CN103274388B - Fluorescent carbon quantum dot preparation method - Google Patents
Fluorescent carbon quantum dot preparation method Download PDFInfo
- Publication number
- CN103274388B CN103274388B CN201310219900.0A CN201310219900A CN103274388B CN 103274388 B CN103274388 B CN 103274388B CN 201310219900 A CN201310219900 A CN 201310219900A CN 103274388 B CN103274388 B CN 103274388B
- Authority
- CN
- China
- Prior art keywords
- quantum dot
- carbon quantum
- leaf
- fluorescent carbon
- gained
- 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.)
- Active
Links
Landscapes
- Luminescent Compositions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to fluorescent carbon quantum dot preparation method, comprise the following steps: the first step: collect plant leaf, and wash only, dry; Second step, carries out calcination process by the clean blade of process, obtains black solid; 3rd step, is ground into powder black solid, and dispersion in a solvent, obtains finely dispersed suspension liquid after magnetic agitation and supersound process; 4th step: by centrifugal for gained suspension liquid or carry out separating treatment with filter membrane, removing precipitation, obtains clear liquid; 5th step; Solvent in removing gained clear liquid, gained solid is fluorescent carbon quantum dot.The inventive method starting material can adopt various plant leaf, wide material sources; Preparation is simple.
Description
Technical field
The present invention relates to a kind of fluorescent carbon quantum dot preparation method, especially a kind of take plant leaf as the fluorescent carbon quantum dot preparation method originated.
Background technology
Fluorescent nano particles, with the optics of its excellence and electric property, is with a wide range of applications in the field such as biological medicine and photoelectric device.Nearest investigators find typical fluorescent nano particles, as CdTe, CdSe, the semiconductor-quantum-point materials such as PbS, due to containing heavy metal element, not only toxic side effect is produced to organism, and severe contamination can be produced to environment, greatly limit such quantum dot in application that is biological and field of Environment Protection.
Carbon quantum dot is a kind of new carbon found in 2004, relative to traditional semiconductor-quantum-point and organic dye, newcomer in this Wei Tan family not only maintains the advantages such as carbon material toxicity is little, good biocompatibility, but also have that light emitting region is adjustable, two photon absorption cross section is large, good light stability, without optical flare, be easy to functionalization, inexpensive, the easy unrivaled advantage such as synthesis on a large scale.The method that current report prepares carbon quantum dot mainly comprises laser apparatus bombardment method of stripping, microwave process for synthesizing, electrochemical oxidation process, chemical oxidization method and high temperature pyrolytic cracking (HTP) etc., and the raw material of employing mainly contains Graphene, carbon nanotube, gac, candle ash and micromolecular compound etc.But, these Measures compare are complicated and consuming time, the raw material adopted is most costly, and product needs, through the stable optical property of the means guarantee carbon quantum dot such as strong acid reflow treatment or finishing, to limit scale operation and the practical application of fluorescent carbon quantum dot.Therefore, find raw material that is cheap and easy to get, Nantural non-toxic, the fluorescent carbon quantum dot utilizing simple and easy effective means to prepare excellent in optical properties fast seems particularly necessary.
In recent years, adopt natural matter to prepare fluorescent carbon quantum dot to attract attention.Such as, application number is that the Chinese invention patent application of 201110049051.X publication No. CN102180459A discloses a kind of to take plant haulm as the fluorescent carbon quantum dot preparation method of raw material, mainly comprise the following steps: the heat starting material in 350 DEG C-450 DEG C in tubular oven obtain soot; In salpeter solution, returned acid boils 10-12 hour; Solid product is obtained except anhydrating; Be incorporated in 105 DEG C-135 DEG C react 48-72 hour with polyoxyethylene glycol and deionized water are mixed; Carbon quantum dot is obtained after centrifugal.Although the starting material in this preparation method are cheap and easy to get, processing step is loaded down with trivial details, high to equipment requirements, and length consuming time, is unfavorable for large-scale production.
Application number is that the Chinese invention patent application of 201210264411.2 publication No. CN102745669A discloses a kind of bean dregs of soybean after squeezing soya-bean milk that utilize as the fluorescent carbon quantum dot preparation method of raw material, mainly comprises the following steps: raw material drying dehydration is obtained bean dregs powder; In 200 DEG C of heating 20-40min carbonization; Grind the meal that sieves to obtain; To be scattered in deionized water and evaporation concentration; By concentrated solution in-50 DEG C of lyophilizes, obtain fluorescent carbon quantum dot.Although the technique of the method is relatively simple, need to carry out pre-treatment to starting material, and lyophilize step improves production cost.In addition, the granularity uniformity of carbon quantum dot obtained in embodiment is poor, and particle size range is wider, about 3-12 μm.
