes the research and the wide application of the nano sheet material.
The invention provides a two-dimensional material Fe3GeTe2The preparation method of the nanosheet comprises the following steps:
1) mixing Fe3GeTe2Grinding the crystal in a liquid phase medium with surface tension for 10 min-24 h;
2) transferring the ground mixture into the same liquid phase medium for stirring, wherein the stirring speed is 100-3000 rpm, the temperature is between room temperature and 80 ℃, and the time is 1-72 h;
3) carrying out ultrasonic treatment on the stirred mixture, wherein the ultrasonic power is 30-2000W, and the ultrasonic treatment time is 10 min-15 h;
4) centrifuging and cleaning the liquid phase medium of the mixture subjected to ultrasonic treatment at a high rotating speed, wherein the centrifugal rotating speed for cleaning the liquid phase medium is 5000-; then, centrifugally separating the two-dimensional nano-sheets at a low rotating speed, wherein the centrifugal rotating speed for separating the nano-sheets is 300-3000 rpm, and the centrifugal time is 10 min-2 h to obtain Fe3GeTe2A two-dimensional nanosheet dispersion;
5) freeze-drying the nanosheet dispersion, and freezing the nanosheet dispersion for 10 min-2 h; vacuum drier cold trap-50-90oC, the vacuum degree is 2-20 Pa, and the drying time is 1-6 days; to obtain Fe3GeTe2Two-dimensional nanosheet powder.
Fe in step 1)3GeTe2Quality of the crystal: the volume ratio of the liquid phase medium is as follows: 1:1-300 (g/mL); the surface tension of the liquid-phase medium is 10-100 mN.m-1。
The liquid phase medium is N-methylpyrrolidone (NMP), N-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), ethanol (EtOH), Acetonitrile (ACN), N-Hexane (HEX), Acetone (ACE), Toluene (TOL) and the like.
The mass ratio of the volume of the liquid phase medium to the used crystal raw material in the step 2) is 1:0.01-10 (L/g)
Preferably, in step 1): fe3GeTe2Quality of the crystal: the volume ratio of the liquid phase medium is as follows: 1:1-20 (g/mL).
Preferably, the mass ratio of the volume of the liquid phase medium to the used crystal raw material in the step 2) is 1:0.01-1 (L/g), the stirring speed is 300-1300 rpm, the temperature is 40-60 ℃, and the time is 5-60 h.
Preferably, the ultrasonic power in the step 3) is 300-1500W, and the time is 30 min-8 h.
Preferably, the centrifugation speed for washing the liquid phase medium in the step 4) is 10000-.
Preferably, the centrifugal rotation speed for separating the nano-sheets in the step 4) is 500-2000 rpm, and the centrifugal time is 30 min-1 h.
Preferably: and step 5), freezing the nanosheet dispersion for 0.5-1.5 h.
Preferably: the vacuum drier cold trap in the step 5) is-60 to-80oC, vacuum degree is 2-10 Pa, and drying time is 2-5 days.
The invention provides a two-dimensional material Fe3GeTe2The preparation method of the nano-sheet can prepare two-dimensional Fe in a macroscopic quantity3GeTe2Nanosheets. The liquid phase stripping method comprises grinding Fe in liquid phase medium3GeTe2Preliminarily thinning the crystal, stirring and soaking under heating condition to promote solvent molecule intercalation, increasing interlayer spacing, realizing lamella peeling by using ultrasound, and obtaining Fe by centrifugal separation3GeTe2Nano-sheet dispersion, finally freeze-drying to obtain single-layer, few-layer and multi-layer Fe3GeTe2The thickness of the nano-sheet powder is mainly concentrated in a few nanometers, and the size of the nano-sheet powder is from tens of nanometers to tens of micrometers (the thickness of the nano-sheet is 1-5 nm, and the size of the nano-sheet powder is 3-30 μm).
Compared with the prior art, the invention adopts the liquid phase method to treat Fe for the first time3GeTe2The crystal is stripped, and the Fe with controllable thickness and size is realized on the premise of ensuring complete structure and excellent performance3GeTe2The preparation of the nano-sheet has the thickness concentrated in the range of single layer, few layers and multiple layers, and the size is nano-grade to micron-grade; and producing the resulting Fe3GeTe2Few defects of the nanosheet, complete retention of the crystal structure, low cost, simple process and hopeful realization of two-dimensional Fe3GeTe2Mass production of materials, which greatly drives Fe3GeTe2Research and application of materials.
Drawings
FIG. 1 is a few layers of Fe in example 13GeTe2Nanoplate Atomic Force Microscopy (AFM) images and thickness curves.
FIG. 2 is the single layer Fe of example 23GeTe2Nanoplate Atomic Force Microscopy (AFM) images and thickness curves.
