CN105417536A - Method for preparing graphene quantum dots with adjustable oxygen content - Google Patents
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention belongs to the technical field of preparation of graphene quantum dots, and relates to a method for preparing graphene quantum dots with adjustable oxygen content. The method comprises the steps that a brown graphene quantum dot water solution containing impurities is prepared through an electrochemistrical cyclic voltammetry method and then dialyzed, and a transparent flavescent graphene quantum dot water solution is obtained; the graphene quantum dots with different oxygen contents are prepared by regulating the oxidoreduction degree of an electrolyte in the electrochemistrical method preparation process. According to the method, the oxygen contents of the graphene quantum dots are effectively regulated, and the speed of preparing the graphene quantum dots through the electrochemistrical cyclic voltammetry method is increased. Meanwhile, the method is simple in preparation procedure, and has the advantages of being environmentally friendly and low in production cost and facilitating industrialization.
Description
The invention belongs to graphene quantum dot preparing technical field, be specifically related in the process of electrochemical production, pass through the redox condition of regulation and control to electrolytic solution, prepare the graphene quantum dot of different oxygen level.
Background technology
In recent years, Graphene receives increasing concern because of the performance of uniqueness, as large specific surface area, high carrier mobility, excellent mechanical flexibility, good heat/chemical stability and to environment, and friendly feature etc.As the newcomer of Graphene family, the zero dimension graphene quantum dot with quantum effect and side effect arises at the historic moment.The photophysical property of the excellence that graphene quantum dot has, good unreactiveness, bio-compatibility and water-solublely make it in bio-imaging, biosensor, catalyzer and medicament transport etc., show application prospect widely.(M.A.Sk, A.Ananthanarayanan, L.Huang, K.H.LimandP.Chen, etal.J.Mater.Chem.C, 2014,2,6954 – 6960) but lower preparation speed and concentration limit the Study and appliance of graphene quantum dot.
Generally speaking, the method preparing graphene quantum dot at present can be summed up as from top to bottom with method from bottom to top, be that large-size carbon material is cut into small size graphene quantum dot by physics or chemical process by finger from top to bottom, comprise acidifying oxidation style, hydrothermal method, solvent-thermal method and electrochemical oxidation process and ultrasonic method etc.; Method comprises electrochemical process and chemical stripping carbon fiber method etc. from bottom to top; (ZhengXT, AnanthanarayananA, LuoKQ, etal..Small, 2015,11,1620-1636) bottom-to-top method then refers to that making precursor with small molecules prepares graphene quantum dot by series of chemical, mainly comprises solution chemical method, ultrasonic wave and microwave method etc.But although from top to bottom in method higher the also existing of quantum yield need to use the shortcomings such as a large amount of strong acid or complex operation step.Although method easily controls the scale topography of graphene quantum dot but required equipment is special, raw materials is expensive, operation steps is very complicated from top to bottom, and prepared graphene quantum dot oxygen-containing functional group is limited is unfavorable for that it dissolves and further to functionalization and the passivation of graphene quantum dot.
In these preparation methods, electrochemical method is convenient to plan as a whole, does not use acid with strong oxidizing property or strong reductant, is had the advantages such as certain commercial viability and show one's talent in numerous method due to easy, the whole preparation process of operating process.Especially enrich with this deposit of graphite, environmentally friendly presoma instead of the expensive material such as graphite oxide, CNT (carbon nano-tube).In general, electrochemical method utilize conductive ion solution and apply power supply to the change accelerating graphite precursor construction mainly based on water molecules in ionic liquid in anodic oxidation and anion intercalated interaction.Preparation process can be divided into four steps: the first step, and water molecules is oxidized on anode, and reaction produces hydroxyl and the oxyradical with oxidisability, and free radical attacks edge and the defect area of graphite grains, is oxidized or hydroxylation, causes anode carbon nanocrystal to decompose; Second step, the oxidizing reaction of fringe region opens frictional belt, is conducive to the intercalation of negatively charged ion, makes graphite anode depolarize and expands; 3rd step, oxidizing reaction makes graphite flake be cracked into GQDs; 4th step, the flap of generation precipitates as graphene nanometer sheet.Meanwhile, preparation GQDs technological process can be summarized as three phases: the first stage is the inductive phase before peeling off generation, electrolytic solution color from colourless to yellow again to burgundy; Second-stage graphite anode obviously expands; Phase III graphite flake peels off from anode, forms black slurry together with electrolytic solution.And electrochemical cyclic voltammetry makes same root graphite electrode constantly exchange between anode and negative electrode, the ionogen around it just experienced by the working cycle of repeatedly anodic oxidation and cathodic reduction in a short period of time.Graphite grains is continuous dilation in the redox working cycle of experience, and this mechanical force makes carbon carbon associative key more easily rupture, and thus accelerates the speed come off at graphite rod of GQDs.(ZhangM, BaiL, ShangW, etal.J.Journalofmaterialschemistry, 2012,22:7461-7467) so prepare the mechanism supposition of GQDs according to electrochemical method, can prepare the different graphene quantum dot of oxygen level by regulation and control ionogen in the redox reaction degree of cathode and anode, the height of simultaneous oxidation degree finally also can produce material impact to the content of graphene quantum dot oxygen level functional group.Generally, the graphene quantum dot solvability of high oxygen-containing functional group content is beneficial to well further to functionalization and the passivation of graphene quantum dot, and the graphene quantum dot of low oxygen-containing functional group content has higher quantum yield.