Summary of the invention
Technical problem to be solved by this invention is: overcome prior art Problems existing, and provide a kind of fluorescent carbon quantum dot preparation method, its starting material can adopt various plant leaf, wide material sources; Preparation is simple.
The invention provides a kind of fluorescent carbon quantum dot preparation method, it is characterized in that comprising the following steps:
The first step, collect plant leaf, and cleaned, dry;
Second step, the first step gained blade is placed in quartz boat, then quartz boat is placed in tube furnace silica tube, carries out calcination process pass into nitrogen in tube furnace after, after cooling, obtain black solid;
3rd step, be ground into powder by second step gained black solid, dispersion in a solvent, is carried out supersound process, is obtained finely dispersed suspension liquid after magnetic agitation at least 10min;
4th step, by centrifugal for the 3rd step gained suspension liquid or carry out separating treatment with filter membrane, removing precipitation, obtains clear liquid;
Solvent in 5th step, removing the 4th step gained clear liquid, gained solid is fluorescent carbon quantum dot.
The perfect further technical scheme of the present invention is as follows:
Preferably, in the first step, described plant leaf is the Leaf of Camphortree of ovalize, or be the Rhizoma Dioscoreae esculentae leaf in heart or leaf of leading a cow, or be the Chinese parasol leaf in palm shape, or for being fan-shaped ginkgo leaf, or for being lance-shaped peach leaves, Folium Pterocaryae or the leaf of bamboo, or be rounded lotus leaf or lotus leaf, or in the pine needle of aciculiform, or for assuming diamond in shape, squama shape, cochlear or leg-of-mutton blade.
Preferably, in second step, described tube furnace calcination temperature is 100 ° of C-500 ° of C, and heating rate is 5 ° of C/min, and the treatment time is 1-5h.
Preferably, in the 3rd step, described solvent is one of water, ethanol, tetracol phenixin, trichloromethane, methylene dichloride, tetrahydrofuran (THF), normal hexane, acetone, toluene, N, N'-DMAA, sherwood oil; In gained suspension liquid, the massfraction of black solid is 0.1-5g/L.
Preferably, in the 3rd step, described supersound process adopts 100w power ultrasonic cleaning apparatus, and ultrasonic frequency is 40kHz, and ultrasonic time is 10-180min.
Preferably, in the 4th step, the centrifugal speed of described centrifugal treating is 8000-14000rpm, and centrifugation time is 5-15min; Described filter membrane process employing aperture is the filter membrane of 0.1-2 μm.
Preferably, in the 5th step, adopt drying mode except desolventizing, bake out temperature is 50 ° of C.
Beneficial effect of the present invention is as follows:
1, fluorescent carbon quantum dot preparation method required equipment provided by the invention is simple, easy to operate, raw material sources extensively, Nantural non-toxic, cheap and easy to get.
2, to obtain the emissive porwer of fluorescent carbon quantum dot adjustable with calcination temperature in the present invention, and have higher luminous efficiency and stable glimmering energy, and glow color is adjustable with excitation wavelength, particle diameter is less than 5 nanometers, and Relative Size is homogeneous.
3, the present invention obtains fluorescent carbon quantum dot and can be used as nanometer ink for spray ink Printing field, also can be used for field of LED illumination and the biologic applications such as biomarker, living imaging.
Accompanying drawing explanation
Fig. 1 is ultra-violet absorption spectrum and the fluorescent reflection spectrum that case 1 of the present invention obtains fluorescent carbon quantum dot.
Fig. 2 is the spectrogram (by 360nm to 500nm, step-length is 20nm to excitation wavelength) that fluorescent reflection curve that case 1 of the present invention obtains fluorescent carbon quantum dot changes with excitation wavelength.
Fig. 3 is the transmission electron microscope picture that case 1 of the present invention obtains fluorescent carbon quantum dot.
Fig. 4 is the infrared spectrogram that case 1 of the present invention obtains fluorescent carbon quantum dot.
Embodiment
With reference to the accompanying drawings and the present invention is described in further detail in conjunction with the embodiments.But the invention is not restricted to given example.
