CN103274388A - Preparation method of fluorescence carbon quantum dots - Google Patents
Preparation method of fluorescence carbon quantum dots Download PDFInfo
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- CN103274388A CN103274388A CN2013102199000A CN201310219900A CN103274388A CN 103274388 A CN103274388 A CN 103274388A CN 2013102199000 A CN2013102199000 A CN 2013102199000A CN 201310219900 A CN201310219900 A CN 201310219900A CN 103274388 A CN103274388 A CN 103274388A
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Abstract
The invention relates to a preparation method of fluorescence carbon quantum dots. The preparation method comprises the following steps: a first step, collecting plant leaves, washing the leaves and drying the leaves in the air; a second step, burning the clean leaves to obtain a black solid; a third step, grinding the black solid into a powder, and dispersing the powder in a solvent to obtain a well dispersed suspension through magnetic stirring and ultrasonic treatment; a fourth step, centrifuging the suspension or carrying on a separating process using a filter membrane, removing precipitation to obtain a clear solution; and a fifth step, removing the solvent in the clear solution, then obtaining the solid of the fluorescence carbon quantum dots. According to the invention, a variety of the plant leaves can be employed as raw materials, sources of the raw materials are wide and preparation processes of the method are simple and easy.
Description
Technical field
The present invention relates to a kind of fluorescence carbon quantum dot preparation method, especially a kind of is the fluorescence carbon quantum dot preparation method in source with the plant leaf.
Background technology
Fluorescent nano particles is with a wide range of applications in fields such as biological medicine and photoelectric devices with its excellent optics and electric property.Investigators find typical fluorescent nano particles recently, as CdTe, CdSe, semiconductor-quantum-point materials such as PbS, owing to contain heavy metal element, not only organism is produced toxic side effect, and can produce severe contamination to environment, limited the application of such quantum dot in biological and environmental protection field greatly.
The carbon quantum dot is a kind of new carbon of finding in 2004, with respect to traditional semiconductor-quantum-point and organic dye, newcomer in this carbon family has not only kept 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 big, good light stability, no optical flare, be easy to functionalization, inexpensive, easy extensive incomparable advantage such as synthetic.Report that at present the method for preparing the 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., the raw material of employing mainly contains Graphene, carbon nanotube, gac, candle ash and micromolecular compound etc.But, these method more complicated and consuming time, the raw material that adopts is relatively more expensive mostly, and product need could guarantee the optical property that the carbon quantum dot is stable through means such as strong acid reflow treatment or finishinges, has limited scale operation and the practical application of fluorescence carbon quantum dot.Therefore, seek raw material cheap and easy to get, Nantural non-toxic, it is particularly necessary that the fluorescence carbon quantum dot that utilizes easy and effective to prepare excellent in optical properties fast seems.
In recent years, adopt natural matter to prepare fluorescence carbon quantum dot and caused people's attention.For example, application number be the Chinese invention patent application of 201110049051.X publication No. CN102180459A to disclose a kind of be the fluorescence carbon quantum dot preparation method of raw material with the plant haulm, mainly may further comprise the steps: the heat starting material in 350 ℃-450 ℃ in tubular oven obtain soot; Returned acid boiled 10-12 hour in salpeter solution; Obtain solid product except anhydrating; With polyoxyethylene glycol and mixed 105 ℃-135 ℃ reactions 48-72 hour that be incorporated in of deionized water; Obtain the carbon quantum dot after centrifugal.Though the starting material among this preparation method are cheap and easy to get, processing step is loaded down with trivial details, and to the equipment requirements height, 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 fluorescence carbon quantum dot preparation method of raw material, mainly may further comprise the steps: the raw material drying dehydration is obtained the bean dregs powder; In 200 ℃ of heating 20-40min carbonization; Grinding sieve meal; Be scattered in the deionized water and evaporation concentration; Concentrated solution in-50 ℃ of lyophilizes, is namely got fluorescence carbon quantum dot.Though the technology of this method is simple relatively, need carry out pre-treatment to starting material, and the lyophilize step has improved production cost.In addition, the granularity uniformity of the carbon quantum dot that makes in the embodiment is poor, and particle size range is wideer, about 3-12 μ m.
