CN103663412A - Preparation method of carbon quantum dots with adjustable fluorescence colors - Google Patents
Preparation method of carbon quantum dots with adjustable fluorescence colors Download PDFInfo
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Abstract
The present invention relates to a preparation method of carbon quantum dots with adjustable fluorescence colors, and belongs to the technical field of nanometer materials. According to method, citric acid or a citrate is adopted as a carbon source, a nitrogen-containing compound is adopted as a nitridation agent, hydrogen peroxide is adopted as an oxidant, a hydrothermal synthesis method is adopted to obtain an aqueous solution of carbon quantum dots emitting blue or green fluorescence under ultraviolet light excitation, reaction conditions are easily controlled, and the method is suitable for scale production. The prepared carbon quantum dots have advantages of adjustable fluorescence color, high yield, high quantum efficiency, good result reproducibility and the like, wherein the product can be directly used for tumor cell labeling and live cell imaging labeling. According to the present invention, only the one reactant is required, the raw materials are easily-available and non-toxic, the production process does not require special protection, the reaction condition is easily controlled, and the obtained carbon quantum dots have advantages of high yield, high quantum efficiency, good result reproducibility and the like; and the method has characteristics of high yield, simple preparation process, low cost, easy scale production and the like.
Description
Technical field
The preparation method who the present invention relates to the photochromic adjustable carbon quantum dot of a kind of fluorescence, belongs to technical field of nano material.
Background technology
CdS quantum dots especially semiconductor-quantum-point due to its excellent photoluminescent property, in a lot of fields, particularly photoelectric device, biomarker and biomedical sector have a wide range of applications.But semiconductor-quantum-point material, owing to often using heavy metal ion in preparation process, as cadmium, lead etc., causes it to have very large bio-toxicity and environmental hazard, has seriously limited its application at biomedical sector.In recent years, carbon quantum dot had shown very large application potential in fields such as optical probe, biometric image probe, photodiode and visible light activity catalysis.Carbon quantum dot has the photoluminescent property of a lot of excellences, as there is compound multicolor fluorescence, utilizing emitted light is adjustable, and there is the advantages such as quantum yield is high, surface chemistry is controlled, low toxicity, good water solubility, become the desirable equivalent material of semiconductor-quantum-point nano material.Particularly, with respect to the high toxicity of the heavy metal element component of semiconductor-quantum-point material, the chief component of carbon quantum dot is atoxic carbon, and therefore, fluorescent carbon quantum dot has huge application prospect at biomedical sector.But because be subject to the impact of the aspects such as preparation method and quality product aspect, the widespread use of carbon quanta point material is greatly limited.Prepare at present the most frequently used method of carbon quantum dot and have the physical methods such as high-energy radiation, laser ablation, and soot oxidation, carbohydrate carbonization, Polymer-pyrolysis, electrochemistry, microwave-assisted pyrolysis and carbon material decomposition etc., but the shortcoming such as these methods often exist that productive rate is low, cost is high or quantum yield is low.In addition, in existing report, carbon quanta point material is main mainly with blue-fluorescence, although blue-fluorescence carbon quanta point material has very important application in fields such as photoelectric device, biomarker and biomedicines, but, because some biological tissue itself also all concentrates on blue wavelength region to the self-absorption of light and autofluorescence, therefore, limited in some cases its application.
Summary of the invention
The object of the invention is to propose the preparation method of the photochromic adjustable carbon quantum dot of a kind of fluorescence; preparation method to existing carbon quantum dot improves, and regulates fluorescence color, to expand the range of application of carbon quantum dot by adding oxygenant; and simplify preparation technology, make its suitability for scale production.
The preparation method of the photochromic adjustable carbon quantum dot of fluorescence that the present invention proposes, can have three kinds of different technical schemes, wherein: the first technical scheme comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, nitridizing agent is joined in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, under room temperature, use magnetic agitation, Citrate trianion and nitridizing agent are fully dissolved, obtain mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains crude product;
(4) crude product of step (3) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues blue-fluorescence.
The second technical scheme comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, using hydrogen peroxide as oxygenant, join in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, oxygenant: citric acid or citrate solution=1:5～25, room temperature lower magnetic force stirs, and makes citric acid or Citrate trianion, nitrogenous compound and hydrogen peroxide fully dissolve and mix, and obtains mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains crude product;
(4) crude product of step (3) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues green fluorescence.
The third technical scheme comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, nitridizing agent is joined in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, under room temperature, use magnetic agitation, citric acid or Citrate trianion and nitridizing agent are fully dissolved, obtain mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains the first crude product;
(4) using hydrogen peroxide as oxygenant, join in the first crude product of step (4), add mol ratio ratio to be: oxygenant: citric acid or Citrate trianion=1:5～25 mix mixed solution under magnetic stirrer;
(5) mixed solution of step (4) is moved in hydrothermal reaction kettle, put into immigration baking oven and carry out hydrothermal oxidization reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains the second crude product;
(6) the second crude product of step (5) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues green fluorescence.
In above-mentioned three schemes, described Citrate trianion is any in Trisodium Citrate, Tripotassium Citrate or ammonium citrate.
In above-mentioned three schemes, described nitrogenous compound is any in bicarbonate of ammonia, volatile salt, ammoniacal liquor or urea.
The preparation method of the photochromic adjustable carbon quantum dot of fluorescence that the present invention proposes, its advantage is, the inventive method raw material is easy to get, nontoxic, in production process without special protection; Synthesis technique is simple, take citric acid or Citrate trianion as carbon source, take nitrogenous compound as nitridizing agent, hydrogen peroxide is oxygenant, by hydrothermal synthesis method, obtain issuing at ultraviolet excitation the carbon quantum dot aqueous solution of blueness or green fluorescence, easy control of reaction conditions, suitability for scale production; The carbon quantum dot preparing has photochromic adjustable, the plurality of advantages such as productive rate is high, quantum yield is high, result is reproducible of fluorescence.And, in the inventive method, by the simple oxygenant that adds, realize the adjusting to fluorescence color, blueness or the green fluorescence carbon quantum dot of preparation, can be applied to cell marking and viable cell imaging, add the substratum that contains blueness or green fluorescence carbon quantum dot to hatch altogether in the cell after cultivating, and observe with fluorescent microscope, and can be directly used in tumour cell mark.
Accompanying drawing explanation
Fig. 1 is embodiment mono-in the embodiment of the present invention, and embodiment six, the blueness of embodiment 11 preparations and the green fluorescence carbon quantum dot photo under daylight and the irradiation of 365 nano-ultraviolet lights.
Fig. 2 is the blue-fluorescence carbon quantum dot of the embodiment of the present invention one preparation fluorescence spectrum and the excitation spectrum under different burst of ultraviolel wavelength.
Fig. 3 is the green fluorescence carbon quantum dot of the embodiment of the present invention six preparation photoluminescence spectrum and the corresponding exciting light spectrogram under different burst of ultraviolel wavelength.
Fig. 4 is fluorescence spectrum and the corresponding excitation spectrum of the green fluorescence carbon quantum dot for preparing of the embodiment of the present invention 11.
Fig. 5 is the blueness prepared of the embodiment of the present invention and the shows fluorescent microscopy images of the quantum dot-labeled tumour cell Hela of green fluorescence carbon cell.
Embodiment
The preparation method of the photochromic adjustable carbon quantum dot of fluorescence that the present invention proposes, can have three kinds of different technical schemes, wherein: the first technical scheme comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, nitridizing agent is joined in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, under room temperature, use magnetic agitation, Citrate trianion and nitridizing agent are fully dissolved, obtain mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains crude product;
(4) crude product of step (3) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues blue-fluorescence.
