CN103626169A - Preparation method of graphene quantum dot - Google Patents
Preparation method of graphene quantum dot Download PDFInfo
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- CN103626169A CN103626169A CN201310542513.0A CN201310542513A CN103626169A CN 103626169 A CN103626169 A CN 103626169A CN 201310542513 A CN201310542513 A CN 201310542513A CN 103626169 A CN103626169 A CN 103626169A
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Abstract
The invention discloses a preparation method of a graphene quantum dot. The method is characterized by directly reacting 1-methyl-2-pyrrolidone with graphite powder in a solvent by utilizing a relatively strong peeling effect of 1-methyl-2-pyrrolidone to prepare a graphene quantum dot mixture, and centrifuging the graphene quantum dot mixture at a high speed to obtain the graphene quantum dot. The preparation method is simple, the raw materials are cheap, and the equipment is simple; moreover, the obtained material has even size and good thermal stability.
Description
Technical field
The present invention relates to quantum dot synthesis technical field, specifically a kind of method of being prepared by Graphite Powder 99 and 1-Methyl-2-Pyrrolidone solvent thermal reaction to graphene quantum dot.
Background technology
Graphene quantum dot is the nano material of accurate zero dimension, and the motion of its internal electron in all directions all limited to, so quantum confinement effect is remarkable especially, has the character of many uniquenesses.Aspect sensor, biomedicine, photodiode and solar cell, there iing very large application.Graphene quantum dot as a kind of sensitizing agent come the solar cell of sensitization and the mode of life of people's Sustainable development from now on closely related, so the research of graphene quantum dot will inevitably promote social development to a certain extent.
Conventionally the preparation method of graphene quantum dot is mainly divided into two large classes: method from top to bottom and from bottom to top.Method is from bottom to top that the method by physics or chemistry cuts into undersized graphene quantum dot by large-sized graphene platelet, comprises that hydrothermal method, electrochemical method and chemical method peel off the methods such as carbon fiber; Method is from bottom to top to using small molecules by series of chemical, to prepare graphene quantum dot as precursor, mainly contains ultrasonic method and microwave method, solution chemical method.Its carbon source of hydrothermal method is generally graphene oxide, its preparation process complexity and the more reagent of needs; The carbon source of electrochemical method is generally graphite rod, makes process more complicated the early stage of graphite, the comparatively complicated and length consuming time of the purifying of graphene quantum dot dialysis step in subsequent experimental; The experimental procedure of chemical solution method is comparatively complicated, the more difficult control of experiment condition in experimentation.Therefore, find a kind of simple graphene quantum dot preparation method extremely urgent.
Summary of the invention
The object of the invention is the triviality of preparing for existing graphene quantum dot and a kind of simple graphene quantum dot preparation method who provides; The even size distribution of prepared graphene quantum dot, this material has good commercial application prospect in area of solar cell.
The concrete technical scheme that realizes the object of the invention is:
A kind of simple preparation method of graphene quantum dot, feature is to utilize the effect of delaminating of 1-Methyl-2-Pyrrolidone, and in solution, direct and Graphite Powder 99 reaction, generates graphene quantum dot, high speed centrifugation obtains the graphene quantum dot of size homogeneous, specifically comprises the following steps:
A, get Graphite Powder 99 and put into container (graphite powders) and add 1-Methyl-2-Pyrrolidone, both are mixed, transfer in the autoclave with tetrafluoroethylene, under 150～200 ℃ of temperature condition, solvent thermal reaction 24h～96h, naturally cool to after room temperature, take out reactant; Wherein, Graphite Powder 99 is 100:1 with the ratio of the amount of substance of 1-Methyl-2-Pyrrolidone;
B, by gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor obtains described graphene quantum dot.
The present invention compared with prior art, has following remarkable advantage:
(1) reaction is the solvent thermal reaction in reactor, and technique is simple, environmental protection, equipment are cheap.
(2) carbon source used is Graphite Powder 99, Graphite Powder 99 aboundresources, and preparation cost is lower.
(3) gained graphene quantum dot size, between 2～4nm, has very strong fluorescent characteristic.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 9 resulting materials uv absorption spectras;
Fig. 2 is the fluorescence spectrum figure of the embodiment of the present invention 9 resulting materials;
Fig. 3 is the transmission electron microscope picture of the embodiment of the present invention 9 resulting materials;
Fig. 4 is the transmission electron microscope picture of the embodiment of the present invention 9 resulting materials.
Embodiment
The invention will be further described by the following examples:
Embodiment 1
Take the Graphite Powder 99 of 0.5g, add 40ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 150 ℃ of temperature condition, solvent thermal reaction 24h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 2
Take the Graphite Powder 99 of 0.25g, add 20ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 150 ℃ of temperature condition, solvent thermal reaction 48h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 3
Take the Graphite Powder 99 of 1g, add 80ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 150 ℃ of temperature condition, solvent thermal reaction 72h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 4
Take the Graphite Powder 99 of 0.5g, add 40ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 180 ℃ of temperature condition, solvent thermal reaction 24h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 5
Take the Graphite Powder 99 of 0.8g, add 64ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 180 ℃ of temperature condition, solvent thermal reaction 48h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 6
Take the Graphite Powder 99 of 0.5g, add 40ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 180 ℃ of temperature condition, solvent thermal reaction 72h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 7
Take the Graphite Powder 99 of 2.0g, add 160ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 200 ℃ of temperature condition, solvent thermal reaction 24h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 8
Take the Graphite Powder 99 of 0.5g, add 40ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 200 ℃ of temperature condition, solvent thermal reaction 48h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 9
Take the Graphite Powder 99 of 0.25g, add 20ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 200 ℃ of temperature condition, solvent thermal reaction 72h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 10
Take the Graphite Powder 99 of 0.6g, add 48ml 1-Methyl-2-Pyrrolidone, mix, transfer to in the autoclave of tetrafluoroethylene under 150 ℃ of temperature condition, solvent thermal reaction 96h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 11
Take the Graphite Powder 99 of 1.5g, add 120ml 1-Methyl-2-Pyrrolidone, mix, after in ultrasonic 10min, transfer to again with in the autoclave of tetrafluoroethylene under 200 ℃ of temperature condition, solvent thermal reaction 24h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Embodiment 12
Take the Graphite Powder 99 of 0.5g, add 40ml 1-Methyl-2-Pyrrolidone, mix, after in ultrasonic 30min, transfer to again with in the autoclave of tetrafluoroethylene under 200 ℃ of temperature condition, solvent thermal reaction 24h, naturally cools to after room temperature, takes out reactant;
By gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor can obtain graphene quantum dot.
