CN105152157A - Method for preparing solid light-emitting carbon point - Google Patents
Method for preparing solid light-emitting carbon point Download PDFInfo
- Publication number
- CN105152157A CN105152157A CN201510584511.7A CN201510584511A CN105152157A CN 105152157 A CN105152157 A CN 105152157A CN 201510584511 A CN201510584511 A CN 201510584511A CN 105152157 A CN105152157 A CN 105152157A
- Authority
- CN
- China
- Prior art keywords
- carbon point
- solid
- preparation
- solid luminescent
- luminescent carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Luminescent Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a method for preparing a solid light-emitting carbon point, namely, a method for preparing a solid light-emitting carbon point from cereal raw materials such as wheat flour, corn powder, rice powder, sorghum flour and millet flour as a C-containing precursor, and belongs to the field of preparation of nano materials. The method comprises the following steps: by taking cereal raw materials such as wheat flour as the C-containing precursor, preparing to obtain a precursor solution of certain concentration, and performing simple post-treatment under hydrothermal conditions without any chemical reagent, thereby achieving green synthesis of the carbon point which can emit light in both liquid and solid states. The method effectively solves the problems that the carbon point prepared by the traditional method emits light in a solution and the phenomenon of solid-state fluorescence quenching is caused after drying. The raw materials of the preparation method are cheap and easy to obtain, the synthesis route is simple, the raw materials are safe and non-toxic, and the product is completely green. The solid light-emitting carbon point prepared by using the method is powdery, easy to disperse, and beneficial for further utilization. The light can be emitted from the solid just like in a solution, and has obvious dependency of excitation wavelength.
Description
Technical field
The invention belongs to the preparation field of nano material, particularly a kind of preparation method of solid luminescent carbon point.
Background technology
Since Late Cambrian carbon point in 2004, carbon point with the optical property of its uniqueness, good water-soluble, be easy to functional modification, excellent chemical stability, bio-toxicity low, be easy to the advantages such as extensive synthesis and have been a great concern in fields such as bio-imaging, medicament transport, fluorescence sense, photoelectric devices.Current carbon point mainly contains physics synthesis method and chemical synthesis, and chemical synthesis mainly comprises: electrochemical synthesis, Microwave-assisted synthesis method, chemical oxidization method, high temperature pyrolytic cracking (HTP), hydrothermal synthesis method etc.
Hydrothermal synthesis method refers to and is placed in autoclave by containing C presoma, utilize material that a series of chemical reaction occurs in aqueous under high-temperature and high-pressure conditions and generate the fluorescent carbon quantum dot with the sub-productive rate of higher amount, products therefrom purity is high, and good dispersity, granularity are easy to control.A class is had to rely on hydrothermal method from natural organic matter, extract the reaction of carbon quantum dot at present.Egg, weeds, silk, leaf, orange juice etc. are natural to be widely used for as carbon source synthesis carbon quantum dot containing C organism.This kind of reaction raw materials is cheap and easy to get, and such natural organic matter safety non-toxic, have broad application prospects.
Due to the optical property of carbon nanomaterial uniqueness, it has huge application prospect in fields such as photoelectric devices.But the carbon point of having reported for work at present is all luminous inside solution mostly, and the Fluorescence-quenching that coagulation causes is ubiquitous in the drying process of carbon point.
Under solid state, lacking of luminous carbon point, limits it as the application of solid fluorescence powder in fields such as photoelectric devices.At present about the report of solid luminescence carbon point is also rarely found, only have some matrix materials based on carbon point to see and report for work.In these systems, in order to suppress the quenching of fluorescence of carbon point, carbon point is often dispersed in the matrix of the polymkeric substance such as PVP, PVA, PAA or glass gels.But the matrix material of this kind of system synthesis often has fixing pattern, and the easy film forming of polymkeric substance, is unfavorable for further dispersion; Changchun ray machine Shen Dezhen seminar reported first carbon quantum dot is doped in the matrix of starch, the amino on carbon quantum dot surface is by forming hydrogen bond with the hydroxyl on starch surface, can suppress the nonradiative transition of surface energy and then effectively suppress the Fluorescence-quenching of solid, the method has potential promotion meaning for the solids applications of carbon quantum dot.But the method is two step synthesis, and namely first synthesize carbon quantum dot, redispersion is in the matrix of starch, and synthesis cycle is long.Therefore, seek simple and fast and can be luminous under being easy to extensive synthesis of solid state carbon quantum dot be the task of top priority in this field.
Summary of the invention
In sum, for the deficiencies in the prior art, the invention provides a kind of simple and fast, safety non-toxic and be beneficial to the synthetic method of the solid luminescent carbon point of extensive synthesis.
