CN104310382A - Preparation method for graphene nanometer screen - Google Patents
Preparation method for graphene nanometer screen Download PDFInfo
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- CN104310382A CN104310382A CN201410514040.8A CN201410514040A CN104310382A CN 104310382 A CN104310382 A CN 104310382A CN 201410514040 A CN201410514040 A CN 201410514040A CN 104310382 A CN104310382 A CN 104310382A
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Abstract
The invention relates to a preparation method for a graphene nanometer screen. The preparation method comprises the following steps: preparing a graphene oxide (GO) aqueous solution by adopting a Hummers method firstly, freezing the GO aqueous solution with a certain concentration in a freezing chamber of a refrigerator to obtain a GO ice block; then preliminarily crushing the ice block into small blocks, putting in a pipe, and freeze-grinding the GO ice blocks in the presence of liquid nitrogen by adopting a freeze-grinding machine; and cooling to room temperature to obtain a GNMs aqueous solution, and carrying out a series of structure characterization. As no chemical reaction happens and no agent is needed in the whole preparation process, the preparation method is a physical method without any pollution and damage to the environment, the preparation method is a true environmental-friendly preparation method. In addition, the preparation method is simple and feasible in operation process, good in repeatability, rich in raw material source and low in cost and has good application prospect.
Description
Technical field
The invention belongs to field of graphene, particularly the preparation method that sieves of a kind of graphene nano.
Background technology
The structure of Graphene because of its uniqueness and the performance of excellence, at nano electron device, nano composite material, chemistry and biosensor, the numerous areas such as solar cell have very large application potential.But the zero band gap semi-metal behavior due to Graphene limits the application of its scene effect transistor aspect.A lot of research shows, the Graphene of zero band gap cuts into graphene nanobelt can open band gap to meet its transistor application at room temperature, but the FET device of single nano belt shows very low drive current and mutual conductance.In addition, actual practical device and circuit often require intensive and orderly nano belt, and this is concerning remaining a large challenge graphene nanobelt at present.
Graphene nano sieve (Graphene nanomeshes, GNMs), another kind of new graphene nano structure, can regard as, on a large graphene film, band gap be opened formation semiconductor film.GNMs has the extensive concern that peculiar stuctures and properties has caused people, open band gap, the specific surface area of expansion, the character such as high light transmission rate, make it at semiconductor devices, photochemical catalysis, all there is good application prospect in the fields such as sensor and energy related system.Compared with Graphene, the periodicity on GNMs or the nanoporous of psuedo-periodicity make it have more avtive spot and edge, thus have the electro catalytic activity of electric transmission and Geng Gao faster.At present, the preparation method of GNMs is mainly through segmented copolymer photoetching, and plasma etching, photochemical catalytic oxidation and chemical vapour deposition, but these methods can only prepare a small amount of GNMs, and these methods all costly, process is loaded down with trivial details.Recently, Qu proposes solution oxide legal system for GNMs and three-dimensional GNMs foam, but in preparation process, relate to many chemical steps, used reagent can be unfriendly to environment.Therefore, developing new method to prepare GNMs is a problem demanding prompt solution.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of a kind of graphene nano sieve (GNMs), and the method operating procedure is simple, and reproducible, abundant raw material source, cost is low, has a good application prospect.
The preparation method of a kind of graphene nano sieve GNMs of the present invention, concrete steps are expressed as follows:
(1) first, adopt Hummers legal system for the graphene oxide GO aqueous solution, the GO aqueous solution is placed on and carries out freezing in freezer compartment of refrigerator, obtain GO ice cube;
(2) then, ice cube is tentatively broken into fritter and loads in pipe, adopt refrigeration grinding machine, under liquid nitrogen condition, GO ice cube is carried out freeze grinding, obtain graphene nano sieve.
The concentration of the GO aqueous solution in described step (1) is 0.01mg/ml ~ 0.5mg/ml.
Freezing time in described step (1) in refrigerator cold-storage is 2h ~ 24h.
Freezing temp in described step (1) in refrigerator cold-storage is-7 DEG C ~-30 DEG C.
The freeze grinding time of the GO ice cube in described step (2) is 30min ~ 360min.
The preparation method that the present invention proposes adopts freeze grinding technology, under condition of ultralow temperature, fast the fragmentation of GO ice can be formed irregular icicle, on the surface of GO sheet, many nano apertures are got under the effect of external force, there is not chemical reaction in whole preparation process, without any need for reagent, being belong to physical method, there is not any pollution and destruction to environment, is a kind of really environmentally friendly Green synthesis technology.
beneficial effect
The fragmentation of GO ice is formed irregular icicle fast by the present invention under condition of ultralow temperature, under the effect of external force, get many nano apertures on the surface of GO sheet, there is not chemical reaction in whole preparation process, without any need for reagent, belong to physical method, there is not any pollution and destruction to environment, be a kind of really environmentally friendly Green synthesis technology, the method operating procedure is simple, reproducible, abundant raw material source, cost is low, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) figure of the GO that embodiment 1 is original;
Fig. 2 is transmission electron microscope (TEM) figure of GNMs prepared by embodiment 1;
Fig. 3 a is Raman spectrum (Raman) figure of the GO that embodiment 2 is original;
Fig. 3 b is Raman spectrum (Raman) figure of GNMs prepared by embodiment 2;
Fig. 3 c is Raman spectrum (Raman) figure of GNMs prepared by embodiment 3;
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Adopt Hummers legal system for graphene oxide (GO) aqueous solution, being made into concentration is that the GO aqueous solution of 0.3mg/ml is placed in freezer compartment of refrigerator and carries out freezing 6h, obtains GO ice cube.Then ice cube being tentatively broken into fritter loads in pipe, and adopt refrigeration grinding machine, under liquid nitrogen condition, GO ice cube is carried out freeze grinding 2h by (-196 DEG C).Until the aqueous solution obtaining GNMs after normal temperature carries out a series of structural characterization.TEM sign is carried out to the GNMs prepared and original GO, the result obtained is as Fig. 1 and 2: after freeze grinding, there is many nano apertures in complete GO lamella, this is the irregular icicle of ice fragmentation formation of process of lapping, and under the effect of external force, icicle is beaten caused by the surface of GO sheet.
Embodiment 2
Adopt Hummers legal system for graphene oxide (GO) aqueous solution, being made into concentration is that the GO aqueous solution of 0.1mg/ml is placed in freezer compartment of refrigerator and carries out freezing 12h, obtains GO ice cube.Then ice cube being tentatively broken into fritter loads in pipe, and adopt refrigeration grinding machine, under liquid nitrogen condition, GO ice cube is carried out freeze grinding 1h by (-196 DEG C).Until the aqueous solution obtaining GNMs after normal temperature carries out a series of structural characterization.Carry out Raman sign to the GNMs prepared and original GO, the result obtained is as Fig. 3 a and 3b: after freeze grinding, and many nano apertures have appearred in complete GO lamella, result in the increase of GO surface imperfection, thus make the I of Fig. 3 b
d/ I
godds ratio Fig. 3 a is large, and this is also caused by freeze grinding process.
Embodiment 3
Adopt Hummers legal system for graphene oxide (GO) aqueous solution, being made into concentration is that the GO aqueous solution of 0.1mg/ml is placed in freezer compartment of refrigerator and carries out freezing 12h, obtains GO ice cube.Then ice cube being tentatively broken into fritter loads in pipe, and adopt refrigeration grinding machine, under liquid nitrogen condition, GO ice cube is carried out freeze grinding 3h by (-196 DEG C).Until the aqueous solution obtaining GNMs after normal temperature carries out a series of structural characterization.Carry out Raman sign to the GNMs of preparation, the result obtained is as Fig. 3 c: after freeze grinding time lengthening, and compared with embodiment 2, the surface imperfection increase of GO is more obvious, thus makes the I of Fig. 3 c
d/ I
godds ratio Fig. 3 b's is larger.
Embodiment 4
Adopt Hummers legal system for graphene oxide (GO) aqueous solution, being made into concentration is that the GO aqueous solution of 0.5mg/ml is placed in freezer compartment of refrigerator and carries out freezing 24h, obtains GO ice cube.Then ice cube being tentatively broken into fritter loads in pipe, and adopt refrigeration grinding machine, under liquid nitrogen condition, GO ice cube is carried out freeze grinding 6h by (-196 DEG C).Until the aqueous solution obtaining GNMs after normal temperature carries out a series of structural characterization.
Claims (5)
1. a preparation method of graphene nano sieve GNMs, concrete steps are expressed as follows:
(1) first, adopt Hummers legal system for the graphene oxide GO aqueous solution, the GO aqueous solution is placed on and carries out freezing in freezer compartment of refrigerator, obtain GO ice cube;
(2) then, ice cube is tentatively broken into fritter and loads in pipe, adopt refrigeration grinding machine, under liquid nitrogen condition, GO ice cube is carried out freeze grinding, obtain graphene nano sieve.
2. the preparation method of a kind of graphene nano sieve according to claim 1, is characterized in that: the concentration of the GO aqueous solution in described step (1) is 0.01mg/ml ~ 0.5mg/ml.
3. the preparation method of a kind of graphene nano sieve according to claim 1, is characterized in that: the freezing time in described step (1) in refrigerator cold-storage is 2h-24h.
4. the preparation method of a kind of graphene nano sieve according to claim 1, is characterized in that: the freezing temp in described step (1) in refrigerator cold-storage is-7 DEG C ~-30 DEG C.
5. the preparation method of a kind of graphene nano sieve according to claim 1, is characterized in that: the freeze grinding time of the GO ice cube in described step (2) is 30min ~ 360min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986333A (en) * | 2017-05-25 | 2017-07-28 | 华中科技大学 | A kind of method that magnanimity controllable preparation graphene nano sieves material |
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| JPS61127612A (en) * | 1984-11-26 | 1986-06-14 | Agency Of Ind Science & Technol | Production of electrically-conductive graphite material |
| CN103058179A (en) * | 2013-01-21 | 2013-04-24 | 张家港市东大工业技术研究院 | Method for preparing spongy graphene oxide by using freeze-drying method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61127612A (en) * | 1984-11-26 | 1986-06-14 | Agency Of Ind Science & Technol | Production of electrically-conductive graphite material |
| CN103058179A (en) * | 2013-01-21 | 2013-04-24 | 张家港市东大工业技术研究院 | Method for preparing spongy graphene oxide by using freeze-drying method |
Non-Patent Citations (1)
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| GUOQING NING ET AL.: "Synthesis and methane storage of binder-free porous graphene monoliths", 《PARTICUOLOGY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986333A (en) * | 2017-05-25 | 2017-07-28 | 华中科技大学 | A kind of method that magnanimity controllable preparation graphene nano sieves material |
| CN106986333B (en) * | 2017-05-25 | 2019-07-19 | 华中科技大学 | A kind of method of magnanimity controllable preparation graphene nano sieve material |
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Effective date of registration: 20170209 Address after: 212000 Zhenjiang Province New District Qinglong mountain road, No. 113, No. Patentee after: Tiannai (Zhenjiang) Material Technology Co., Ltd. Address before: 201620 Shanghai Songjiang new town, North Renmin Road, No. 2999, No. Patentee before: Donghua University |
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Address after: 212000 Zhenjiang Province New District Qinglong mountain road, No. 113, No. Patentee after: Jiangsu Nanai Polytron Technologies Inc Address before: 212000 Zhenjiang Province New District Qinglong mountain road, No. 113, No. Patentee before: Tiannai (Zhenjiang) Material Technology Co., Ltd. |
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