The step that the present embodiment prepares fluorescent carbon quantum dot is as follows:
The first step, collect plant leaf, and cleaned, dry;
Described plant leaf is the Leaf of Camphortree of ovalize, or be the Rhizoma Dioscoreae esculentae leaf in heart or leaf of leading a cow, or be the Chinese parasol leaf in palm shape, or for being fan-shaped ginkgo leaf, or for being lance-shaped peach leaves, Folium Pterocaryae or the leaf of bamboo, or be rounded lotus leaf or lotus leaf, or in the pine needle of aciculiform, or for assuming diamond in shape, squama shape, cochlear or leg-of-mutton blade.
Second step, the first step gained blade is placed in quartz boat, and (quartz boat diameter is 2cm, be highly 1cm, length is 8cm), then quartz boat is placed in tube furnace silica tube, carry out calcination process pass into nitrogen in tube furnace after, after cooling, obtain black solid;
Described tube furnace calcination temperature is 100 ° of C-500 ° of C, and heating rate is 5 ° of C/min, and the treatment time is 1-5h.
3rd step, be ground into powder by second step gained black solid, dispersion in a solvent, is carried out supersound process, is obtained finely dispersed suspension liquid after magnetic agitation at least 10min;
Described solvent is one of water, ethanol, tetracol phenixin, trichloromethane, methylene dichloride, tetrahydrofuran (THF), normal hexane, acetone, toluene, N, N'-DMAA, sherwood oil; In gained suspension liquid, the massfraction of black solid is 0.1-5g/L.
Described supersound process adopts 100w power ultrasonic cleaning apparatus, and ultrasonic frequency is 40kHz, and ultrasonic time is 10-180min.
4th step, by centrifugal for gained suspension liquid or carry out separating treatment with filter membrane, removing precipitation, obtains clear liquid;
The centrifugal speed of described centrifugal treating is 8000-14000rpm, and centrifugation time is 5-15min;
Described filter membrane process employing aperture is the filter membrane of 0.1-2 μm.
Solvent in 5th step, removing the 4th step gained clear liquid, gained solid is fluorescent carbon quantum dot;
Adopt drying mode except desolventizing, bake out temperature is 50 ° of C.
Embody rule case is as shown in the table.
The each case of table 1 relates to parameter
The parameter of fluorescent carbon quantum dot obtained by each case of table 2
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (6)
1. a fluorescent carbon quantum dot preparation method, is characterized in that comprising the following steps:
The first step, collect plant leaf, and cleaned, dry;
Second step, the first step gained blade is placed in quartz boat, then quartz boat is placed in tube furnace silica tube, carries out calcination process pass into nitrogen in tube furnace after, after cooling, obtain black solid; Described tube furnace calcination temperature is 100 DEG C-500 DEG C, and heating rate is 5 DEG C/min, and the treatment time is 1-5h;
3rd step, be ground into powder by second step gained black solid, dispersion in a solvent, is carried out supersound process, is obtained finely dispersed suspension liquid after magnetic agitation at least 10min; In gained suspension liquid, the massfraction of black solid is 0.1-5g/L;
4th step, by centrifugal for the 3rd step gained suspension liquid or carry out separating treatment with filter membrane, removing precipitation, obtains clear liquid; The centrifugal speed of described centrifugal treating is 8000-14000rpm, and centrifugation time is 5-15min;
Solvent in 5th step, removing the 4th step gained clear liquid, gained solid is fluorescent carbon quantum dot.
2. fluorescent carbon quantum dot preparation method according to claim 1, it is characterized in that, in the first step, described plant leaf is the Leaf of Camphortree of ovalize, or is the Rhizoma Dioscoreae esculentae leaf in heart or leaf of leading a cow, or be the Chinese parasol leaf in palm shape, or for being fan-shaped ginkgo leaf, or be in lance-shaped peach leaves, Folium Pterocaryae or the leaf of bamboo, or be rounded lotus leaf or lotus leaf, or in the pine needle of aciculiform, or for assuming diamond in shape, squama shape, cochlear or leg-of-mutton blade.
3. fluorescent carbon quantum dot preparation method according to claim 1, it is characterized in that, in 3rd step, described solvent is one of water, ethanol, tetracol phenixin, trichloromethane, methylene dichloride, tetrahydrofuran (THF), normal hexane, acetone, toluene, N, N ＇-DMAA, sherwood oil.
4. fluorescent carbon quantum dot preparation method according to claim 3, is characterized in that, in the 3rd step, described supersound process adopts 100w power ultrasonic cleaning apparatus, and ultrasonic frequency is 40kHz, and ultrasonic time is 10-180min.
