CN105181660A - Method for preparing graphene fluorescence quantum dots through electrochemical pulse - Google Patents
Method for preparing graphene fluorescence quantum dots through electrochemical pulse Download PDFInfo
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- CN105181660A CN105181660A CN201510358196.6A CN201510358196A CN105181660A CN 105181660 A CN105181660 A CN 105181660A CN 201510358196 A CN201510358196 A CN 201510358196A CN 105181660 A CN105181660 A CN 105181660A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000002096 quantum dot Substances 0.000 title abstract description 31
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 28
- 239000010439 graphite Substances 0.000 claims abstract description 28
- 239000003792 electrolyte Substances 0.000 claims abstract description 12
- 150000001450 anions Chemical class 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 24
- 239000008151 electrolyte solution Substances 0.000 claims description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 11
- 238000000502 dialysis Methods 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- GTKRFUAGOKINCA-UHFFFAOYSA-M chlorosilver;silver Chemical compound [Ag].[Ag]Cl GTKRFUAGOKINCA-UHFFFAOYSA-M 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 2
- 150000001768 cations Chemical class 0.000 abstract 1
- 239000006228 supernatant Substances 0.000 description 9
- 239000010410 layer Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
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- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The present invention discloses a method for preparing graphene fluorescence quantum dots by using electrochemical pulse. The method comprises that: a graphite electrode is adopted as a first electrode, and the graphite electrode at least forms an electrochemical system with a second electrode, a reference electrode and an electrolyte; and an electrochemical pulse method is used to repeatedly and alternately apply positive potential and negative potential on the first electrode to make anions and cations in the electrolyte alternately enter between the layers of the graphite so as to make the layers of the graphite be peeled to obtain the graphene fluorescent quantum dots. With the method of the present invention, the rapid preparation of the high-quality, high-dispersity and the small-size graphene quantum dots can be achieved, the process is simple, the energy consumption is low, the efficiency is high, the industrial large-scale production is easily achieved, and the wide practical values and the industrial prospects are provided.
Description
Technical field
The present invention relates to a kind of preparation method of graphene quantum dot, particularly a kind of galvanochemistry pulse system is for the method for Graphene fluorescence quantum, belongs to grapheme material scientific domain.
Background technology
Graphene, as the thinnest two-dimensional material, forms by monolayer carbon atom is tightly packed.Graphene, because of the structure of himself uniqueness, shows the performance of numerous excellence, comprises electricity, optics, and calorifics and mechanical property become gradually in recent years at chemistry, the study hotspot in material science and physics field.
As the graphene quantum dot of zero dimension in Graphene, progressively attract the interest of people this year.Compared with traditional semiconductor-quantum-point, graphene quantum dot is cheap, and dissolubility is excellent, and photoluminescence performance is stablized, and specific surface area is large, and energy gap is adjustable, the low and bio-compatibility of cytotoxicity.Because these advantage graphene quantum dots are in photocatalysis, photoelectron, cell imaging, biological medicine, there is huge application potential sensor aspect.
The method preparing graphene quantum dot at present mainly contains method and from bottom to top method from top to bottom.Wherein, method mainly does presoma with Small molecular from bottom to top, by chemical reactive synthesis quantum dot, comprises solution chemical method, ultrasonic method and microwave method.And large-sized carbon source is mainly divided into undersized quantum dot by the method for physics or chemistry by rule, comprise hydro-thermal method from top to bottom, electrochemical stripping method, chemical stripping method.Then these methods are time consumption and energy consumption all relatively, and preparation process is loaded down with trivial details.
Summary of the invention
Fundamental purpose of the present invention is to provide a kind of galvanochemistry pulse system that utilizes for the method for Graphene fluorescence quantum, to overcome deficiency of the prior art.
For realizing aforementioned invention object, providing a kind of galvanochemistry pulse system that utilizes in a case study on implementation of the present invention for the method for Graphene fluorescence quantum, comprising:
Using graphite electrode as the first electrode, and at least jointly build electrochemical system with the second electrode, contrast electrode and electrolytic solution;
Adopt galvanochemistry impulse method, by repeatedly alternately applying positive potential and negative potential to the first electrode, the anions and canons in electrolytic solution is made repeatedly alternately to enter graphite between layers, and then graphite is peeled off between layers, obtain Graphene fluorescence quantum (also can be called for short graphene quantum dot as follows).
Among a comparatively preferred embodiment, described method also can comprise: after generating Graphene fluorescence quantum by repeatedly alternately applying positive potential and negative potential to the first electrode, again removing obtain sediment in mixed reaction solution, and dialysis treatment is carried out to the remaining stillness of night and removes electrolyte ion, obtain the Graphene fluorescence quantum of purifying.