Detailed Description
The invention is further described with reference to specific examples. The specific experimental procedures and equipment involved in the examples were carried out in a conventional manner or under the conditions recommended by the manufacturer's instructions unless otherwise specified; all reagents involved are commercially available.
The following examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Various modifications and the like can be made to the invention as described herein after with reference to the drawings and which are within the scope of the appended claims.
Example 1
(1) Weighing 1 g of Fe3GeTe2The crystals were placed in 1 ml of N-methylpyrrolidone (NMP) and ground for 1 h with a mortar.
(2) The milled mixture was dispersed and transferred to a beaker with 100 mL NMP, 80 ℃ at 1000 rpm, and stirred in a water (oil) bath or heating mantle for 24 h.
(3) The liquid mixture was sonicated at 300W for 3 h.
(4) Centrifuging the mixture after ultrasonic treatment for 1 h at 18000 rpm by using a high-speed (freezing) centrifuge, removing a liquid phase medium, re-dissolving the precipitate by using deionized water, and repeating the centrifuging and re-dissolving operations for 6 times; centrifuging at 500 rpm for 1 h to obtain Fe3GeTe2A nanosheet dispersion.
(5) Freezing the dispersion liquid in liquid nitrogen for 0.5h, and placing the dispersion liquid in a vacuum drier with a cold trap of-50 to-90 DEGoC, vacuum degree of 2-10 Pa, drying for 3 days to obtain Fe3GeTe2The nano-sheet powder has a nano-sheet thickness of 1-5 nm and a size of 3-30 μm.
Fe3GeTe2The preparation method of the crystal comprises the following steps: the high purity Fe, Ge, Te elements were stoichiometrically mixed and vacuum sealed in a quartz tube. The test tube is placed in a double-zone horizontal furnace with the hot end temperature of 800 ℃ and the cold end temperature of 750 ℃ to be sintered for 2 weeks, so as to obtain the blazed crystal.
Example 2
(1) 20 g of Fe are weighed3GeTe2The crystals were placed in 20 ml NMP and ground in a mortar for 7 h.
(2) The milled mixture was dispersed and transferred to a beaker with 200 mL NMP, 80 ℃ at 1000 rpm, and stirred in a water (oil) bath or heating mantle for 24 h.
The steps (3), (4) and (5) are the same as the operation steps in the embodiment 1, and the obtained nanosheet is 1-2 nm in thickness and 3-30 microns in size.
Example 3
Steps (1) and (2) were the same as those in example 1.
(3) The liquid mixture was sonicated for 3 h at a power of 800W.
The steps (4) and (5) are the same as the operation steps in the embodiment 1, and the obtained nanosheet is 1-5 nm in thickness and 0.05-3 mu m in size.
Example 4
Steps (1), (2) and (3) were the same as those of example 1.
(4) Centrifuging the mixture after ultrasonic treatment for 20 min at 20000 rpm in a high speed (freezing) centrifuge, removing liquid phase medium, re-dissolving the precipitate with deionized water, and repeating the above centrifuging and re-dissolving operations for 6 times; centrifuging at 1500 rpm for 30 min to obtain Fe3GeTe2A nanosheet dispersion.
The step (5) is the same as the operation step of the embodiment 1, and the obtained nanosheet is 1-5 nm in thickness and 3-10 microns in size.
Example 5
(1) Weighing 1 g of Fe3GeTe2The crystals were placed in 1 mL DMF and ground for 1 h with a mortar.
(2) The milled mixture was dispersed and transferred to a beaker with 100 mL DMF at 80 ℃ at 700 rpm with stirring in a water (oil) bath or heating mantle for 24 h.
The steps (3), (4) and (5) are the same as the operation steps in the embodiment 1, and the obtained nanosheet is 1-5 nm in thickness and 10-30 microns in size.
Example 6
(1) Weighing 1 g of Fe3GeTe2The crystals were taken up in 1 mL of DMF and ground for 0.5h with a mortar.
(2) The milled mixture was dispersed and transferred to a beaker with 100 mL DMF at 80 ℃ at 700 rpm with stirring in a water (oil) bath or heating mantle for 18 h.
(3) The liquid mixture was sonicated at 300W for 1.5 h.
The steps (4) and (5) are the same as the operation steps in the embodiment 1, and the obtained nanosheet is 5-30 nm in thickness and 10-30 microns in size.