Summary of the invention
Electrochemical process is utilized to regulate and control the redox reaction degree of ionogen in cathode and anode to prepare the different graphene quantum dot of oxygen level.The implementation method of regulation and control electrolyte redox degree has a lot, composition etc. that such as regulate electrochemical process, that change electrolytic solution.
The preparation method of a kind of oxygen level is adjustable graphene quantum dot, it is characterized in that: first employing electrochemical cyclic voltammetry prepares the graphene quantum dot aqueous solution that brown contains impurity, again the graphene quantum dot aqueous solution that brown contains impurity is dialysed, obtain the transparent flaxen graphene quantum dot aqueous solution; By the redox condition of regulation and control to electrolytic solution in the process of electrochemical production, prepare graphene quantum dot that is different and oxygen level;
Implementation method is: the phosphate buffered saline buffer loading a certain amount of hydrogen peroxide in No. 1 reaction vessel is electrolyte solution, in No. 2 reaction vessels, load phosphate buffered saline buffer is electrolyte solution, No. 1 and No. 2 reaction units are connected in parallel, with the ultraviolet radiation reaction unit of certain wavelength, electrochemical cyclic voltammetry is utilized to prepare concentration high, the graphene quantum dot that oxygen level is different.
The concrete preparation process of the present invention comprises the following steps:
Step 1), in No. 1 reaction vessel, add 0.1mol/L,, PH=7 phosphate buffered saline buffer (PBS), form certain volume proportion with 30wt.% hydrogen peroxide, and two ultrapure graphite rods are inserted in solution as working electrode with to electrode;
Step 2), in No. 2 reaction vessels, add 0.1mol/L, the phosphate buffered saline buffer (PBS) of PH=7, two ultrapure graphite rod to be inserted in solution as working electrode with to electrode, uses uviolizing reaction soln;
Step 3), by above-mentioned steps 1) and step 2) No. 1 and No. 2 high-purity carbon-points of reaction vessel be parallel-connected to electrochemical workstation, using Ag/AgCl as reference electrode, scan with electrochemical cyclic voltammetry.
Described step 1) described in 0.1mol/L, the phosphate buffered saline buffer (PBS) of PH=7 and the volume proportion of 30wt.% hydrogen peroxide close is 40:1/1:1; Step 2) described in ultraviolet source power be 18 ~ 300W, ultraviolet wavelength is 100 ~ 365nm.
The working parameter of described electrochemical cyclic voltammetry is: Ag/AgCl makes reference electrode, cyclic voltammetric voltage 1 ~ 5V, scanning speed 0.1 ~ 0.6V/s, the scanning number of turns 1700 ~ 216000.
Described dialysis is filtered by the filtering head of the brown aqueous solution 220nm obtained in two containers, then dialyses with the dialysis tubing that molecular weight cut-off is 3500 ~ 14000Da, and compartment changes water dialysis at regular intervals, removes unnecessary ion.Dialysis time, at 5 ~ 9 days, often changes a deionized water at regular intervals, and finally obtain two kinds of transparent faint yellow aqueous solution, the described transparent flaxen aqueous solution is the graphene quantum dot aqueous solution.Measure the concentration of solution, and carry out the contamination that x-ray photoelectron power spectrum and examination of infrared spectrum determine to show oxygen-containing functional group.