Further, described graphite electrode can as working electrode, also can as to electrode, relative, and the second electrode can as to electrode or working electrode.
Further, describedly can comprise platinum electrode or graphite electrode to electrode, but be not limited thereto.
Further, described contrast electrode can comprise saturated calomel electrode or silver silver chloride electrode, but is not limited thereto.
Further, described electrolytic solution can be selected from acid solution, alkaline solution and neutral solution.Such as, described electrolytic solution at least optional self-contained KOH, NaOH, KCl, Na
2sO
4, H
2sO
4in the solution of the combination of any one or more.
Among a comparatively preferred embodiment, the span of described positive potential is 0V ~ 5V, and preferably as 3V ~ 5V, the span of negative potential is-5V ~ 0V, preferably as-5V ~-3V.
In the process, holding time of positive and negative current potential is prepared and the impact that do not make significant difference graphene quantum dot, and only can affect the quantity of stripping, and the time that therefore positive and negative current potential maintains can set according to actual needs.
Among one comparatively specific embodiment, described method also can comprise: adopt centrifugation removing obtain sediment in mixed reaction solution, wherein centrifugal rotational speed is at more than 5000rpm.And when centrifugal rotational speed is higher, it there is no impact to the quality of graphene quantum dot.
In the process, can select according to electrolyte component for dialysis membrane, such as can adopt MwCO about 10,000 cellulose dialysis film, it is mainly in order to remove electrolyte ion, and does not make significant difference to the quality of graphene quantum dot.
Among one more specifically case study on implementation, described method can comprise the steps:
Step 1, using coated graphite rod electrrode as working electrode, large area platinized platinum is as to electrode, and saturated calomel electrode forms three-electrode system as contrast electrode, and electrolytic solution is 6MKOH solution;
Step 2, employing galvanochemistry impulse method are peeled off, anode potential maintains 100s, change polarity cathode potential and maintain 100s, repeatedly to 6h, the zwitterion in electrolytic solution is made repeatedly alternately to enter graphite rod between layers, utilize electronic repulsion forces that graphite rod is peeled off between layers, obtain graphene quantum dot;
Step 3, the solution centrifugal that will obtain, get supernatant liquor;
Dialysis when step 4, employing dialysis membrane are long, removing electrolyte ion.
Further, the particle diameter of described Graphene fluorescence quantum is about 2 ~ 4nm.
Further, described Graphene fluorescence quantum also has fluorescent characteristic, such as can under wavelength is about the fluorescence of 365nm blue light-emitting.
The inventive method make use of cathode current cleverly and anode current alternate repetition applies, and makes the negative ion in electrolyte and kation alternately enter graphite layers, utilizes electronic repulsion forces to make Graphene splitting obtain graphene quantum dot.Specifically, in the method for the invention, when maintaining constant potential certain hour when positive potential, the negative ion in electrolytic solution can be made to be attracted interlayer that intercalation enters graphite, change positive potential into negative potential again and maintain constant potential certain hour, negative ion in graphite intercalation is released, and the kation in electrolytic solution is drawn into graphite rod interlayer by negative potential, further intercalation.So repeatedly carry out galvanochemistry pulse stripping, then carry out centrifugal to gained solution, except sub-cloud peels off the powdered graphite got off, obtain the supernatant liquor containing graphene quantum dot.Then dialyse to supernatant liquor, the electrolyte ion in removing solution, obtains high-quality graphene quantum dot.
Compared with prior art, the graphene quantum dot that the present invention utilizes galvanochemistry impulse method to prepare repeatedly enters due to zwitterion and is released in graphite layers, charge stripping efficiency prepares graphene quantum dot higher than generic electrochemical method, and technique is simple, simple operation, energy consumption are low, can be used for industrial mass production and prepare graphene quantum dot, there is practical value and industrial prospect widely.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention 1 obtain the photo of graphene quantum dot aqueous solution;
Fig. 2 be the embodiment of the present invention 1 obtain the photoluminescence photo of graphene quantum dot;
Fig. 3 be the embodiment of the present invention 1 obtain the transmission electron microscope picture of graphene quantum dot;
Fig. 4 be the embodiment of the present invention 1 obtain the high-resolution-ration transmission electric-lens figure of graphene quantum dot;
Fig. 5 be the embodiment of the present invention 1 obtain the grain size distribution of graphene quantum dot.