Summary of the invention
Technical problem to be solved by this invention is: overcome the problem that prior art exists, a kind of fluorescence carbon quantum dot preparation method is provided, its starting material can adopt various plant leafs, wide material sources; Preparation is simple.
The invention provides a kind of fluorescence carbon quantum dot preparation method, it is characterized in that may further comprise the steps:
The first step, collect plant leaf, and it is cleaned, dries;
Second step, the first step gained blade is placed quartz boat, then quartz boat is placed the tube furnace silica tube, feed in the tube furnace and carry out calcination behind the nitrogen and handle, obtain black solid after the cooling;
The 3rd goes on foot, the second step gained black solid is ground into powder, and is dispersed in the solvent, carries out supersound process behind the 10min at least through magnetic agitation, obtains finely dispersed suspension liquid;
The 4th step, the 3rd step gained suspension liquid is centrifugal or carry out separating treatment with filter membrane, remove precipitation, obtain clear liquid;
The 5th goes on foot, removes the solvent in the 4th step gained clear liquid, and the gained solid is fluorescence carbon quantum dot.
The present invention further perfect technical scheme is as follows:
Preferably, in the first step, described plant leaf is the Leaf of Camphortree of ovalize, perhaps for being heart-shaped Rhizoma Dioscoreae esculentae leaf or the leaf of leading a cow, perhaps for being the Chinese parasol leaf of slapping shape, perhaps for being fan-shaped ginkgo leaf, perhaps for being lance-shaped peach leaves, Folium Pterocaryae or the leaf of bamboo, perhaps be rounded lotus leaf or lotus leaf, perhaps for being the pine needle of aciculiform, perhaps for assume 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 water, ethanol, tetracol phenixin, trichloromethane, methylene dichloride, tetrahydrofuran (THF), normal hexane, acetone, toluene, N, one of N'-DMAA, sherwood oil; The massfraction of black solid is 0.1-5g/L in the gained suspension liquid.
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 is handled and adopted the aperture is the filter membrane of 0.1-2 μ m.
Preferably, in the 5th step, adopt the drying mode desolventizing, bake out temperature is 50 ° of C.
Beneficial effect of the present invention is as follows:
1, fluorescence carbon quantum dot preparation method required equipment provided by the invention is simple, easy to operate, and raw material sources are extensive, Nantural non-toxic, cheap and easy to get.
2, it is adjustable with calcination temperature that the present invention makes the emissive porwer of fluorescence carbon quantum dot, have higher luminous efficiency and stable glimmering energy, and glow color is adjustable with excitation wavelength, and particle diameter is less than 5 nanometers, and granulometric facies are to homogeneous.
3, the present invention makes fluorescence carbon quantum dot and can be used as the nanometer ink for the spray ink Printing field, also can be used for biologic applications such as LED lighting field and biomarker, living imaging.
Description of drawings
Fig. 1 makes ultra-violet absorption spectrum and the fluorescence reflection spectrum of fluorescence carbon quantum dot for case 1 of the present invention.
Fig. 2 makes the fluorescence reflectivity curve of fluorescence carbon quantum dot with the spectrogram (excitation wavelength is by 360nm to 500nm, and step-length is 20nm) of excitation wavelength variation for case 1 of the present invention.
Fig. 3 makes the transmission electron microscope picture of fluorescence carbon quantum dot for case 1 of the present invention.
Fig. 4 makes the infrared spectrogram of fluorescence carbon quantum dot for case 1 of the present invention.
Embodiment
With reference to the accompanying drawings and in conjunction with the embodiments the present invention is described in further detail.But the invention is not restricted to given example.
The step that present embodiment prepares fluorescence carbon quantum dot is as follows:
The first step, collect plant leaf, and it is cleaned, dries;
Described plant leaf is the Leaf of Camphortree of ovalize, perhaps for being heart-shaped Rhizoma Dioscoreae esculentae leaf or the leaf of leading a cow, perhaps for being the Chinese parasol leaf of slapping shape, perhaps for being fan-shaped ginkgo leaf, perhaps for being lance-shaped peach leaves, Folium Pterocaryae or the leaf of bamboo, perhaps be rounded lotus leaf or lotus leaf, perhaps for being the pine needle of aciculiform, perhaps for assume diamond in shape, squama shape, cochlear or leg-of-mutton blade.