A preparation method for solid luminescent carbon point, with parts by weight, comprises the following steps:
A. the cereal materials taking 0.8-3 parts is dispersed in the deionized water of 40-60ml and is made into the precursor solution that concentration is 0.02-0.05g/ml, stirs on magnetic stirring apparatus;
B. the precursor solution after stirring is proceeded in autoclave, carry out hydrothermal treatment consists;
C. by the product after hydro-thermal first through centrifugation, remove oarse-grained impurity, then use filter membrane secondary filtration, and collect filtrate;
D. the filtrate of gained is used cryodesiccated method, namely can obtain the powder of solid luminescent carbon point.
Further, described cereal materials is the one in flour, Semen Maydis powder, rice flour, sorghum meal, Semen setariae powder.
Further, the hydrothermal temperature of described hydrothermal treatment consists is 180 DEG C, and the time is 3-6h.
Further, the rotating speed of described centrifugation is 6000rpm, and centrifugation time is 10min.
Further, the secondary filtration in described step c, filter sizes used is 0.22 μm.
Further, described cryodesiccated temperature is-50 DEG C.
beneficial effect:
1, synthesis path of the present invention is simple, and materials safety is nontoxic, is green syt completely.
2, the solid luminescent carbon point that prepared by the present invention is Powdered, is easy to dispersion, is conducive to further utilization.Be different from traditional method be dispersed in the matrix of polymkeric substance, there is specific profile.
3, the pressed powder that prepared by the present invention has good water-soluble, and solid luminescence is as it is luminous in the aqueous solution, has the dependency of obvious excitation wavelength.
Accompanying drawing explanation
Fig. 1 is the in kind photo of carbon point before and after 365nm ultra violet lamp prepared by the present invention.
Fig. 2 is the XRD figure of carbon point prepared by the present invention
Fig. 3 is the fluorescence spectrum figure of carbon point prepared by the present invention
Fig. 4 is the spectrogram that the fluorescence emission peak of carbon point prepared by the present invention becomes with excitation wavelength.
Fig. 5 is the transmission electron microscope picture of carbon point prepared by the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated:
embodiment 1
A preparation method for solid luminescent carbon point, comprises the steps:
A, the sorghum meal taking 1.5g are dispersed in the deionized water of 60ml, are made into the precursor solution that concentration is 0.025g/ml, on magnetic stirring apparatus, fully stir 30min.
B, by stir after precursor solution put into autoclave, 180 DEG C of hydro-thermal 4h.
C, by reacted product with the centrifugal 10min of the centrifugation rate of 6000rpm, remove oarse-grained impurity, and collect filtrate; Be that the filtrate of filter membrane to previous step of 0.22 μm is filtered again with aperture,
D, collection filtrate, carry out lyophilize at-50 DEG C to filtrate.
See Fig. 1, be the in kind photo of solid carbon point before and after 365nm ultra violet lamp synthesized under this condition.As seen from the figure under ultra violet lamp, carbon point sends obvious macroscopic blue light.
See Fig. 2, it is the XRD figure of solid carbon point of synthesizing under this condition.
See Fig. 3, be the fluorescence spectrum figure of solid carbon point synthesized under this condition.
See Fig. 4, the spectrogram that the fluorescence emission peak for the carbon point of composite solid state under this condition becomes with excitation wavelength.
See Fig. 5 (a), it is the transmission electron microscope picture of the carbon point prepared under this condition.
embodiment 2:
A preparation method for solid luminescent carbon point, comprises the steps:
A, the rice flour taking 2.0g are dispersed in the deionized water of 50ml, are made into the precursor solution that concentration is 0.04g/ml, on magnetic stirring apparatus, fully stir 30min.
B, by stir after precursor solution proceed in autoclave, 180 DEG C of hydro-thermal 3h.
C, by reacted product with the centrifugal 10min of the centrifugation rate of 6000rpm, remove oarse-grained impurity, then filter with the filter membrane that aperture is 0.22 μm;
D, filtrate collection, at-50 DEG C, lyophilize is carried out to filtrate.
See Fig. 5 (b), be prepare under this condition carbon point transmission electron microscope picture.
embodiment 3:
A preparation method for solid luminescent carbon point, comprises the steps:
A, the Semen Maydis powder taking 2.0g are dispersed in the deionized water of 40ml, are made into the precursor solution that concentration is 0.05g/ml, on magnetic stirring apparatus, fully stir 30min.
B, by stir after precursor solution proceed in autoclave, hydro-thermal 4h at 180 DEG C.
C, by reacted product with the centrifugal 10min of the centrifugation rate of 6000rpm, go out oarse-grained impurity, then filter with the filter membrane that aperture is 0.22 μm.
D, collection filtrate, carry out lyophilize at-50 DEG C to filtrate.