By changing the mode of electrochemical cyclic voltammetry electrolyte solution, namely 0.1mol/L is used, carry out a certain proportion of proportioning with hydrogen peroxide in the phosphate buffered saline buffer (PBS) of PH=7 and prepare electrolyte solution, and then it is high successfully to prepare concentration fast, is rich in the graphene quantum dot of a large amount of oxygen-containing functional group; Hydrogen peroxide can become hydroxyl radical free radical and the strong high free radical of superoxide radical isoreactivity high oxidative by electrochemical oxidation on coated graphite rod electrrode, can be oxidized and accelerate the peeling rate of graphene quantum dot, and then it is high successfully to prepare concentration fast, is rich in the graphene quantum dot of a large amount of oxygen-containing functional group.
In suitably distance, radiation is carried out to the device that electrochemical process peels off graphene quantum dot with the ultraviolet lamp of certain wavelength and power.Because water can produce reducing substances in radiative process in radiative process, and strong uv-radiation can cause coming off of graphene quantum dot oxygen-containing functional group, thus can prepare fast concentration high, be rich in less oxygen-containing functional group graphene quantum dot.
The preparation method of oxygen level is adjustable graphene quantum dot, described method is by regulating the redox ability of electrolyte solution, and then it is high to utilize electrochemical production to go out concentration, the graphene quantum dot that oxygen level is different.
The present invention has has not only regulated and controled graphene quantum dot oxygen level effectively, also improves the speed of the graphene quantum dot prepared by electrochemical cyclic voltammetry.Meanwhile, this preparation method does not relate to any organic solvent, corrodibility strong acid, does not relate to complicated preparation section, has the advantage that environmental protection, production cost are low, be easy to industrialization.
Accompanying drawing explanation
Fig. 1 is the fast preparation method schema of oxygen level controllable graphene quantum dot
Embodiment
The fast preparation method of oxygen level controllable graphene quantum dot
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is explained in further detail.Should be appreciated that specific embodiment described herein only for explaining the present invention, being not intended to limit the present invention.
The present invention relates to the fast preparation method of oxygen level controllable graphene quantum dot.Described preparation method can regulate and control the oxygen-containing functional group content of graphene quantum dot and can improve the synthesis speed of graphene quantum dot.The intermediate product of preparation comprises the graphene quantum dot aqueous solution, and the described graphene quantum dot aqueous solution comprises graphene quantum dot, and described method cost of material is lower, and operation steps is simple, avoids adopting severe corrosive acid in preparation process.Hydrogen peroxide is electrochemically oxidized at anode and is oxidized to hydroxyl radical free radical and superoxide radical isoreactivity is high, oxidisability is strong free radical in the electrolytic solution, can accelerate the peeling rate of graphene quantum dot on high-purity carbon-point and can increase the content of prepared graphene quantum dot surface especially edge hydroxyl, carboxyl, epoxy group(ing) and carbonyl.High-strength ultraviolet radiation can not only make rupturing containing oxygen oxygen-containing functional group on Graphene quantum, catalytic water can also decompose the hydroperoxyl radical producing and have strong reducing property, namely graphene quantum dot reduction be reduced the content of oxygen-containing functional group; The free radical produced also can accelerate the peeling rate of graphene quantum dot on high-purity carbon-point.
In order to explain the present invention further, specific embodiment is adopted to make an explanation to the present invention.
Embodiment one
Compound concentration is 0.1mol/L, the phosphate buffered saline buffer (PBS) of PH=7, add the superoxol (volume proportion is 1:1) of biological phosphate buffer soln and 30wt.% in No. 1 container (quartz or glasswork), two high purity graphite rods are inserted as working electrode with to electrode; Add the phosphate buffer soln of certain volume in No. 2 containers (quartz or glasswork), inserting two high purity graphite rods as working electrode with to electrode, take wavelength as ultraviolet radiation No. 2 devices of 254nm; No. 1 container and No. 2 containers are parallel-connected to electrochemical workstation, adopt electrochemical cyclic voltammetry.Ag/AgCl makes reference electrode, light prepares water-soluble graphene quantum dots as working electrode with to electrode electro Chemical cyclic voltammetry simultaneously: using high purity graphite rod simultaneously as working electrode with to electrode, Ag/AgCl makes reference electrode, cyclic voltammetric voltage-1.5 is to+1.5V, scanning speed 0.1V/s, the scanning number of turns 216000.The filtering head of the brown aqueous solution 220nm obtained in two containers is filtered, then dialyses with the dialysis tubing that molecular weight cut-off is 3500Da, remove unnecessary ion.
