CN107572505A - A kind of preparation method of Ag doping graphene quantum dot - Google Patents

A kind of preparation method of Ag doping graphene quantum dot Download PDF

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Publication number
CN107572505A
CN107572505A CN201610516357.4A CN201610516357A CN107572505A CN 107572505 A CN107572505 A CN 107572505A CN 201610516357 A CN201610516357 A CN 201610516357A CN 107572505 A CN107572505 A CN 107572505A
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China
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quantum dot
graphene quantum
doping
doping graphene
preparation
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CN201610516357.4A
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Chinese (zh)
Inventor
李学铭
唐利斌
钱福丽
杨培志
马逊
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Yunnan University YNU
Yunnan Normal University
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Yunnan Normal University
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Abstract

A kind of preparation method of the graphene quantum dot of metallic element doping, belongs to technical field of nano material, and in particular to the Hydrothermal Synthesiss technology of preparing of Ag doping graphene quantum dot.The hydrothermal preparing process of a kind of Ag doping graphene quantum dot of the present invention, it is characterised in that sugar generates water-soluble metal Ag doping graphene quantum dot with silver acetate under hydrothermal reaction condition.The technology of the present invention is related to the introducing metal silver ion into graphene quantum dot, and the more excellent photoelectric properties of graphene quantum dot are realized by adjusting graphene quantum dot level structure.The preparation method process is easy, and the cost of raw material is low, equipment is simple, is advantageous to enterprise scale production, and obtained quantum dot good water solubility, fluorescence property is notable, there is important application value in fields such as photocatalysis, photoelectron, solar cell and chemical sensitisations.

Description

A kind of preparation method of Ag doping graphene quantum dot
Technical field
The present invention relates to a kind of preparation method of metal-silver-doped graphene quantum dot, by adding into graphene quantum dot Enter doped chemical silver, new level structure is introduced in graphene forbidden band, realizes that the band gap of graphene quantum dot is adjustable.The present invention Belong to technical field of nanometer material preparation.Preparation technology simplicity, safety, cost are low in the present invention, and product has good water solubility, glimmering The advantages that optical property is notable, size uniform.
Background technology
In recent years, a focus of the graphene as investigation of materials field, is constantly subjected to the favor of scientific research personnel.As stone A member of Mo Xi families, graphene quantum dot is except the excellent properties with graphene, also because quantum confined effect, surface are imitated Should, Dielectric confinement effect and show a series of new characteristics, therefore attracted each field such as chemistry, physics, material and biology The extensive concern of scientist.But the defects of its fluorescence quantum yield is not high, avtive spot is relatively fewer, limits to a certain extent Its application in practice, and then can solve these to a certain extent using exotic atom doped graphene quantum dot and ask Topic.
With deepening continuously for graphene research, some special performances that graphene low-dimensional materials are shown are also increasingly Attract attention.According to quantum confined effect, quantum size effect, edge effect scheduling theory, the various nano materials of graphene are striven Mutually occur, wherein, graphene quantum dot is graphene all restricted nano material in three dimensions, and it opens graphene Band gap, compensate for the shortcoming of the band gap of graphene zero.For the performance of further optimization graphene quantum dot, researcher is carried out to it Doping treatment, as a result obtain the adjustable graphene quantum dot of band gap.Graphene has been expanded in bio-imaging, microelectronics, function The broad development space in the fields such as material, chemical sensitisation, solar cell.
At present, the doped chemical research of graphene quantum dot is concentrated mainly on the nonmetalloids such as N, S, CL, F, Less to metal-doped research, the metal-doped performance that can effectively improve graphene at optically and electrically aspect, this is to stone The application and development of black alkene is significant.At this stage, the technology of preparing of nano material is broadly divided into two classes:" from top to bottom " " from bottom to top " method.The former is that directly large scale material is cut by a series of physics, chemistry and electrochemical process It is cut into as nano-scale;The latter focuses on chemical synthesis, is using some small molecules as presoma, is converted by chemically reacting For nano material." from top to bottom " method is due to being main at this stage with the advantage such as preparation technology is simple, production cost is low One of preparation method of nano material.
It is 201410362337.5 in number of patent application, entitled " Ag doping graphene extrusion coating paper and preparation method thereof " In Chinese patent, it is ultrasonically treated by raw material of graphene oxide, is adding nitric acid silver reaction, product must arrive silver through pervaporation Graphene oxide is adulterated, then Ag doping graphene is obtained by reduction treatment.It is entitled " a kind of nitrogen-doped graphene quantum dot Chemical preparation process "(Number of patent application is 201410376809.4)Chinese patent in, it is sweet by the use of graphite oxide as carbon source Nitrogen-doped graphene quantum dot is made as nitrogen source in propylhomoserin under high temperature annealing condition., this hair different from foregoing invention of the invention Bright technology, which is related to, prepares graphene quantum dot, and into graphene quantum dot introduce impurity element silver, using sugar and silver acetate as Raw material obtain Ag doping graphene quantum dot by hydro-thermal process, have good water solubility, size small and uniformly and fluoresce Etc. characteristic.
The content of the invention
The present invention realizes the easy of silver element doped graphene quantum dot with simple step chemical reaction and prepared, the gold The incorporation for belonging to element plays an important role to the modulation of graphene quantum dot level structure, while changes the properties of graphene. A kind of hydro-thermal synthetic preparation method of Ag doping graphene quantum dot in the present invention, using sugar and silver acetate as raw material, deionization Water is solvent, and water-soluble metal Ag doping graphene quantum dot is prepared with reaction under pressure at a certain temperature.
The present invention Ag doping graphene quantum dot hydro-thermal synthetic preparation method, it is characterised in that this method be by with Under step realize:The first step, proper amount of sugar and silver acetate solid are taken, add deionized water stirring it is fully dissolved;Second step, The solution that the first step configures is transferred in hydrothermal reaction kettle, isothermal reaction a few hours;3rd step, after reaction terminates, take product Carry out dialysis purification, you can obtain the aqueous solution of Ag doping graphene quantum dot.
Wherein, the sugar described in the first step can be any one in fructose, glucose or sucrose, and sugared dosage is 0.5 gram, 0.2 gram of silver acetate, 40 milliliters of deionized water.
Wherein, the solution prepared is transferred in hydrothermal reaction kettle by second step, and reactor is placed in 170 DEG C of constant temperature oven Middle reaction, time are 4 hours.
Wherein, the 3rd step takes out reaction solution bag filter dialysis purification, and dialysis time is 10~20 minutes.
Ag doping graphene quantum dot effectively increases the electronic transition energy of graphene while graphene band gap is opened Level., will be in sp by toward metal silver ion is mixed in graphene quantum dot2The π and π of carbon*Silver-colored energy level is introduced between energy level, is realized Electron transition mode diversification, this is advantageous to material answering in fields such as photocatalysis, bio-imaging, opto-electronic device and detectors With.
The present invention has the following advantages that:(1)Cost is cheap:What Ag doping graphene quantum dot prepared by the present invention used Reaction unit is hydrothermal reaction kettle, and reaction temperature requires low, has the advantages of high efficiency, low cost;(2)Safety and environmental protection:Present invention system Reactant used in standby Ag doping graphene quantum dot is nontoxic, pollution-free, and whole preparation process is without potential safety hazard;(3)Product water Dissolubility is good:Ag doping graphene quantum dot prepared by the present invention has a variety of hydrophilic functional groups, therefore soluble in water;(4)Production Thing fluorescent characteristic is notable:Ag doping graphene quantum dot prepared by the present invention, fluoresces under ultraviolet light, be advantageous to it The application in the fields such as bio-imaging, fluorescence labeling.
Brief description of the drawings
Fig. 1 is Ag doping graphene quantum dot transmission electron microscope picture.
Fig. 2 is Ag doping graphene quantum dot X-ray diffractogram.
Fig. 3 is photoluminescence spectrum of the Ag doping graphene quantum dot in the case where wavelength is 440 nm exciting lights.
Fig. 4 is Ag doping graphene quantum dot ultraviolet visible absorption spectra.
Embodiment
Embodiment 1:0.5 gram of sucrose is weighed, 0.2 gram of silver acetate, adding 40 ml deionized waters makes reactant fully dissolve. The reaction solution configured is transferred in hydrothermal reaction kettle, is put into heated at constant temperature 4 hours in 170 DEG C of baking oven.After reaction terminates, Solution is taken out, dialysis purification is carried out to sample with bag filter, the time is 15~20 minutes, and bag filter external environment is deionization Water, finally collect and obtain potassium doped graphene quantum dot solution.