See Fig. 5 (c), it is the transmission electron microscope picture of the carbon point prepared under this condition.
embodiment 4:
A preparation method for solid luminescent carbon point, comprises the steps:
A, take 2.0g flour and be dispersed in the deionized water of 40ml, be made into the precursor solution that concentration is 0.04g/ml, on magnetic stirring apparatus, fully stir 30min.
B, by stir after precursor solution proceed in autoclave, hydro-thermal 4h at 180 DEG C.
C, by reacted product with the centrifugal 10min of the centrifugation rate of 6000rpm, go out oarse-grained impurity, then filter with the filter membrane that aperture is 0.22 μm.
D, collection filtrate, carry out lyophilize at-50 DEG C to filtrate.
See Fig. 5 (d), it is the transmission electron microscope picture of the carbon point prepared under this condition.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (6)
1. a preparation method for solid luminescent carbon point, is characterized in that, with parts by weight, comprises the following steps:
A. the cereal materials taking 0.8-3 parts is dispersed in the deionized water of 40-60ml and is made into the precursor solution that concentration is 0.02-0.05g/ml, stirs on magnetic stirring apparatus;
B. the precursor solution after stirring is proceeded in autoclave, carry out hydrothermal treatment consists;
C. by the product after hydro-thermal first through centrifugation, remove oarse-grained impurity, then use filter membrane secondary filtration, and collect filtrate;
D. the filtrate of gained is used cryodesiccated method, namely can obtain the powder of solid luminescent carbon point.
2. the preparation method of a kind of solid luminescent carbon point according to claim 1, is characterized in that described cereal materials is the one in flour, Semen Maydis powder, rice flour, sorghum meal, Semen setariae powder.
3. the preparation method of a kind of solid luminescent carbon point according to claim 1, is characterized in that: the hydrothermal temperature of described hydrothermal treatment consists is 180 DEG C, and the time is 3-6h.
4. the preparation method of a kind of solid luminescent carbon point according to claim 1, is characterized in that: the rotating speed of described centrifugation is 6000rpm, and centrifugation time is 10min.
5. the preparation method of a kind of solid luminescent carbon point according to claim 1, it is characterized in that: the secondary filtration in described step c, filter sizes used is 0.22 μm.
6. the preparation method of a kind of solid luminescent carbon point according to claim 1, is characterized in that: described cryodesiccated temperature is-50 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510584511.7A CN105152157B (en) | 2015-09-15 | 2015-09-15 | Method for preparing solid light-emitting carbon point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510584511.7A CN105152157B (en) | 2015-09-15 | 2015-09-15 | Method for preparing solid light-emitting carbon point |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105152157A true CN105152157A (en) | 2015-12-16 |
| CN105152157B CN105152157B (en) | 2017-04-12 |
Family
ID=54793287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510584511.7A Expired - Fee Related CN105152157B (en) | 2015-09-15 | 2015-09-15 | Method for preparing solid light-emitting carbon point |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105152157B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419792A (en) * | 2015-12-28 | 2016-03-23 | 江南大学 | Preparation method of carbon dots soluble in water phase and organic phase |
| CN105542759A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing fluorescence carbon dots based on sweet potato extract |
| CN105542761A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing fluorescence carbon dots taking rice bran as carbon source |
| CN105647529A (en) * | 2016-03-09 | 2016-06-08 | 沈阳大学 | Method for preparing carbon-dot solid-state fluorescent powder |
| CN108069414A (en) * | 2017-12-19 | 2018-05-25 | 重庆文理学院 | A kind of method for preparing carbon nanomaterial using discarded pine tree tower |
| CN108101022A (en) * | 2017-12-27 | 2018-06-01 | 重庆文理学院 | A kind of method that carbon quantum dot is prepared using fennel seeds as raw material |
| CN110724528A (en) * | 2019-11-07 | 2020-01-24 | 东北林业大学 | Rosin-based carbon dot material and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588189A (en) * | 2013-07-04 | 2014-02-19 | 上海交通大学 | Egg-based method for realizing hydrothermal synthesis of carbon quantum dots |
| CN104340965A (en) * | 2014-10-17 | 2015-02-11 | 中国科学技术大学 | Macroscopic preparation method of fluorescent carbon quantum dots |
| CN104555978A (en) * | 2013-10-17 | 2015-04-29 | 中国科学院理化技术研究所 | Preparation method of photoluminescence carbon quantum dots |
| CN104591124A (en) * | 2014-12-10 | 2015-05-06 | 西南交通大学 | Preparation method for fluorescent carbon quantum dot with vitamin as carbon source |
-
2015