Get the GQDs aqueous solution of above-mentioned preparation respectively, drip the clean silicon chip surface being coated onto 0.5 × 0.5cm, show through infrared spectra and the test of x-ray photoelectron power spectrum: compared with the graphene quantum dot prepared by electrochemical cyclic voltammetry usual way (phosphate buffered saline buffer of PH=7 is that electrolyte solution does not add ultraviolet radiation), the graphene quantum dot prepared in No. 1 container has the oxygen-containing functional group of more high-content, and the graphene quantum dot prepared in No. 2 containers has less oxygen-containing functional group.The concentration of two kinds of graphene quantum dot solution is all higher.
Embodiment two
Compound concentration is 0.1mol/L, the phosphate buffered saline buffer (PBS) of PH=7, (volume proportion is (40:1), inserts two high purity graphites rods as working electrode with to electrode to add the superoxol of phosphate buffer soln and 30wt.% in No. 1 container (quartz or glasswork); Add the phosphate buffer soln of certain volume in No. 2 containers (quartz or glasswork), inserting two high purity graphite rods as working electrode with to electrode, take wavelength as ultraviolet radiation No. 2 devices of 365nm; No. 1 container and No. 2 containers are parallel-connected to electrochemical workstation, adopt electrochemical cyclic voltammetry.Ag/AgCl makes reference electrode, light prepares water-soluble graphene quantum dots as working electrode with to electrode electro Chemical cyclic voltammetry simultaneously: using high purity graphite rod simultaneously as working electrode with to electrode, Ag/AgCl makes reference electrode, cyclic voltammetric voltage-1.5 is to+1.5V, scanning speed 0.1V/s, the scanning number of turns 216000.The filtering head of the brown aqueous solution 220nm obtained in two containers is filtered, then dialyses with the dialysis tubing that molecular weight cut-off is 3500Da, remove unnecessary ion.
Get the GQDs aqueous solution of above-mentioned preparation respectively, drip the clean silicon chip surface being coated onto 0.5 × 0.5cm, show through infrared spectra and the test of x-ray photoelectron power spectrum: compared with the graphene quantum dot prepared by electrochemical cyclic voltammetry usual way (phosphate buffered saline buffer of PH=7 is that electrolyte solution does not add ultraviolet radiation), the graphene quantum dot prepared in No. 1 container has the oxygen-containing functional group of more high-content, and the graphene quantum dot prepared in No. 2 containers has less oxygen-containing functional group.The concentration of two kinds of graphene quantum dot solution is all higher.
Claims (5)
1. the preparation method of the adjustable graphene quantum dot of oxygen level, it is characterized in that: first employing electrochemical cyclic voltammetry prepares the graphene quantum dot aqueous solution that brown contains impurity, again the graphene quantum dot aqueous solution that brown contains impurity is dialysed, obtain the transparent flaxen graphene quantum dot aqueous solution; By the redox condition of regulation and control to electrolytic solution in the process of electrochemical production, prepare graphene quantum dot that is different and oxygen level;
Implementation method is: the phosphate buffered saline buffer loading a certain amount of hydrogen peroxide in No. 1 reaction vessel is electrolyte solution, in No. 2 reaction vessels, load phosphate buffered saline buffer is electrolyte solution, No. 1 and No. 2 reaction units are connected in parallel, with the ultraviolet radiation reaction unit of certain wavelength, electrochemical cyclic voltammetry is utilized to prepare concentration high, the graphene quantum dot that oxygen level is different.
2. the preparation method of the adjustable graphene quantum dot of oxygen level according to claim 1, is characterized in that: described concrete preparation process comprises the following steps:
Step 1), in No. 1 reaction vessel, add 0.1mol/L, the phosphate buffered saline buffer (PBS) of PH=7, form certain volume proportion with 30wt.% hydrogen peroxide, and two ultrapure graphite rods are inserted in solution as working electrode with to electrode;
Step 2), in No. 2 reaction vessels, add 0.1mol/L, the phosphate buffered saline buffer (PBS) of PH=7, two ultrapure graphite rod to be inserted in solution as working electrode with to electrode, uses uviolizing reaction soln;
Step 3), by above-mentioned steps 1) and step 2) No. 1 and No. 2 high-purity carbon-points of reaction vessel be parallel-connected to electrochemical workstation, using Ag/AgCl as reference electrode, scan with electrochemical cyclic voltammetry.
3. the preparation method of the adjustable graphene quantum dot of oxygen level according to claim 2, it is characterized in that: described step 1) described in 0.1mol/L, it is 40:1/1:1 that the phosphate buffered saline buffer (PBS) of PH=7 and the volume proportion of 30wt.% hydrogen peroxide close; Step 2) described in ultraviolet source power be 18 ~ 300W, ultraviolet wavelength is 100 ~ 365nm.