5. fluorescent carbon quantum dot preparation method according to claim 1, is characterized in that, in the 4th step, described filter membrane process employing aperture is the filter membrane of 0.1-2 μm.
6. fluorescent carbon quantum dot preparation method according to claim 1, is characterized in that, in the 5th step, adopt drying mode except desolventizing, bake out temperature is 50 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310219900.0A CN103274388B (en) | 2013-06-03 | 2013-06-03 | Fluorescent carbon quantum dot preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310219900.0A CN103274388B (en) | 2013-06-03 | 2013-06-03 | Fluorescent carbon quantum dot preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103274388A CN103274388A (en) | 2013-09-04 |
| CN103274388B true CN103274388B (en) | 2015-08-05 |
Family
ID=49057051
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310219900.0A Active CN103274388B (en) | 2013-06-03 | 2013-06-03 | Fluorescent carbon quantum dot preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103274388B (en) |
Families Citing this family (29)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355301A (en) * | 2014-09-26 | 2015-02-18 | 安徽工程大学 | Preparation method for water-soluble carbon dots |
| CN104261386A (en) * | 2014-10-15 | 2015-01-07 | 中国人民解放军防化学院 | Method for preparing carbon dots with hydrothermal process on basis of plant leaves |
| KR20170093826A (en) * | 2014-11-06 | 2017-08-16 | 윌리엄 마쉬 라이스 유니버시티 | Methods of making graphene quantum dots from various carbon sources |
| CN104789217B (en) * | 2015-04-28 | 2017-01-18 | 安徽大学 | Amphipathy carbon quantum dot and preparation method thereof |
| CN105060269A (en) * | 2015-07-23 | 2015-11-18 | 华南理工大学 | Soybean-based carbon quantum dot and porous carbon material as well as preparation method therefor and application thereof |
| CN105060273A (en) * | 2015-08-09 | 2015-11-18 | 安徽大学 | Super hydrophilic carbon quantum dot for promoting catalytic polymerization, preparation method therefor and application thereof |
| CN105462587A (en) * | 2015-12-14 | 2016-04-06 | 上海交通大学 | Method for preparing blue molybdenum disulfide quantum dot solutions |
| CN105689700A (en) * | 2016-01-29 | 2016-06-22 | 云南师范大学 | Method for preparing germanium quantum dots |
| CN105819409B (en) * | 2016-04-01 | 2017-12-22 | 云南师范大学 | A kind of preparation method of selenium quantum dot |
| CN106395789B (en) * | 2016-09-27 | 2019-02-12 | 安徽师范大学 | A kind of synthetic method of carbon dots |
| CN106564877B (en) * | 2016-11-22 | 2018-09-28 | 秦皇岛中科瀚祺科技有限公司 | A kind of carbon quantum dot and preparation method thereof |
| CN106753354A (en) * | 2016-12-05 | 2017-05-31 | 广西师范学院 | The preparation method of the Water-soluble carbon quantum dot with sisal hemp as raw material |
| CN106629663B (en) * | 2016-12-26 | 2019-05-21 | 齐齐哈尔大学 | The preparation method of carbon nano dot based on mangosteen and its application that ferric ion is detected as fluorescence probe |
| CN107651685B (en) * | 2017-10-27 | 2019-12-31 | 江苏大学 | Method for preparing porous biomass charcoal through chemical activation |
| CN107651665A (en) * | 2017-10-27 | 2018-02-02 | 西安理工大学 | A kind of method that water-solubility fluorescent carbon quantum dot is prepared with dried peppermint leaf |
| CN107857248A (en) * | 2017-11-01 | 2018-03-30 | 长春中医药大学 | Preparation method, carbon-based nano particle and its application of carbon-based nano particle |
| CN110337482B (en) | 2018-01-02 | 2023-06-02 | 北京师范大学 | Triangular carbon quantum dot and composition and application thereof |
| CN108084998A (en) * | 2018-01-29 | 2018-05-29 | 兴义民族师范学院 | It is a kind of using white orchid blade as fluorescent carbon quantum dot of carbon source and preparation method thereof |
| CN108872171A (en) * | 2018-06-19 | 2018-11-23 | 江苏大学 | A kind of application of fluorescent carbon point and preparation method thereof and detection tetracycline |
| 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 |
| CN109399610A (en) * | 2018-12-13 | 2019-03-01 | 宁波诺丁汉新材料研究院有限公司 | A kind of preparation method of biomass carbon quantum dot |
| CN109880620A (en) * | 2019-03-02 | 2019-06-14 | 福建医科大学 | It is a kind of using biomass as the preparation and application of the green fluorescence carbon quantum dot of presoma |
| CN110157423B (en) * | 2019-06-27 | 2022-03-22 | 蚌埠学院 | Method for preparing carbon quantum dots based on straws and application |
