CN105668530A - Preparation method of two-dimensional nanomaterial - Google Patents
Preparation method of two-dimensional nanomaterial Download PDFInfo
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- CN105668530A CN105668530A CN201610023583.9A CN201610023583A CN105668530A CN 105668530 A CN105668530 A CN 105668530A CN 201610023583 A CN201610023583 A CN 201610023583A CN 105668530 A CN105668530 A CN 105668530A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a preparation method of a two-dimensional nanomaterial. The method comprises the following steps: mixing a certain amount of a material with a layered structure with lithium chloride and aluminium chloride particles, heating and carrying out thermal insulation and cooling and carrying out thermal insulation for many times to repeatedly melt and freeze a salt mixture under a certain condition while intercalation and stripping of a material with a layered structure are continuously carried out during the process, and finally washing, separating and drying the sample so as to obtain the two-dimensional nanomaterial. The preparation method has advantages of low cost and simple process, no complex equipment is required, and the preparation method is green and environmentally friendly. Due to physical stripping, a prepared sample has complete crystallinity and is suitable for scientific research and industrial production.
Description
Technical field
The present invention relates to field of material technology, the preparation method being specifically related to a kind of two-dimension nano materials.
Background technology
Graphene (Graphene) is the Two-dimensional Carbon material with cellular atomic structure and monolayer atomic thickness. Its discovery not only broken for a long time two dimensional crystal cannot in nature the prophesy of stable existence, the excellent properties of himself also makes Graphene all great potential in basic and applied research. Up to the present, have hundreds of two-dimensional material quilt it has been found that this includes the 4th main group simple substance, the binary compound that the 3rd and the 5th main group is constituted, metal chalcogenide compound, composite oxides, etc. The two-dimension single layer accumulation that this kind of material is only several atom by thickness forms, and is van der Waals effect between layers. In the traditional view of people, when the number of plies of this kind of stratified material is progressively reduced until in the process of monolayer, its electronic structure and physical property tend to occur very big change, and such as band gap width enlarges markedly, indirect band gap changes to direct band gap, and the change of crystal vibration energy etc. Especially the existence of dirac cone (Diraccone) imparts physical phenomenon and the electronic property of the many novelties of Graphene, for instance half-integer, mark and fractal quantum hall effect, superelevation mobility etc.
But preparing now the method difficulty of these two-dimensional material, means are limited, are mostly other milligram of magnitude of laboratory-scale, also have very remote distance from laboratory applications test or production. Therefore developing a kind of convenient, environmental protection, pervasive preparation means not only to production, also that scientific research is particularly important, the present invention comes therefrom.
Summary of the invention
The preparation method that the technical problem to be solved is to provide a kind of convenient, environmental protection, pervasive convenient, environmental protection, pervasive two-dimension nano materials.
In order to solve above-mentioned technical problem, the preparation method of a kind of two-dimension nano materials provided by the invention, a certain amount of material with layer structure is mixed by (1) with lithium chloride and aluminum chloride granule,
(2) it is incubated the salt-mixture making lithium chloride and aluminum chloride thawing and solidification repeatedly under certain atmosphere after insulation and cooling after then passing through intensification repeatedly, there is the material of layer structure in the process constantly by intercalation and stripping,
(3) final sample separates dried through washing, obtains two-dimension nano materials.
It is 0.5%～10% that the described a certain amount of material with layer structure accounts for the salt-mixture mass ratio of lithium chloride and aluminum chloride granule, it is preferable that mass ratio is 0.5%～5%.
The described material with layer structure refers to graphite, graphite oxide, expanded graphite, hexagonal boron nitride, molybdenum bisuphide, tungsten disulfide, rhenium disulfide, black phosphorus, 4th main group simple substance, the binary compound that the 3rd and the 5th main group is constituted, metal sulfide, layered lithium manganate, stratiform cobalt acid lithium stratified material and with the above-mentioned doping vario-property material for material of main part.
The molar ratio of described lithium chloride and aluminum chloride is 1:0.9～1.1.
Mixing in described step (1) refers to grinding, stirs, shakes, rocks mode.
Described step (2) repeatedly refers to 5～100 times, it is preferable that 20～50 times.
After intensification in described step (2), insulation refers to that being warmed up to 144 DEG C～200 DEG C starts insulation, heating rate is 0.1～100 DEG C/s, temperature retention time is 1～60 minute, preferably it is warmed up to 144 DEG C～180 DEG C and starts insulation, preferred heating rate is 1～10 DEG C/s, it is preferable that temperature retention time is 10～30 minutes.
After cooling in described step (2), insulation refers to that cooling to-60 DEG C～140 DEG C starts insulation, and rate of temperature fall is 0.1～100 DEG C/s, and temperature retention time is 1～60 minute; Preferably cool to 0 DEG C～80 DEG C and start insulation, it is preferable that rate of temperature fall is 1～10 DEG C/s, it is preferable that temperature retention time is 10～30 minutes.
Described atmosphere be selected from vacuum, air, oxygen, hydrogen, nitrogen, noble gas, oxidizing gas, reducibility gas, sour gas, one or more in alkaline gas, it is preferable that atmosphere be air, hydrogen, nitrogen one or more; Relative pressure is 0～10MPa.
A second aspect of the present invention provides the two-dimension nano materials that a kind of said method prepares.
Described two-dimension nano materials is the number of plies is 1～20 layer, and thickness is 0～10nm.
The invention has the beneficial effects as follows: compared with prior art, the present invention obtains ionic liquid after common low cost indifferent salt utilizes eutectic point melted, lithium ion, aluminium ion, chloride ion all has less ionic radius, it is easily accessible the formation intercalation between layers of layer structure material, fuse salt crystallization and freezing is made afterwards by cooling, ionic crystal growth in intercalation thus supportting big by interlamellar spacing, repeatedly repeating this process makes interlamellar spacing constantly support greatly, stratified material is completely exfoliated the most at last, and obtains two-dimension nano materials by process such as washings. The preparation method technique of the present invention is simple, and processing ease is with low cost, it is not necessary to complex device, and environmental protection; Peel off because the inventive method is Physical, so the two-dimension nano materials prepared has intact crystallinity, be suitable for research application and industrialized production.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the graphene nanometer sheet prepared by the embodiment of the present invention 1.
The scanning electron microscope (SEM) photograph of the hexagonal boron nitride nanosheet prepared by Fig. 2 position embodiment of the present invention 3.
Detailed description of the invention:
For being further appreciated by the present invention, below in conjunction with specific embodiment, preferred version of the present invention is described, but it is to be understood that these describe simply as further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
Embodiment 1
5g graphite flake is mixed with 100g lithium chloride and aluminum chloride powder (mol ratio 1:1) by grinding, mixed sample heats to 200 DEG C with the heating rate of 1 DEG C/s under air normal pressure and is incubated 600 seconds and makes mixture melt, it is cooled to 80 DEG C with the rate of temperature fall of 1 DEG C/s afterwards and is incubated 1200 seconds and makes mixture solidify, after repeating this melting and solidification process 50 times, dry run is separated by washing, thus obtaining the thick graphene nanometer sheet of 3nm, as shown in Figure 1.
Embodiment 2
0.1g black phosphorus is mixed with 100g lithium chloride and aluminum chloride powder (mol ratio 1:1) by stirring, mixed sample heats to 180 DEG C with the heating rate of 80 DEG C/s under vacuo and is incubated 600 seconds and makes mixture melt, it is cooled to 100 DEG C with the rate of temperature fall of 1 DEG C/s afterwards and is incubated 600 seconds and makes mixture solidify, after repeating this melting and solidification process 20 times, dry run is separated, thus obtaining black phosphorus nanometer sheet by washing.
Embodiment 3
2g hexagonal boron nitride is mixed with 100g lithium chloride and aluminum chloride powder (mol ratio 1:1) by shaking, mixed sample heats to 160 DEG C with the heating rate of 10 DEG C/s under air normal pressure and is incubated 3000 seconds and makes mixture melt, it is cooled to 20 DEG C with the rate of temperature fall of 10 DEG C/s afterwards and is incubated 3000 seconds and makes mixture solidify, after repeating this melting and solidification process 20 times, dry run is separated by washing, thus obtaining the thick hexagonal boron nitride nanosheet of 5nm, as shown in Figure 2.
Embodiment 4
1g molybdenum bisuphide is mixed with 100g lithium chloride and aluminum chloride powder (mol ratio 1:1) by shaking; mixed sample heats to 160 DEG C with the heating rate of 5 DEG C/s under nitrogen protection and is incubated 1800 seconds and makes mixture melt; it is cooled to 50 DEG C with the rate of temperature fall of 5 DEG C/s afterwards and is incubated 1800 seconds and makes mixture solidify; after repeating this melting and solidification process 20 times; dry run is separated, thus obtaining molybdenum disulfide nano sheet by washing.
Embodiment 5
0.5g tungsten disulfide is mixed with 100g lithium chloride and aluminum chloride powder (mol ratio 1:1) by shaking; mixed sample heats to 160 DEG C with the heating rate of 5 DEG C/s under reducing atmosphere (5% hydrogen nitrogen blender) is protected and is incubated 1800 seconds and makes mixture melt; it is cooled to 50 DEG C with the rate of temperature fall of 5 DEG C/s afterwards and is incubated 1800 seconds and makes mixture solidify; after repeating this melting and solidification process 20 times; dry run is separated, thus obtaining tungsten disulfide nano slices by washing.
The technology contents of the present invention and technical characteristic have revealed that as above; but those of ordinary skill in the art are still potentially based on teachings of the present invention and announcement and do all replacements without departing substantially from spirit of the present invention and modification; therefore; scope should be not limited to the content that embodiment is disclosed; and the various replacement without departing substantially from the present invention and modification should be included, and contained by present patent application claim.
Claims (10)
1. the preparation method of a two-dimension nano materials, it is characterised in that its method comprises the steps:
(1) a certain amount of material with layer structure is mixed with lithium chloride and aluminum chloride granule,
(2) it is incubated the salt-mixture making lithium chloride and aluminum chloride thawing and solidification repeatedly under certain atmosphere after insulation and cooling after then passing through intensification repeatedly, there is the material of layer structure in the process constantly by intercalation and stripping,
(3) final sample separates dried through washing, obtains two-dimension nano materials.
2. the preparation method of two-dimension nano materials according to claim 1, it is characterised in that described in there is the material of layer structure to account for the salt-mixture mass ratio of lithium chloride and aluminum chloride granule be 0.5%～10%.
3. the preparation method of two-dimension nano materials according to claim 1, it is characterised in that described in there is the material of layer structure refer to graphite, graphite oxide, expanded graphite, hexagonal boron nitride, molybdenum bisuphide, tungsten disulfide, rhenium disulfide, black phosphorus, 4th main group simple substance, the binary compound that the 3rd and the 5th main group is constituted, metal sulfide, layered lithium manganate, stratiform cobalt acid lithium stratified material and with the above-mentioned doping vario-property material for material of main part.
4. the preparation method of two-dimension nano materials according to claim 1, it is characterised in that the molar ratio of described lithium chloride and aluminum chloride is 1:0.9～1.1.
5. the preparation method of two-dimension nano materials according to claim 1, it is characterised in that repeatedly refer to 5～100 times in described step (2).
6. the preparation method of two-dimension nano materials according to claim 1, it is characterized in that, after intensification in described step (2), insulation refers to that being warmed up to 144 DEG C～200 DEG C starts insulation, and heating rate is 0.1～100 DEG C/s, and temperature retention time is 1～60 minute.
7. the preparation method of two-dimension nano materials according to claim 1, it is characterized in that, after cooling in described step (2), insulation refers to that cooling to-60 DEG C～140 DEG C starts insulation, and rate of temperature fall is 0.1～100 DEG C/s, and temperature retention time is 1～60 minute.
8. the preparation method of two-dimension nano materials according to claim 1, it is characterised in that described atmosphere is selected from vacuum, air, oxygen, hydrogen, nitrogen, noble gas, oxidizing gas, reducibility gas, sour gas, one or more in alkaline gas; Relative pressure is 0～10MPa.
9. a two-dimension nano materials, its method described in any one of claim 1-9 prepares.
10. two-dimension nano materials according to claim 9, it is characterised in that described two-dimension nano materials is the number of plies is 1～20 layer, and thickness is 0～10nm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082148A (en) * | 2016-06-21 | 2016-11-09 | 江苏大学 | A kind of method utilizing liquid nitrogen gasification preparation two dimension hexagonal boron nitride nanosheet |
| CN106335927A (en) * | 2016-08-22 | 2017-01-18 | 河南师范大学 | Method for preparing 2H phase single layer tungsten disulfide nano sheet |
| CN106841338A (en) * | 2017-01-25 | 2017-06-13 | 东南大学 | A kind of gas sensor and preparation method thereof |
| CN107039587A (en) * | 2017-03-31 | 2017-08-11 | 东南大学 | Negative differential resistance and preparation method based on black phosphorus/rhenium disulfide hetero-junctions |
| CN109368703A (en) * | 2018-11-15 | 2019-02-22 | 厦门大学 | A kind of tungstic acid preparation of sections method |
| CN111151145A (en) * | 2018-11-08 | 2020-05-15 | 中国石油化工股份有限公司 | Super-hydrophobic separation membrane and preparation method and application thereof |
| CN111547770A (en) * | 2020-06-05 | 2020-08-18 | 中国科学技术大学 | Preparation method of functionalized modified molybdenum disulfide nanosheet |
| CN116169012A (en) * | 2023-04-26 | 2023-05-26 | 南京理工大学 | Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082148B (en) * | 2016-06-21 | 2018-04-20 | 江苏大学 | A kind of method that two-dimentional hexagonal boron nitride nanosheet is prepared using liquid nitrogen gasification |
| CN106082148A (en) * | 2016-06-21 | 2016-11-09 | 江苏大学 | A kind of method utilizing liquid nitrogen gasification preparation two dimension hexagonal boron nitride nanosheet |
| CN106335927A (en) * | 2016-08-22 | 2017-01-18 | 河南师范大学 | Method for preparing 2H phase single layer tungsten disulfide nano sheet |
| CN106841338A (en) * | 2017-01-25 | 2017-06-13 | 东南大学 | A kind of gas sensor and preparation method thereof |
| CN107039587A (en) * | 2017-03-31 | 2017-08-11 | 东南大学 | Negative differential resistance and preparation method based on black phosphorus/rhenium disulfide hetero-junctions |
| CN111151145A (en) * | 2018-11-08 | 2020-05-15 | 中国石油化工股份有限公司 | Super-hydrophobic separation membrane and preparation method and application thereof |
| CN111151145B (en) * | 2018-11-08 | 2022-04-05 | 中国石油化工股份有限公司 | Super-hydrophobic separation membrane and preparation method and application thereof |
| CN109368703B (en) * | 2018-11-15 | 2020-01-07 | 厦门大学 | Preparation method of tungsten trioxide thin sheet |
| CN109368703A (en) * | 2018-11-15 | 2019-02-22 | 厦门大学 | A kind of tungstic acid preparation of sections method |
| CN111547770A (en) * | 2020-06-05 | 2020-08-18 | 中国科学技术大学 | Preparation method of functionalized modified molybdenum disulfide nanosheet |
| CN111547770B (en) * | 2020-06-05 | 2021-05-07 | 中国科学技术大学 | Preparation method of functionalized modified molybdenum disulfide nanosheet |
| CN116169012A (en) * | 2023-04-26 | 2023-05-26 | 南京理工大学 | Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity |
| CN116169012B (en) * | 2023-04-26 | 2023-08-08 | 南京理工大学 | Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity |
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