Embodiment
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Embodiment 1:
Step 1, using graphite rod as working electrode, platinized platinum as to electrode, and connects saturated calomel reference electrode composition three-electrode system, adds concentration and is about the KOH solution of 6M as electrolytic solution;
Step 2, employing galvanochemistry impulse method are peeled off, 100s when contrived experiment parameter is constant potential positive potential 3V, 100s during negative potential-3V, and circulate about 6h and so forth;
Step 3, by step 2 obtain dark solution with the rotating speed centrifugal treating of 5000rpm, discard lower floor's powdered graphite, retain supernatant liquor;
Step 4, by step 3 obtain supernatant liquor and carry out dialyse (cellulose dialysis film can be adopted, MwCO about 10,000), electrolyte ion in removing solution, obtain graphene quantum dot aqueous solution, it is as shown in Figure 1.Refer to shown in Fig. 2, obtain graphene quantum dot and be about blue light-emitting under the fluorescence of 365nm at wavelength.Refer to Fig. 3-Fig. 5 again, the graphene quantum dot that obtains is homogeneously dispersed state, and size is even, and particle diameter is about about 2.8nm.
Embodiment 2:
Step 1, using graphite rod as working electrode, platinized platinum as to electrode, and connects saturated calomel reference electrode composition three-electrode system, adds the Na that concentration is about 0.5M
2sO
4solution is as electrolytic solution;
Step 2, employing galvanochemistry impulse method are peeled off, 100s when contrived experiment parameter is constant potential positive potential 3V, 100s during negative potential-3V, and circulate about 6h and so forth;
Step 3, by step 2 obtain dark solution with the rotating speed centrifugal treating of 5000rpm, discard lower floor's powdered graphite, retain supernatant liquor;
Step 4, by step 3 obtain supernatant liquor and carry out dialyse (cellulose dialysis film can be adopted, MwCO about 10,000), electrolyte ion in removing solution, obtains graphene quantum dot aqueous solution.
Embodiment 3:
Step 1, using graphite rod as working electrode, platinized platinum as to electrode, and connects saturated calomel reference electrode composition three-electrode system, adds concentration and is about the KOH solution of 6M as electrolytic solution;
Step 2, employing galvanochemistry impulse method are peeled off, 100s when contrived experiment parameter is constant potential positive potential 5V, 100s during negative potential-5V, and circulate about 6h and so forth;
Step 3, by step 2 obtain dark solution with the rotating speed centrifugal treating of 5000rpm, discard lower floor's powdered graphite, retain supernatant liquor;
Step 4, by step 3 obtain supernatant liquor and carry out dialyse (cellulose dialysis film can be adopted, MwCO about 10,000), electrolyte ion in removing solution, obtains graphene quantum dot aqueous solution.
Utilize method of the present invention, can realize the quick preparation of high-quality, high degree of dispersion, small size graphene quantum dot, and technique is simple, energy consumption is low, and efficiency is high, is easy to realize industrialization large-scale production.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all make in spirit of the present invention any amendment, supplement or similar fashion substitute etc., all should be included within protection scope of the present invention.
Claims (9)
1. utilize galvanochemistry pulse system for a method for Graphene fluorescence quantum, it is characterized in that comprising:
Using graphite electrode as the first electrode, and at least jointly build electrochemical system with the second electrode, contrast electrode and electrolytic solution;
Adopt galvanochemistry impulse method, by repeatedly alternately applying positive potential and negative potential to the first electrode, making the anions and canons in electrolytic solution repeatedly alternately enter graphite between layers, and then graphite is peeled off between layers, obtain Graphene fluorescence quantum.
2. the galvanochemistry pulse system that utilizes according to claim 1 is for the method for Graphene fluorescence quantum, it is characterized in that comprising: after generating Graphene fluorescence quantum by repeatedly alternately applying positive potential and negative potential to the first electrode, again removing obtain sediment in mixed reaction solution, and dialysis treatment is carried out to the remaining stillness of night and removes electrolyte ion, obtain the Graphene fluorescence quantum of purifying.
3. the galvanochemistry pulse system that utilizes according to claim 1 and 2 is for the method for Graphene fluorescence quantum, it is characterized in that described second electrode is working electrode or to electrode.
4. the galvanochemistry pulse system that utilizes according to claim 3 is for the method for Graphene fluorescence quantum, it is characterized in that describedly comprising platinum electrode or graphite electrode to electrode, and described contrast electrode comprises saturated calomel electrode or silver silver chloride electrode.
5. the galvanochemistry pulse system that utilizes according to claim 1 is for the method for Graphene fluorescence quantum, it is characterized in that described electrolytic solution is selected from acid solution, alkaline solution and neutral solution.
6. the galvanochemistry pulse system that utilizes according to claim 5 is for the method for Graphene fluorescence quantum, it is characterized in that described electrolytic solution is at least selected from and comprises KOH, NaOH, KCl, Na
2sO
4, H
2sO
4in the solution of the combination of any one or more.
7. the galvanochemistry pulse system that utilizes according to claim 1 and 2 is for the method for Graphene fluorescence quantum, it is characterized in that the span of described positive potential is 0V ~ 5V, and the span of negative potential is-5V ~ 0V.