| CN110371949B (en) * | 2019-08-09 | 2022-12-06 | 华南师范大学 | Green and rapid carbon quantum dot synthesis method, carbon quantum dot and application thereof |
| CN111122524B (en) * | 2019-12-11 | 2021-05-14 | 山西大学 | Fluorescent probe for rapidly detecting morin based on fluorescence quenching method and preparation method and application thereof |
| CN112126427B (en) * | 2020-03-30 | 2023-03-14 | 桂林电子科技大学 | Water-soluble fluorescent carbon dot, preparation method thereof and application of water-soluble fluorescent carbon dot in detection of multiple heavy metals |
| CN111944585B (en) * | 2020-08-28 | 2022-10-18 | 攀枝花学院 | Lipophilic carbon quantum dot base nano lubricating oil additive and its preparation method |
| CN111977645A (en) * | 2020-08-31 | 2020-11-24 | 合肥福纳科技有限公司 | Carbon quantum dot and preparation method thereof |
| CN112979353A (en) * | 2021-01-12 | 2021-06-18 | 华南农业大学 | Preparation method and application of low-cost environment-friendly carbon quantum dot nano fertilizer |
-
2013
- 2013-06-03 CN CN201310219900.0A patent/CN103274388B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| Facile synthesis of fluorescent carbon dots using watermelon peel as a carbon source;Jiaojiao Zhou et al;《Materials Letters》;20110827;第66卷;222-224 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103274388A (en) | 2013-09-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103274388B (en) | Fluorescent carbon quantum dot preparation method | |
| CN102583307B (en) | Fluorescent carbon quantum dots extracted from eggs and preparation method and application thereof | |
| CN102745669B (en) | Method for preparing photoluminescence carbon quantum dot | |
| CN104449693B (en) | The preparation method of the fluorescent carbon quantum dot of nitrogen sulfur doping | |
| CN101973541B (en) | Method for extracting carbon quantum dots from activated carbon | |
| CN102180459B (en) | Method for preparing carbon quantum dots | |
| CN109385273B (en) | Ultra-long-life room temperature phosphorescent material, and preparation method and application thereof | |
| Chen et al. | Multi-bandgap-sensitized ZnO nanorod photoelectrode arrays for water splitting: an X-ray absorption spectroscopy approach for the electronic evolution under solar illumination | |
| CN104071769B (en) | Chemical oxidization method prepares the method for fluorescent carbon point and fluorescent carbon point thereof and application | |
| CN104030269B (en) | The preparation method of red carbon quantum dot and application | |
| CN109135738B (en) | Waste tobacco stem-based nitrogen-doped carbon dots and synthesis method and application thereof | |
| CN103911151B (en) | Nitrogen co-doped carbon point of the sulphur phosphorus that a kind of fluorescence property is adjustable and preparation method thereof | |
| CN110669515B (en) | Two-photon near-infrared carbon dot with high brightness and ultra-narrow half-peak width and preparation method thereof | |
| Jamaludin et al. | Natural biomass as carbon sources for the synthesis of photoluminescent carbon dots | |
| CN104355301A (en) | Preparation method for water-soluble carbon dots | |
| CN105271172A (en) | Preparation method of super-high-quantum-yield carbon quantum dots with citric acid-urea as raw materials | |
| Liu et al. | Strong infrared laser ablation produces white-light-emitting materials via the formation of silicon and carbon dots in silica nanoparticles | |
| CN107841307A (en) | A kind of large-scale preparation method of fluorescent carbon quantum dot | |
| CN109110747A (en) | It is a kind of using extract oil residue as raw material prepare fluorescent carbon point method and its manufactured fluorescent carbon point | |
| CN106892421A (en) | A kind of red carbon quantum dot preparation method of full green | |
| CN105600780B (en) | The cofiring preparation method of chlorine doped graphene quantum dot | |
| CN105694879A (en) | Method for preparing carbon dots from organic wastewater and realizing coagulation recovery of carbon dots | |
| CN105670617A (en) | Simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots | |
| Mansouri et al. | Lily (Iris Persica) pigments as new sensitizer and TiO2 nanofibers as photoanode electrode in dye sensitized solar cells | |
| CN111807348A (en) | Carbon quantum dot and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |