CN105502340A - Preparation method of fluorescent carbon dots - Google Patents
Preparation method of fluorescent carbon dots Download PDFInfo
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- CN105502340A CN105502340A CN201511023736.1A CN201511023736A CN105502340A CN 105502340 A CN105502340 A CN 105502340A CN 201511023736 A CN201511023736 A CN 201511023736A CN 105502340 A CN105502340 A CN 105502340A
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Abstract
The invention provides a preparation method of fluorescent carbon quantum dots, belongs to the technical field of preparation of nanomaterials, particularly relates to a preparation method of a fluorescent material, and aims at solving the problems that an existing semiconductor quantum dot and organic dye preparation method is fussy, high in price and unfriendly to environment, and photo-bleaching is easily generated. The method comprises the following steps: (1) with crystalline flake graphite as a raw material, preparing graphite oxide (GOFe) by a K2FeO4 oxidation method; and (2) with graphite oxide powder as the raw material, preparing the carbon quantum dots (CDots) by a microwave hydrothermal method. The method provided by the invention is simple and clear in synthetic process, high in efficiency and short in period; the obtained carbon quantum dots are high in purity and small in particle sizes and have monodispersity, water solubility and up-conversion and down-conversion fluorescence characteristics; and the prepared fluorescent carbon quantum dots are applied to biological fluorescent labeling and solar hydrogen production.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of preparation method of fluorescent material.
Background technology
Broadly say, fluorescent carbon quantum dot is divided into three kinds: Nano diamond, fluorescent carbon nano particle and graphene quantum dot.Wherein fluorescent carbon nano particle is commonly referred to as carbon quantum dot.Carbon quantum dot is most important one in fluorescent carbon nano material, also referred to as carbon point, carbon nano dot, carbon nano-crystal, carbon back point, be size at below 10nm, monodispersed, geometrical shape is close to a kind of emerging carbon nano-functional material of accurate ball-type.In 2004, Scrivens group carried out in the electrophoresis experiment process of purifying single armed carbon nanotube, surprisingly obtained this product with photoluminescent property.2006, sun etc. utilized the method for laser ablation to prepare the very little nanoparticle of size of particles, then use polymer P EG
1500Ncarry out passivation, obtain the fluorescent substance that visible region is adjustable.Cause the interest that increasing investigator studies this fluorescent carbon nano particle thus.Before carbon quantum dot occurs, investigator thinks that carbon material has very low water-soluble and bad fluorescence property mostly.Therefore the fluorescence property of carbon quantum dot excellence receives the favor of investigator.The raw materials of carbon quantum dot is extensive, and preparation method is varied, and in research in recent years, carbon quantum dot becomes the nova in carbon material family gradually.
By the effort of more than ten years, scientist explores the preparation method of carbon quantum dot, have studied the character of carbon quantum dot, has opened up the practical application of carbon quantum dot.Can fluorescent quenching be there is in the carbon quantum dot in solution with photoluminescent property under the effect of electron donor or electron donor, carbon quantum dot is this is subject to the radiation of light and the transfer transport phenomenon occurred, and carbon quantum dot can be played a significant role in transform light energy and related application.Particularly, except normal or can be described as except the carbon quantum dot of down-conversion fluorescent character, the discovery with the carbon quantum dot of up-conversion fluorescence character makes the photocatalyst of the catalyst system taking carbon quantum dot as base to design, thus effectively utilizes sun power entirely to compose.
Relative to traditional semiconductor-quantum-point and organic dye, (preparation method is loaded down with trivial details, expensive, environment is unfriendly, easily photobleaching etc. occurs), fluorescent carbon quantum dot particle diameter is little, good water solubility, unreactiveness is high, is easy to functionalization, resistance to photobleaching, hypotoxicity, and there is good biocompatibility.Therefore increasing investigator is by its required bio-imaging and cell marking.Recently, investigator has prepared the carbon quantum dot under near infrared light excites with photoluminescent property.Thisly excited by near infrared light that to produce the carbon quantum dot of fluorescence phenomenon unusual at the research application value of in vivo marker.
Summary of the invention
The present invention will solve existing semiconductor-quantum-point and organic dye preparation method is loaded down with trivial details, and expensive, environment is unfriendly, the problem of photobleaching easily occurs, and provides a kind of preparation method of fluorescent carbon quantum dot.