Second step, the first step gained blade is placed quartz boat (the quartz boat diameter is 2cm, highly be 1cm, and length is 8cm), then quartz boat is placed the tube furnace silica tube, carry out the calcination processing in the tube furnace behind the feeding nitrogen, obtain black solid after the cooling;
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.
The 3rd goes on foot, the second step gained black solid is ground into powder, and is dispersed in the solvent, carries out supersound process behind the 10min at least through magnetic agitation, obtains finely dispersed suspension liquid;
Described solvent is water, ethanol, tetracol phenixin, trichloromethane, methylene dichloride, tetrahydrofuran (THF), normal hexane, acetone, toluene, N, one of N'-DMAA, sherwood oil; The massfraction of black solid is 0.1-5g/L in the gained suspension liquid.
Described supersound process adopts 100w power ultrasonic cleaning apparatus, and ultrasonic frequency is 40kHz, and ultrasonic time is 10-180min.
The 4th step, the gained suspension liquid is centrifugal or carry out separating treatment with filter membrane, remove precipitation, obtain clear liquid;
The centrifugal speed of described centrifugal treating is 8000-14000rpm, and centrifugation time is 5-15min;
Described filter membrane is handled and adopted the aperture is the filter membrane of 0.1-2 μ m.
The 5th goes on foot, removes the solvent in the 4th step gained clear liquid, and the gained solid is fluorescence carbon quantum dot;
Adopt the drying mode desolventizing, bake out temperature is 50 ° of C.
Concrete application case is as shown in the table.
Each case of table 1 relates to parameter
The parameter of the obtained fluorescence carbon of each case of table 2 quantum dot
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 requirement of the present invention.
Claims (7)
1. fluorescence carbon quantum dot preparation method is characterized in that may further comprise the steps:
The first step, collect plant leaf, and it is cleaned, dries;
Second step, the first step gained blade is placed quartz boat, then quartz boat is placed the tube furnace silica tube, feed in the tube furnace and carry out calcination behind the nitrogen and handle, obtain black solid after the cooling;
The 3rd goes on foot, the second step gained black solid is ground into powder, and is dispersed in the solvent, carries out supersound process behind the 10min at least through magnetic agitation, obtains finely dispersed suspension liquid;
The 4th step, the 3rd step gained suspension liquid is centrifugal or carry out separating treatment with filter membrane, remove precipitation, obtain clear liquid;
The 5th goes on foot, removes the solvent in the 4th step gained clear liquid, and the gained solid is fluorescence carbon quantum dot.
2. fluorescence 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, perhaps for being heart-shaped Rhizoma Dioscoreae esculentae leaf or the leaf of leading a cow, perhaps for being the Chinese parasol leaf of slapping shape, for to be fan-shaped ginkgo leaf, perhaps for being lance-shaped peach leaves, Folium Pterocaryae or the leaf of bamboo, perhaps be rounded lotus leaf or lotus leaf perhaps, perhaps for being the pine needle of aciculiform, perhaps for assume diamond in shape, squama shape, cochlear or leg-of-mutton blade.
3. fluorescence carbon quantum dot preparation method according to claim 1 and 2 is characterized in that, 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.
4. fluorescence carbon quantum dot preparation method according to claim 1, it is characterized in that, in the 3rd step, described solvent is water, ethanol, tetracol phenixin, trichloromethane, methylene dichloride, tetrahydrofuran (THF), normal hexane, acetone, toluene, N, one of N'-DMAA, sherwood oil; The massfraction of black solid is 0.1-5g/L in the gained suspension liquid.
5. fluorescence carbon quantum dot preparation method according to claim 4 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.
6. fluorescence carbon quantum dot preparation method according to claim 1 is characterized in that, in the 4th step, the centrifugal speed of described centrifugal treating is 8000-14000rpm, and centrifugation time is 5-15min; Described filter membrane is handled and adopted the aperture is the filter membrane of 0.1-2 μ m.
7. fluorescence carbon quantum dot preparation method according to claim 1 is characterized in that, in the 5th step, adopts the drying mode desolventizing, and bake out temperature is 50 ° of C.
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