Claims (1)
1. a preparation method for graphene quantum dot, is characterized in that the method comprises following concrete steps:
A, get Graphite Powder 99 and put into container and add 1-Methyl-2-Pyrrolidone, both are mixed, transfer in the autoclave with tetrafluoroethylene, under 150～200 ℃ of temperature condition, solvent thermal reaction 24h～96h, naturally cools to after room temperature, takes out reactant; Wherein, Graphite Powder 99 is 100:1 with the ratio of the amount of substance of 1-Methyl-2-Pyrrolidone;
B, by gained reactant high speed centrifugation 15min under 9000 rotating speeds, obtain yellow supernatant liquor, concentrated yellow supernatant liquor obtains described graphene quantum dot.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104401981A (en) * | 2014-11-10 | 2015-03-11 | 朱熹 | Preparation method of nitrogen-containing oxidative graphene quantum dot capable of giving off fluorescence in three primary colors |
| CN104556004A (en) * | 2014-12-26 | 2015-04-29 | 西北大学 | Preparation method of controlled fluorescent graphene quantum dot |
| CN104843679A (en) * | 2015-04-03 | 2015-08-19 | 北京理工大学 | Method for solvothermal peeling preparation of microcrystalline graphene from microcrystalline graphite |
| CN105860966A (en) * | 2015-01-23 | 2016-08-17 | 复旦大学 | Synthetic method of polymer-wrapped nitrogen-doped fluorescent carbon nanodots |
| CN106883851A (en) * | 2017-04-03 | 2017-06-23 | 桂林理工大学 | A kind of Mn2+Ion modification fluorescence Graphene and preparation method thereof |
| CN107010620A (en) * | 2016-01-27 | 2017-08-04 | 合肥工业大学 | A kind of method for preparing graphene quantum dot suitable for mass |
| CN107473207A (en) * | 2017-09-28 | 2017-12-15 | 中国科学技术大学 | A kind of preparation method of graphene quantum dot |
| KR20180078573A (en) * | 2016-12-30 | 2018-07-10 | 한양대학교 에리카산학협력단 | Method for preparing doped graphene quantum dots, doped graphene quantum dots produced thereby and photocatalyst comprising the same |
| CN113277499A (en) * | 2021-05-07 | 2021-08-20 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dot |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104401981A (en) * | 2014-11-10 | 2015-03-11 | 朱熹 | Preparation method of nitrogen-containing oxidative graphene quantum dot capable of giving off fluorescence in three primary colors |
| CN104556004A (en) * | 2014-12-26 | 2015-04-29 | 西北大学 | Preparation method of controlled fluorescent graphene quantum dot |
| CN105860966B (en) * | 2015-01-23 | 2018-10-26 | 复旦大学 | A kind of synthetic method of the N doping fluorescent carbon nano dot of polymer wrapped |
| CN105860966A (en) * | 2015-01-23 | 2016-08-17 | 复旦大学 | Synthetic method of polymer-wrapped nitrogen-doped fluorescent carbon nanodots |
| CN104843679A (en) * | 2015-04-03 | 2015-08-19 | 北京理工大学 | Method for solvothermal peeling preparation of microcrystalline graphene from microcrystalline graphite |
| CN107010620A (en) * | 2016-01-27 | 2017-08-04 | 合肥工业大学 | A kind of method for preparing graphene quantum dot suitable for mass |
| CN107010620B (en) * | 2016-01-27 | 2019-06-18 | 合肥工业大学 | A method of graphene quantum dot is prepared suitable for mass |
| KR20180078573A (en) * | 2016-12-30 | 2018-07-10 | 한양대학교 에리카산학협력단 | Method for preparing doped graphene quantum dots, doped graphene quantum dots produced thereby and photocatalyst comprising the same |
| KR101901901B1 (en) | 2016-12-30 | 2018-09-28 | 한양대학교 에리카산학협력단 | Method for preparing doped graphene quantum dots, doped graphene quantum dots produced thereby and photocatalyst comprising the same |
| CN106883851A (en) * | 2017-04-03 | 2017-06-23 | 桂林理工大学 | A kind of Mn2+Ion modification fluorescence Graphene and preparation method thereof |
| CN107473207A (en) * | 2017-09-28 | 2017-12-15 | 中国科学技术大学 | A kind of preparation method of graphene quantum dot |
| CN107473207B (en) * | 2017-09-28 | 2020-05-05 | 中国科学技术大学 | Preparation method of graphene quantum dots |
| CN113277499A (en) * | 2021-05-07 | 2021-08-20 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dot |
| CN113277499B (en) * | 2021-05-07 | 2022-11-08 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dots |
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Application publication date: 20140312 |