CN102190296A - Hydrothermal method for preparing water-soluble graphene quantum dots - Google Patents
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Abstract
The invention discloses a hydrothermal method for preparing water-soluble graphene quantum dots. The invention relates to the preparation method of graphene quantum dots, and especially relates to a hydrothermal method for preparing water-soluble graphene quantum dots. The method provided by the present invention is characterized in that: 0.01 to 1.0M of an aqueous solution of polyhydroxyl carbohydrate is added to a hydrothermal reaction vessel; the aqueous solution is heated for 10 to 600 minutes under a temperature of 120 to 220 DEG C; sugar molecules are polymerized into graphene quantum dots with sizes of 1 to 10nm, such that target products are obtained. The graphene quantum dots prepared with the method provided by the present invention has characteristics of water-solubility, monodispersity and special photoelectrical characteristics. The raw materials are cheap, and the sources of the raw materials are wide. With environmental-protective technology, the method is suitable for volume production.
Description
Technical field
The present invention relates to the technology of preparing of graphene quantum dot, especially a kind of hydrothermal preparation technology of water-soluble graphene quantum dot.
Background technology
Graphene is a class carbon-based material, and carbon atom is with sp
2It is the two dimensional surface film of the cellular crystalline network of hexangle type of 0.142nm that the hydridization form is formed the bond distance.The technology of preparing of Graphene mainly contains tape stripping method, chemical Vapor deposition process, SiC heating method, graphene oxide reduction method etc., every kind of technology of preparing all has relative merits, and wherein the chemical Vapor deposition process technology is the major technique for preparing the big area single-layer graphene at present.Because Graphene is the special carbon material of a class, its special electricity, optics, calorifics, mechanical property demonstrate important potential using value at aspects such as transistor, unit molecule gas detection, unicircuit, transparency conductive electrode, biological device, ultracapacitor and power electric couplers at present.Yet the semi-metal of Graphene zero can limit its application at photoelectric field with character.Recently, Rice Univ USA (Rice University) studies show that graphene quantum dot can be realized the unit molecule transmitter.Professor Li Shutang of City University of Hong Kong (CityU) leader's group has also prepared the carbon quantum dot with electrochemical method, and has observed the photoluminescence phenomenon of carbon quantum dot.At present, the breakthrough that obtains about the preparation and the photoelectric property research of graphene quantum dot is indicating that also it is openable that Graphene can be with in the world, and has huge using value.
Existingly open the technology that Graphene can be with and mainly contain two kinds of methods, the firstth, introduce size and quantum confined effect, form nano belt or quantum dot; The secondth, chemical doping.Many breakthrough important research are being done aspect the preparation of graphene nanobelt and the applied research by professor Dai Hongjie of Stanford Univ USA leader's research group, they have all realized the graphene nanobelt of certain width with multinomial technology, have up to 10 based on the field-effect transistor of graphene nanobelt preparation
7The on-off ratio of the order of magnitude, these researchs have shown that fully Graphene can be with the importance of cutting.
Water-soluble graphene quantum dot is a kind of graphene quantum dot that can dissolve or be dispersed in the water.By the control preparation condition, can prepare dispersed narrower quantum dot.Because the existence of quantum confined effect, graphene quantum dot has certain energy gap, has characteristic of semiconductor such as tangible photoabsorption and photoluminescence property.It can be widely used in aspects such as biological fluorescent labelling, opto-electronic device, over capacity battery, advanced composite material.
Summary of the invention
The present invention solves present Graphene can be with and be difficult for opening, do not have problems such as the difficult modulation of semiconductor property, optics and electric property, by shrink polyreaction by glycan molecule under the hydrothermal condition, and the water-soluble graphene quantum dot that preparation size is controlled.
The hydrothermal preparing process of a kind of water-soluble graphene quantum dot of the present invention, it is characterized in that this method is the aqueous solution that adds 0.01～1.0M poly-hydroxy carbohydrate in hydrothermal reaction kettle, under 120～220 ℃ of temperature, heated 10～600 minutes, allow glycan molecule shrink to aggregate into the graphene quantum dot that is of a size of 1～10nm and be prepared into.
Described poly-hydroxy carbohydrate is glucose, sucrose or fructose.
The poly-hydroxy carbohydrate is a reactant among the described preparation method, and water is solvent, and reaction system is a sealing system.