- 2015-09-15 CN CN201510584511.7A patent/CN105152157B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588189A (en) * | 2013-07-04 | 2014-02-19 | 上海交通大学 | Egg-based method for realizing hydrothermal synthesis of carbon quantum dots |
| CN104555978A (en) * | 2013-10-17 | 2015-04-29 | 中国科学院理化技术研究所 | Preparation method of photoluminescence carbon quantum dots |
| CN104340965A (en) * | 2014-10-17 | 2015-02-11 | 中国科学技术大学 | Macroscopic preparation method of fluorescent carbon quantum dots |
| CN104591124A (en) * | 2014-12-10 | 2015-05-06 | 西南交通大学 | Preparation method for fluorescent carbon quantum dot with vitamin as carbon source |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419792A (en) * | 2015-12-28 | 2016-03-23 | 江南大学 | Preparation method of carbon dots soluble in water phase and organic phase |
| CN105542759A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing fluorescence carbon dots based on sweet potato extract |
| CN105542761A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing fluorescence carbon dots taking rice bran as carbon source |
| CN105647529A (en) * | 2016-03-09 | 2016-06-08 | 沈阳大学 | Method for preparing carbon-dot solid-state fluorescent powder |
| CN105647529B (en) * | 2016-03-09 | 2018-04-13 | 沈阳大学 | A kind of preparation method of carbon dots solid phosphor |
| CN108069414A (en) * | 2017-12-19 | 2018-05-25 | 重庆文理学院 | A kind of method for preparing carbon nanomaterial using discarded pine tree tower |
| CN108101022A (en) * | 2017-12-27 | 2018-06-01 | 重庆文理学院 | A kind of method that carbon quantum dot is prepared using fennel seeds as raw material |
| CN110724528A (en) * | 2019-11-07 | 2020-01-24 | 东北林业大学 | Rosin-based carbon dot material and preparation method and application thereof |
| CN110724528B (en) * | 2019-11-07 | 2020-08-11 | 东北林业大学 | Rosin-based carbon dot material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105152157B (en) | 2017-04-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105152157A (en) | Method for preparing solid light-emitting carbon point | |
| Du et al. | The rapid and large‐scale production of carbon quantum dots and their integration with polymers | |
| Wang et al. | Synthesis and applications of red‐emissive carbon dots | |
| Zhang et al. | Tricolor white-light-emitting carbon dots with multiple-cores@ shell structure for WLED application | |
| CN106044743B (en) | A kind of preparation method and applications of the Water-soluble carbon quantum dot based on egg shell membrane | |
| He et al. | Construction and multifunctional applications of visible-light-excited multicolor long afterglow carbon dots/boron oxide composites | |
| Gong et al. | A novel rapid and green synthesis of highly luminescent carbon dots with good biocompatibility for cell imaging | |
| CN109385273B (en) | Ultra-long-life room temperature phosphorescent material, and preparation method and application thereof | |
| CN102180459B (en) | Method for preparing carbon quantum dots | |
| Zhu et al. | Carbon dots with efficient solid-state red-light emission through the step-by-step surface modification towards light-emitting diodes | |
| CN105647526A (en) | Near-full-spectrum fluorescent nanocarbon dots and preparation method thereof | |
| CN104591124A (en) | Preparation method for fluorescent carbon quantum dot with vitamin as carbon source | |
| CN103848410A (en) | Hydrothermal preparation method of fluorescent carbon quantum dots | |
| CN103303902A (en) | Preparation method of environment-friendly economic luminescent carbon quantum dot | |
| CN108128767A (en) | A kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment | |
| CN106497560B (en) | The controllable carbon dots based compound nano material and the preparation method and application thereof of luminescent properties | |
| CN103864055A (en) | Method for rapidly preparing fluorescent carbon dots | |
| CN105694888A (en) | Mg2+ doped NaREF4 upconversion fluorescence material and preparation method thereof | |
| CN105594739A (en) | Visible light catalysis compound antibacterial material and preparation method therefor | |
| AU2021100604A4 (en) | Preparations of ultrahigh fluorescence quantum yield carbon dots, carbon dots/PVA phosphor film and the LED application of the phosphor film | |
| CN104263366A (en) | Red-light emission fluorescent carbon dot with up and down conversion function and preparation method of red-light emission fluorescent carbon dot | |
| CN113913186B (en) | Carbon dot-based room-temperature phosphorescent composite material capable of stably emitting afterglow and preparation method, application and use method thereof | |
| CN109988571A (en) | A kind of preparation of solid state fluorescence carbon quantum dot material and application | |
| CN104059644A (en) | Simple and quick preparation method of nitrogen-doped carbon quantum dots | |
| Han et al. | Seeking eye protection from biomass: Carbon dot-based optical blocking films with adjustable levels of blue light blocking |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170412 Termination date: 20190915 |