A kind of preparation method of fluorescent carbon quantum dot carries out according to the following steps:
One, be add K in the vitriol oil of 95% ~ 98% to mass concentration under the condition of stirring at room temperature
2feO
4and natural flake graphite, churning time is 1h ~ 1.5h, obtains reaction solution, carries out centrifugation to reaction solution, obtains liquid and precipitation, liquids recovery, and to pelleting centrifugation washing 3 ~ 5 times, standing and drying, obtains graphite oxide powder; Described K
2feO
4quality and mass concentration be the volume ratio of the vitriol oil of 95% ~ 98% be 1kg:(30 ~ 50) L; The quality of described natural flake graphite and mass concentration are the volume ratio of the vitriol oil of 95% ~ 98% is 1kg:(5 ~ 10) L;
Two, graphite oxide powder step 2 obtained and concentration be 65% ~ 68% concentrated nitric acid be mixed to join in microwave reactor carry out microwave hydrothermal reaction under temperature be the condition of 80 DEG C ~ 150 DEG C, reaction times is 15min ~ 60min, obtain solution, solution is cooled to room temperature, adopt sodium carbonate that the pH of solution is adjusted to 7, centrifugation obtains supernatant liquor, dialyses to supernatant liquor, by inner side solution lyophilize after dialysis, obtain carbon quantum dot; The quality of the graphite oxide powder that described step 2 obtains and concentration are the volume ratio of the concentrated nitric acid of 65% ~ 68% is 1kg:(20 ~ 40) L.
The invention has the beneficial effects as follows:
Preparation cycle of the present invention is short, and efficiency is high, and technique is simple and clear, easy and simple to handle, and can prepare in a large number.Starting material are natural flake graphite, and natural flake graphite is general reagent, wide material sources, low price.Production unit is microwave reactor, easy to operate, can complete fast, energy-and time-economizing in 1 hour, and can produce in a large number simultaneously.Product carbon quantum dot has upper conversion and lower conversion fluorescence property, can by regulating reaction parameter and to product separation, preparing the carbon quantum dot with upper conversion and lower conversion fluorescent characteristic.
Accompanying drawing explanation
Fig. 1 is the TEM photo of the carbon quantum dot that embodiment one obtains;
Fig. 2 is the lower conversion fluorescence spectrum of carbon quantum dot under 354nm excitation wavelength that embodiment one obtains;
Fig. 3 is the TEM photo of the carbon quantum dot that embodiment two obtains;
Fig. 4 is the upper conversion fluorescence spectrum of carbon quantum dot under 962nm excitation wavelength that embodiment two obtains.
Embodiment
Embodiment one: the preparation method of a kind of fluorescent carbon quantum dot of present embodiment carries out according to the following steps:
One, be add K in the vitriol oil of 95% ~ 98% to mass concentration under the condition of stirring at room temperature
2feO
4and natural flake graphite, churning time is 1h ~ 1.5h, obtains reaction solution, carries out centrifugation to reaction solution, obtains liquid and precipitation, liquids recovery, and to pelleting centrifugation washing 3 ~ 5 times, standing and drying, obtains graphite oxide powder; Described K
2feO
4quality and mass concentration be the volume ratio of the vitriol oil of 95% ~ 98% be 1kg:(30 ~ 50) L; The quality of described natural flake graphite and mass concentration are the volume ratio of the vitriol oil of 95% ~ 98% is 1kg:(5 ~ 10) L;
Two, graphite oxide powder step one obtained and concentration be 65% ~ 68% concentrated nitric acid be mixed to join in microwave reactor carry out microwave hydrothermal reaction under temperature be the condition of 80 DEG C ~ 150 DEG C, reaction times is 15min ~ 60min, obtain solution, solution is cooled to room temperature, the pH of solution is adjusted to 7, and centrifugation obtains supernatant liquor, dialyses to supernatant liquor, the solution lyophilize be retained down inner side after dialysis, obtains carbon quantum dot; The quality of the graphite oxide powder that described step one obtains and concentration are the volume ratio of the concentrated nitric acid of 65% ~ 68% is 1kg:(20 ~ 40) L.