The graphene quantum dot that inventive method is prepared into is the zero dimension grapheme material that a kind of three dimensions all are subjected to the quantum confinement effect, and its particle size range is 1.0～10nm, has following characteristics:
1, water-soluble, graphene quantum dot can disperse, be dissolved in the water, forms stable graphene quantum dot dispersion system.
2, monodispersity, the median size of the graphene quantum dot of preparation are 2.3nm, and it is narrow that quantum dot is evenly distributed size, can obtain the quantum dot solution of controllable size by control quantum dot synthesis condition.
3, raw material sources are extensive and cheap, and the raw material of use is a sugar, as poly-hydroxy carbohydrate such as glucose, sucrose, fructose.
4, technology environmental protection, preparation technology's one-step synthesis does not relate to processes such as the preparation of intermediate and purifying.
5, be easy to produce in batches, only need high voltage bearing hydrothermal reaction kettle just can finish preparation technology.
6, special photoelectric characteristic, graphene quantum dot has semiconductor property, has characteristics such as photoabsorption, photoluminescence, field-effect, can be widely used at optoelectronic areas.
Description of drawings
Fig. 1 is the graphene quantum dot for preparing under the different heating time conditions.
Fig. 2 is the UV, visible light optical absorption spectra of graphene quantum dot.
Fig. 3 is the low enlargement ratio TEM figure of graphene quantum dot.
Fig. 4 is the high enlargement ratio TEM figure of graphene quantum dot.
Fig. 5 is the graphene quantum dot high-resolution-ration transmission electric-lens figure that contains the Graphene lattice fringe.
Fig. 6 is the electron-diffraction diagram of graphene quantum dot 101 diffraction rings.
Fig. 7 is that mean sizes is the graphene quantum dot size distribution statistical graph of 2.3nm.
Embodiment
Embodiment 1: preparation 0.5M D/W, in the polytetrafluoroethyllining lining container of hydrothermal reaction kettle, add 40ml solution, cover tight lid and form enclosed space, reactor is put in 190 ℃ the stove, heated 120 minutes, and promptly obtained the graphene quantum dot that mean sizes is 2.3nm.
Embodiment 2: preparation 0.01M aqueous sucrose solution, get 40ml solution in reactor, and cover tight lid and form enclosed space, reactor is put in 220 ℃ the stove, heated 600 minutes.Obtain the graphene quantum dot that mean sizes is 4.3nm.
Embodiment 3: preparation 1.0M fructose water solution, the solution of getting certain volume cover tight lid and form enclosed space in reactor, reactor are put in 150 ℃ the stove, heat 120 minutes.Obtain the graphene quantum dot that mean sizes is 3.8nm.
Embodiment 4: preparation 0.01M D/W, the solution of getting certain volume cover tight lid and form enclosed space in reactor, reactor are put in 200 ℃ the stove, heat 500 minutes.Obtain the graphene quantum dot that mean sizes is 3.5nm.
Embodiment 5: preparation 1.0M fructose water solution, the solution of getting certain volume cover tight lid and form enclosed space in reactor, reactor are put in 120 ℃ the stove, heat 120 minutes.Obtain the graphene quantum dot that mean sizes is 2.0 nm.
Embodiment 6: preparation 0.01M D/W, the solution of getting certain volume cover tight lid and form enclosed space in reactor, reactor are put in 220 ℃ the stove, heat 10 minutes.Obtain the graphene quantum dot that mean sizes is 1.6 nm.
Claims (3)
1. the hydrothermal preparing process of a water-soluble graphene quantum dot, it is characterized in that this method is the aqueous solution that adds 0.01～1.0M poly-hydroxy carbohydrate in hydrothermal reaction kettle, under 120～220 ℃ of temperature, heated 10～600 minutes, allow glycan molecule shrink to aggregate into the graphene quantum dot that is of a size of 1～10nm and be prepared into.
2. the hydrothermal preparing process of a kind of water-soluble graphene quantum dot as claimed in claim 1 is characterized in that described poly-hydroxy carbohydrate is glucose, sucrose or fructose.
3. the hydrothermal preparing process of a kind of water-soluble graphene quantum dot as claimed in claim 1 is characterized in that the poly-hydroxy carbohydrate is a reactant among the described preparation method, and water is solvent, and reaction system is a sealing system.
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