4. the preparation method of the adjustable graphene quantum dot of oxygen level according to claim 1 and 2, it is characterized in that: it is characterized in that the working parameter of described electrochemical cyclic voltammetry is: Ag/AgCl makes reference electrode, cyclic voltammetric voltage 1 ~ 5V, scanning speed 0.1 ~ 0.6V/s, the scanning number of turns 1700 ~ 216000.
5. the preparation method of the adjustable graphene quantum dot of oxygen level according to claim 1, it is characterized in that described dialysis is filtered by the filtering head of the brown aqueous solution 220nm obtained in two containers, then dialyse with the dialysis tubing that molecular weight cut-off is 3500 ~ 14000Da, compartment changes water dialysis at regular intervals, removes unnecessary ion.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105862057A (en) * | 2016-04-15 | 2016-08-17 | 北京科技大学 | Phosphorus-doped graphene quantum dot and electrochemistry preparing method thereof |
| CN106676563A (en) * | 2017-01-11 | 2017-05-17 | 肇庆学院 | Ultrasonic electrolytic preparation method for carboxylated carbon nanosheet |
| CN108117066A (en) * | 2017-12-19 | 2018-06-05 | 浙江工业大学 | A kind of nitrogen-doped graphene quantum dot electrochemical preparation method |
| CN108190877A (en) * | 2018-02-22 | 2018-06-22 | 国家纳米科学中心 | A kind of graphene oxide, preparation method and purposes |
| CN108468071A (en) * | 2017-02-23 | 2018-08-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electrochemical ion impact prepares the method and its application of inorganic non-metallic material quantum dot |
| CN108795421A (en) * | 2018-04-11 | 2018-11-13 | 北京科技大学 | A kind of Preparation method and use of chlorine doped graphene quantum dot |
| CN108842157A (en) * | 2018-02-08 | 2018-11-20 | 浙江工业大学 | A method of multicolor fluorescence graphene quantum dot is prepared in same electrolytic tank electrolysis |
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| CN105862057A (en) * | 2016-04-15 | 2016-08-17 | 北京科技大学 | Phosphorus-doped graphene quantum dot and electrochemistry preparing method thereof |
| CN105862057B (en) * | 2016-04-15 | 2018-07-31 | 北京科技大学 | A kind of p-doped graphene quantum dot and its electrochemical preparation method |
| CN106676563A (en) * | 2017-01-11 | 2017-05-17 | 肇庆学院 | Ultrasonic electrolytic preparation method for carboxylated carbon nanosheet |
| CN106676563B (en) * | 2017-01-11 | 2018-08-10 | 肇庆学院 | A kind of ultrasonic electrolysis preparation method of carboxylated carbon nanosheet |
| CN108468071A (en) * | 2017-02-23 | 2018-08-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electrochemical ion impact prepares the method and its application of inorganic non-metallic material quantum dot |
| CN108117066A (en) * | 2017-12-19 | 2018-06-05 | 浙江工业大学 | A kind of nitrogen-doped graphene quantum dot electrochemical preparation method |
| CN108842157A (en) * | 2018-02-08 | 2018-11-20 | 浙江工业大学 | A method of multicolor fluorescence graphene quantum dot is prepared in same electrolytic tank electrolysis |
| CN108190877A (en) * | 2018-02-22 | 2018-06-22 | 国家纳米科学中心 | A kind of graphene oxide, preparation method and purposes |
| CN108795421A (en) * | 2018-04-11 | 2018-11-13 | 北京科技大学 | A kind of Preparation method and use of chlorine doped graphene quantum dot |
| CN110205709A (en) * | 2019-05-21 | 2019-09-06 | 湖南东映碳材料科技有限公司 | A kind of preparation method of high-performance mesophase pitch-based carbon fibers |
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| CN111252759A (en) * | 2019-11-20 | 2020-06-09 | 厦门大学 | Method for preparing graphene oxide by illumination and product |
| CN111252759B (en) * | 2019-11-20 | 2021-03-09 | 厦门大学 | Method for preparing graphene oxide by illumination and product |
| CN112938950A (en) * | 2021-03-19 | 2021-06-11 | 西安理工大学 | Graphene quantum dot solution prepared by electrochemical method and method |
| CN112938950B (en) * | 2021-03-19 | 2022-12-02 | 西安理工大学 | Graphene quantum dot solution prepared by electrochemical method and method |
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