Embodiment two: present embodiment and embodiment one are unlike K described in step one
2feO
4quality and mass concentration be the volume ratio of the vitriol oil of 95% ~ 98% be 1kg:40L.Other are identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the quality of natural flake graphite described in step one and mass concentration are the volume ratio of the vitriol oil of 95% ~ 98% is 6kg:40L.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: be carry out microwave hydrothermal reaction under the condition of 100 DEG C in temperature in step 2.Other are identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: in step 2, the reaction times is 40min.Other are identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: the quality of the graphite oxide powder that step one described in step 2 obtains and concentration are the volume ratio of the concentrated nitric acid of 65% ~ 68% is 1kg:30L.Other are identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: the cutoff of dialysis tubing adopted of dialysing described in step 2 is 1000 ~ 4000.Other are identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: the time of dialysing described in step 2 is 24h ~ 48h.Other are identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight are unlike cryodesiccated time 12h ~ 24h described in step 2.Other are identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: described in step 2, the pH of solution is adjusted to 7 adopt anhydrous sodium carbonates carry out.Other are identical with one of embodiment one to nine.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one: a kind of preparation method of fluorescent carbon quantum dot carries out according to the following steps:
One, be add 6gK in the vitriol oil of 98% to 100mL mass concentration under the condition of stirring at room temperature
2feO
4with 1g natural flake graphite, churning time is 1h, obtains reaction solution, carries out centrifugation to reaction solution, obtains liquid and precipitation, liquids recovery, washs 4 times, standing and drying to pelleting centrifugation, obtains graphite oxide powder;
Two, graphite oxide powder 0.2g step one obtained and 6mL concentration be 65% concentrated nitric acid be mixed to join in microwave reactor carry out microwave hydrothermal reaction under temperature be the condition of 120 DEG C, reaction times is 45min, obtain solution, solution is cooled to room temperature, adopt anhydrous sodium carbonate that the pH of solution is adjusted to 7, centrifugation obtains supernatant liquor, the dialysis tubing that supernatant liquor employing cutoff is 1000 is dialysed, the solution lyophilize 24h be retained down inner side after dialysis 48h, obtains carbon quantum dot.
Fig. 1 is the TEM photo of the carbon quantum dot that embodiment one obtains; As shown in Figure 1, carbon quantum dot is a kind of almost spherical, favorable dispersity, and particle diameter is nano particle between 1 ~ 10nm.
Fig. 2 is the lower conversion fluorescence spectrum of carbon quantum dot under 354nm excitation wavelength that embodiment one obtains; As shown in Figure 2, carbon quantum dot has the characteristic of lower conversion fluorescence, and can be that the phototransformation of 354nm is the light of wavelength in 450 ~ 650nm scope by excitation wavelength, the fluorescent wavelength ranges after conversion be wider.
Embodiment two: a kind of preparation method of fluorescent carbon quantum dot carries out according to the following steps:
One, be add 6gK in the vitriol oil of 98% to 100mL mass concentration under the condition of stirring at room temperature
2feO
4with 1g natural flake graphite, churning time is 1.2h, obtains reaction solution, carries out centrifugation to reaction solution, obtains liquid and precipitation, liquids recovery, washs 4 times, standing and drying to pelleting centrifugation, obtains graphite oxide powder;
Two, graphite oxide powder 0.2g step one obtained and 6mL concentration be 65% concentrated nitric acid be mixed to join in microwave reactor carry out microwave hydrothermal reaction under temperature be the condition of 140 DEG C, reaction times is 30min, obtain solution, solution is cooled to room temperature, adopt anhydrous sodium carbonate that the pH of solution is adjusted to 7, centrifugation obtains supernatant liquor, the dialysis tubing that supernatant liquor employing cutoff is 3500 is dialysed, the solution lyophilize 24h be retained down inner side after dialysis 48h, obtains carbon quantum dot.
Fig. 3 is the TEM photo of the carbon quantum dot that embodiment two obtains; As shown in Figure 3, carry out high resolution transmission electron microscopy sign to carbon quantum dot, display carbon quantum dot crystalline structure is perfect, demonstrates carbon quantum dot and has crystalline structure.
Fig. 4 is the upper conversion fluorescence spectrum of the carbon quantum dot that embodiment two obtains; As shown in Figure 4, carbon quantum dot has the characteristic of upper conversion fluorescence, and can be that the phototransformation of 962nm is the light of wavelength in 540-680nm scope by excitation wavelength, the fluorescent wavelength ranges after conversion be wider.
Claims (10)
1. a preparation method for fluorescent carbon quantum dot, is characterized in that the preparation method of fluorescent carbon quantum dot carries out according to the following steps:
One, be add K in the vitriol oil of 95% ~ 98% to mass concentration under the condition of stirring at room temperature
2feO
4and natural flake graphite, churning time is 1h ~ 1.5h, obtains reaction solution, carries out centrifugation to reaction solution, obtains liquid and precipitation, liquids recovery, and to pelleting centrifugation washing 3 ~ 5 times, standing and drying, obtains graphite oxide powder; Described K
2feO
4quality and mass concentration be the volume ratio of the vitriol oil of 95% ~ 98% be 1kg:(30 ~ 50) L; The quality of described natural flake graphite and mass concentration are the volume ratio of the vitriol oil of 95% ~ 98% is 1kg:(5 ~ 10) L;
Two, graphite oxide powder step one obtained and concentration be 65% ~ 68% concentrated nitric acid be mixed to join in microwave reactor carry out microwave hydrothermal reaction under temperature be the condition of 80 DEG C ~ 150 DEG C, reaction times is 15min ~ 60min, obtain solution, solution is cooled to room temperature, the pH of solution is adjusted to 7, and centrifugation obtains supernatant liquor, dialyses to supernatant liquor, the solution lyophilize be retained down inner side after dialysis, obtains carbon quantum dot; The quality of the graphite oxide powder that described step one obtains and concentration are the volume ratio of the concentrated nitric acid of 65% ~ 68% is 1kg:(20 ~ 40) L.
2. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that K described in step one
2feO
4quality and mass concentration be the volume ratio of the vitriol oil of 95% ~ 98% be 1kg:40L.
3. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that the quality of natural flake graphite described in step one and mass concentration be the volume ratio of the vitriol oil of 95% ~ 98% are 6kg:40L.
4. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that under temperature is the condition of 100 DEG C, carrying out microwave hydrothermal reaction in step 2.
5. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that in step 2, the reaction times is 40min.
6. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that the quality of the graphite oxide powder that step one described in step 2 obtains and concentration be the volume ratio of the concentrated nitric acid of 65% ~ 68% are 1kg:30L.
7. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, the cutoff of the dialysis tubing adopted that it is characterized in that dialysing described in step 2 is 1000 ~ 4000.
8. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that the time of dialysing described in step 2 is 24h ~ 48h.
9. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that cryodesiccated time 12h ~ 24h described in step 2.
10. the preparation method of a kind of fluorescent carbon quantum dot according to claim 1, is characterized in that described in step 2, the pH of solution being adjusted to 7 adopts anhydrous sodium carbonate to carry out.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880881A (en) * | 2017-11-27 | 2018-04-06 | 陕西科技大学 | A kind of preparation method of carbon quantum dot |
| CN109097035A (en) * | 2018-08-31 | 2018-12-28 | 中国石油大学(北京) | Carbon quantum dot and its preparation and application with high fluorescent characteristic |
| CN109437154A (en) * | 2018-10-25 | 2019-03-08 | 河南理工大学 | A method of the controllable carbon quantum dot of energy band is prepared by raw material of coal |
| CN109588375A (en) * | 2018-11-02 | 2019-04-09 | 大连工业大学 | Fluorescent natural silk preparation method based on Spanish mackerel internal organ and the compound carbon dots of mulberry leaf |
| CN113788479A (en) * | 2021-10-29 | 2021-12-14 | 凯盛石墨碳材料有限公司 | Preparation method of graphite-based quantum dots |
| WO2023194683A1 (en) * | 2022-04-06 | 2023-10-12 | Université De Lorraine | Solid-state fluorescent graphene-based quantum dots |
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| CN103738941A (en) * | 2013-11-14 | 2014-04-23 | 盐城增材科技有限公司 | Graphene quantum dot preparation method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880881A (en) * | 2017-11-27 | 2018-04-06 | 陕西科技大学 | A kind of preparation method of carbon quantum dot |
| CN109097035A (en) * | 2018-08-31 | 2018-12-28 | 中国石油大学(北京) | Carbon quantum dot and its preparation and application with high fluorescent characteristic |
| CN109097035B (en) * | 2018-08-31 | 2020-11-10 | 中国石油大学(北京) | Carbon quantum dot with high fluorescence characteristic and preparation and application thereof |
| CN109437154A (en) * | 2018-10-25 | 2019-03-08 | 河南理工大学 | A method of the controllable carbon quantum dot of energy band is prepared by raw material of coal |
| CN109437154B (en) * | 2018-10-25 | 2020-12-11 | 河南理工大学 | Method for preparing energy band controllable carbon quantum dots by taking coal as raw material |
| CN109588375A (en) * | 2018-11-02 | 2019-04-09 | 大连工业大学 | Fluorescent natural silk preparation method based on Spanish mackerel internal organ and the compound carbon dots of mulberry leaf |
| CN113788479A (en) * | 2021-10-29 | 2021-12-14 | 凯盛石墨碳材料有限公司 | Preparation method of graphite-based quantum dots |
| WO2023194683A1 (en) * | 2022-04-06 | 2023-10-12 | Université De Lorraine | Solid-state fluorescent graphene-based quantum dots |
| FR3134385A1 (en) * | 2022-04-06 | 2023-10-13 | Université De Lorraine | Quantum dots based on solid-state fluorescent graphene |
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