Claims (5)

1. a kind of hydro-thermal synthetic preparation method of Ag doping graphene quantum dot, it is characterised in that this method is by following What step was realized:
The first step, proper amount of sugar and silver acetate is taken to add deionized water stirring to be uniformly dissolved it;
Second step, the first step is obtained into solution and is transferred in hydrothermal reaction kettle, carry out isothermal reaction;
3rd step, after reaction terminates, negate solution after answering and carry out dialysis purification with bag filter, collect product.
2. the hydro-thermal synthetic preparation method of a kind of Ag doping graphene quantum dot according to right 1, it is characterised in that described Sugar can be any one in fructose, glucose or sucrose.
3. the hydro-thermal synthetic preparation method of a kind of Ag doping graphene quantum dot according to right 1, it is characterised in that first It is 0.5 gram to walk sugared dosage, 0.2 gram of silver acetate, 40 milliliters of deionized water.
4. the hydro-thermal synthetic preparation method of a kind of Ag doping graphene quantum dot according to right 1, it is characterised in that second It is 170 DEG C to walk isothermal reaction condition, and the reaction time is 4 hours.
5. the hydro-thermal synthetic preparation method of a kind of Ag doping graphene quantum dot according to right 1, it is characterised in that the 3rd Walk the use bag filter to dialyse to product, purify, dialysis time is 10~20 minutes.
CN201610516357.4A 2016-07-04 2016-07-04 A kind of preparation method of Ag doping graphene quantum dot Pending CN107572505A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108318438A (en) * 2018-01-19 2018-07-24 广东工业大学 The detection method of Ag doping fluorescent carbon quantum dot, preparation method and cholesterol
CN108892130A (en) * 2018-04-04 2018-11-27 三峡大学 The green synthesis method of graphene quantum dot is prepared using starch
CN110052267A (en) * 2019-05-07 2019-07-26 三峡大学 The preparation method and applications of the stable silver of graphene quantum dot and/or rhodium nanoparticles
CN110064389A (en) * 2019-04-22 2019-07-30 三峡大学 The preparation method and applications of the stable silver-colored rhodium duplex metal nano granule of graphene quantum dot
CN110066655A (en) * 2019-05-14 2019-07-30 安徽师范大学 Ag doping carbon quantum dot and its preparation method and application

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103172051A (en) * 2013-04-16 2013-06-26 苏州大学 Water-soluble carbon quantum dot and preparation method thereof
CN103359727A (en) * 2013-07-24 2013-10-23 云南师范大学 Preparation method of oxygen and chlorine co-doped graphene quantum dots
CN103833029A (en) * 2014-01-10 2014-06-04 云南师范大学 Preparation method of high-efficient multicolor-fluorescence water-soluble sulfur oxygen-codoped graphene quantum dot

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103172051A (en) * 2013-04-16 2013-06-26 苏州大学 Water-soluble carbon quantum dot and preparation method thereof
CN103359727A (en) * 2013-07-24 2013-10-23 云南师范大学 Preparation method of oxygen and chlorine co-doped graphene quantum dots
CN103833029A (en) * 2014-01-10 2014-06-04 云南师范大学 Preparation method of high-efficient multicolor-fluorescence water-soluble sulfur oxygen-codoped graphene quantum dot

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108318438A (en) * 2018-01-19 2018-07-24 广东工业大学 The detection method of Ag doping fluorescent carbon quantum dot, preparation method and cholesterol
CN108892130A (en) * 2018-04-04 2018-11-27 三峡大学 The green synthesis method of graphene quantum dot is prepared using starch
CN110064389A (en) * 2019-04-22 2019-07-30 三峡大学 The preparation method and applications of the stable silver-colored rhodium duplex metal nano granule of graphene quantum dot
CN110052267A (en) * 2019-05-07 2019-07-26 三峡大学 The preparation method and applications of the stable silver of graphene quantum dot and/or rhodium nanoparticles
CN110066655A (en) * 2019-05-14 2019-07-30 安徽师范大学 Ag doping carbon quantum dot and its preparation method and application
CN110066655B (en) * 2019-05-14 2022-04-12 安徽师范大学 Silver-doped carbon quantum dot and preparation method and application thereof

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