The invention provides a two-dimensional material Fe3GeTe2The preparation method of the nanosheet mainly comprises the following steps: fe3GeTe2Grinding the crystals in a liquid medium; transferring the ground mixture into a certain amount of same liquid phase medium, heating and stirring; subjecting the stirred mixture to ultrasonic treatment; centrifugal classificationTo obtain Fe3GeTe2A two-dimensional nanosheet dispersion; freeze drying to obtain Fe3GeTe2Two-dimensional nanosheet powder. The invention overcomes the defects that the prior art still stays in a mechanical stripping stage, wastes time and labor and cannot be produced in mass. Compared with the prior art, the method has the following advantages: (1) the process is simple, and the preparation period is short; (2) macro preparation can be realized; (3) can prepare Fe with controllable thickness3GeTe2Nanosheets, mainly concentrated in single, few and multi-layer ranges; (4) can prepare Fe with controllable size3GeTe2Nanosheets, having a size in the range of nanometers to micrometers; (5) preparation of the resulting Fe3GeTe2Few defects of the nano-sheet are generated, and the crystal structure is completely reserved. The method is simple and feasible, and can greatly promote Fe3GeTe2Research and application of materials.
Claims (10)
1. Two-dimensional material Fe3GeTe2The preparation method of the nanosheet is characterized by comprising the following steps:
1) mixing Fe3GeTe2Grinding the crystal in a liquid phase medium with surface tension for 10 min-24 h;
2) transferring the ground mixture into the same liquid phase medium for stirring, wherein the stirring speed is 100-3000 rpm, the temperature is between room temperature and 80 ℃, and the time is 1-72 h;
3) carrying out ultrasonic treatment on the stirred mixture, wherein the ultrasonic power is 30-2000W, and the ultrasonic treatment time is 10 min-15 h;
4) centrifuging and cleaning the liquid phase medium of the mixture subjected to ultrasonic treatment at a high rotating speed, wherein the centrifugal rotating speed for cleaning the liquid phase medium is 5000-; then, centrifugally separating the two-dimensional nano-sheets at a low rotating speed, wherein the centrifugal rotating speed for separating the nano-sheets is 300-3000 rpm, and the centrifugal time is 10 min-2 h to obtain Fe3GeTe2A two-dimensional nanosheet dispersion;
5) freeze-drying the nanosheet dispersion, and freezing the nanosheet dispersion for 10 min-2 h; vacuum drier cold trap-50-90oC, the vacuum degree is 2-20 Pa, and the drying time is 1-6 days; to obtain Fe3GeTe2Two-dimensional nanosheet powder.
2. The method according to claim 1, wherein Fe is used in step 1)3GeTe2Quality of the crystal: the volume ratio of the liquid phase medium is as follows: 1:1-300, g/mL; the surface tension of the liquid-phase medium is 10-100 mN.m-1。
3. The method of claim 1, wherein the liquid medium is N-methylpyrrolidone (NMP), N-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), ethanol (EtOH), Acetonitrile (ACN), N-Hexane (HEX), Acetone (ACE), Toluene (TOL), or the like.
4. The production method according to claim 1, wherein the mass ratio of the volume of the liquid phase medium to the crystal raw material used in the step 2) is 1:0.01 to 10, L/g.
5. The production method according to claim 1, characterized in that in step 1): fe3GeTe2Quality of the crystal: the volume ratio of the liquid phase medium is as follows: 1:1-20, g/mL.
6. The production method according to claim 1, wherein the mass ratio of the volume of the liquid phase medium to the crystal raw material used in step 2) is 1:0.01 to 1L/g; the stirring speed is 300-1300 rpm, the temperature is 40-60 ℃, and the time is 5-60 h.
7. The method as claimed in claim 1, wherein the ultrasonic power in step 3) is 300-1500W and the time is 30 min-8 h.
8. The method according to claim 1, wherein the centrifugation speed for washing the liquid phase medium in the step 4) is 10000-; the centrifugal rotating speed for separating the nano-sheets in the step 4) is 500-2000 rpm, and the centrifugal time is 30 min-1 h.
9. The method of preparation according to claim 1, characterized in that step 5) the nanoplatelet dispersion is frozen for 0.5-1.5 h; the vacuum drier cold trap in the step 5) is-60 to-80oC, vacuum degree is 2-10 Pa, and drying time is 2-5 days.
10. Fe obtained by the production method according to any one of claims 1 to 93GeTe2A two-dimensional nanoplatelet material.
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Cited By (3)
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| CN113667934A (en) * | 2021-07-20 | 2021-11-19 | 杭州电子科技大学 | Two-dimensional magnetic composite material with controllable magnetism and preparation method thereof |
| CN113839295A (en) * | 2021-09-02 | 2021-12-24 | 山东大学 | Laser pulse modulator based on BiOCl crystal and application thereof in all-solid-state laser |
| CN114361289A (en) * | 2022-01-10 | 2022-04-15 | 北京工业大学 | Construction method of self-driven ultrafast photoelectric detector based on van der Waals metal electrode |
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| CN114361289A (en) * | 2022-01-10 | 2022-04-15 | 北京工业大学 | Construction method of self-driven ultrafast photoelectric detector based on van der Waals metal electrode |
| CN114361289B (en) * | 2022-01-10 | 2024-03-15 | 北京工业大学 | Construction method of self-driven ultra-fast photoelectric detector based on van der Waals metal electrode |
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