8. the galvanochemistry pulse system that utilizes according to claim 2 is for the method for Graphene fluorescence quantum, it is characterized in that comprising: adopt centrifugation removing obtain sediment in mixed reaction solution, wherein centrifugal rotational speed is at more than 5000rpm.
9. the galvanochemistry pulse system that utilizes according to claim 1 is for the method for Graphene fluorescence quantum, it is characterized in that the particle diameter of described Graphene fluorescence quantum is 2 ~ 4nm.
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| CN105417537A (en) * | 2015-12-31 | 2016-03-23 | 焦云 | Device for quickly stripping graphene through synergistic effect of ultrasound and electric field and method for quickly stripping graphene by utilizing same |
| CN105417536A (en) * | 2015-12-31 | 2016-03-23 | 北京科技大学 | Method for preparing graphene quantum dots with adjustable oxygen content |
| CN105502369A (en) * | 2015-12-31 | 2016-04-20 | 北京科技大学 | Post redox treatment method for adjusting photoluminescent property of graphene quantum dots |
| CN105714323A (en) * | 2016-03-01 | 2016-06-29 | 常州大学 | Method for rapidly preparing fluorescent carbon quantum dot by using direct-current pulse process |
| CN105862057A (en) * | 2016-04-15 | 2016-08-17 | 北京科技大学 | Phosphorus-doped graphene quantum dot and electrochemistry preparing method thereof |
| CN106587018A (en) * | 2016-12-08 | 2017-04-26 | 山西大同大学 | Preparation method of graphene aggregate sol |
| CN107366003A (en) * | 2016-05-12 | 2017-11-21 | 成都中医药大学 | A kind of polymolecularity shuttle-type graphene oxide and preparation method thereof |
| 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 |
| CN109844183A (en) * | 2016-09-14 | 2019-06-04 | 爱法组装材料公司 | The manufacture of graphene |
| CN111606317A (en) * | 2020-07-03 | 2020-09-01 | 清华大学 | Nano fluorescent carbon dots and preparation method thereof |
| CN113260692A (en) * | 2018-09-07 | 2021-08-13 | 梦工厂株式会社 | Preparation method of graphene quantum dots |
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| CN105417536A (en) * | 2015-12-31 | 2016-03-23 | 北京科技大学 | Method for preparing graphene quantum dots with adjustable oxygen content |
| CN105502369A (en) * | 2015-12-31 | 2016-04-20 | 北京科技大学 | Post redox treatment method for adjusting photoluminescent property of graphene quantum dots |
| CN105417537A (en) * | 2015-12-31 | 2016-03-23 | 焦云 | Device for quickly stripping graphene through synergistic effect of ultrasound and electric field and method for quickly stripping graphene by utilizing same |
| CN105417536B (en) * | 2015-12-31 | 2018-02-27 | 北京科技大学 | A kind of preparation method of the adjustable graphene quantum dot of oxygen content |
| CN105714323A (en) * | 2016-03-01 | 2016-06-29 | 常州大学 | Method for rapidly preparing fluorescent carbon quantum dot by using direct-current pulse process |
| CN105714323B (en) * | 2016-03-01 | 2017-12-05 | 常州大学 | The method that dc-pulse method quickly prepares fluorescent carbon quantum dot |
| 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 |
| CN107366003A (en) * | 2016-05-12 | 2017-11-21 | 成都中医药大学 | A kind of polymolecularity shuttle-type graphene oxide and preparation method thereof |
| CN107366003B (en) * | 2016-05-12 | 2019-06-11 | 成都中医药大学 | A kind of polymolecularity shuttle-type graphene oxide and preparation method thereof |
| CN109844183A (en) * | 2016-09-14 | 2019-06-04 | 爱法组装材料公司 | The manufacture of graphene |
| CN115676813A (en) * | 2016-09-14 | 2023-02-03 | 爱法组装材料公司 | Manufacture of graphene |
| CN106587018A (en) * | 2016-12-08 | 2017-04-26 | 山西大同大学 | Preparation method of graphene aggregate sol |
| CN106587018B (en) * | 2016-12-08 | 2021-12-31 | 山西大同大学 | Preparation method of graphene aggregate sol |
| 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 |
| CN113260692A (en) * | 2018-09-07 | 2021-08-13 | 梦工厂株式会社 | Preparation method of graphene quantum dots |
| US11718531B2 (en) | 2018-09-07 | 2023-08-08 | Dxome Co., Ltd. | Method for producing graphene quantum dots |
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| CN111606317A (en) * | 2020-07-03 | 2020-09-01 | 清华大学 | Nano fluorescent carbon dots and preparation method thereof |
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