The second technical scheme comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, using hydrogen peroxide as oxygenant, join in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, oxygenant: citric acid or citrate solution=1:5～25, room temperature lower magnetic force stirs, and makes citric acid or Citrate trianion, nitrogenous compound and hydrogen peroxide fully dissolve and mix, and obtains mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains crude product;
(4) crude product of step (3) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues green fluorescence.
The third technical scheme comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, nitridizing agent is joined in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, under room temperature, use magnetic agitation, citric acid or Citrate trianion and nitridizing agent are fully dissolved, obtain mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains the first crude product;
(4) using hydrogen peroxide as oxygenant, join in the first crude product of step (4), add mol ratio ratio to be: oxygenant: citric acid or Citrate trianion=1:5～25 mix mixed solution under magnetic stirrer;
(5) mixed solution of step (4) is moved in hydrothermal reaction kettle, put into immigration baking oven and carry out hydrothermal oxidization reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains the second crude product;
(6) the second crude product of step (5) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues green fluorescence.
In above-mentioned three schemes, described Citrate trianion is any in Trisodium Citrate, Tripotassium Citrate or ammonium citrate.
In above-mentioned three schemes, described nitrogenous compound is any in bicarbonate of ammonia, volatile salt, ammoniacal liquor or urea.
In the inventive method, the hydrothermal reaction kettle of use is with polytetrafluoroethyllining lining.
Below introduce the embodiment of the inventive method:
Embodiment mono-, prepare the carbon quantum dot that ultraviolet excitation issues blue-fluorescence:
(1) take 0.4 gram of Tripotassium Citrate is carbon source, joins in 20 ml waters and dissolves, and forms the Tripotassium Citrate aqueous solution;
(2) take 2.8 grams of volatile salts, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Tripotassium Citrate and volatile salt fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 180 degrees Celsius, react 3 hours, obtain the brown solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 500 through molecular weight cut-off is dialysed, and obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues blue-fluorescence.
The photoluminescent property of the carbon quantum dot of this embodiment mono-preparation characterizes: with the ultraviolet lamp of wavelength 365 nanometers, carbon quantum dot aqueous sample is irradiated, can be observed obvious blue light, as shown in Figure 1, wherein A is sample photo under white light, B is that hand-held ultraviolet lamp 365 nano-ultraviolet lights irradiate lower fluorescent photo, with spectrophotofluorometer, obtain the photoluminescence spectrogram of carbon quantum dot and excite accordingly spectrogram, further proved is invented prepared carbon quantum dot and send blue-fluorescence under burst of ultraviolel, as shown in Figure 2, fluorescence spectrum (solid line, 360 nanometers excite, peak position is set to 447 nanometers) and corresponding excitation spectrum (dotted line, 447 nanometer transmittings, excitation spectrum peak position is set to 360 nanometers).
Embodiment bis-, prepare the carbon quantum dot that ultraviolet excitation issues blue-fluorescence:
(1) take 0.04 gram of Tripotassium Citrate is carbon source, adds in 20 ml waters and dissolves;
(2) take 0.3 gram of volatile salt, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Tripotassium Citrate and volatile salt fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 170 degrees Celsius, react 12 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 4000 through molecular weight cut-off is dialysed and obtain launching the carbon quantum dot aqueous solution of blue light under the ultraviolet lamp of 365 nanometers.
Embodiment tri-, prepare the carbon quantum dot that ultraviolet excitation issues blue-fluorescence:
(1) take 0.4 gram of Trisodium Citrate is carbon source, adds in 20 ml waters and dissolves;
(2) take 1 gram of urea, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Trisodium Citrate and urea fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 150 degrees Celsius, react 24 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 3000 through molecular weight cut-off is dialysed and obtain launching the carbon quantum dot aqueous solution of blue light under the ultraviolet lamp of 365 nanometers.
Embodiment tetra-, prepare the carbon quantum dot that ultraviolet excitation issues blue-fluorescence:
(1) take 0.04 gram of ammonium citrate is carbon source, adds in 20 ml waters and dissolves;
(2) take the ammoniacal liquor of 3 milliliter 30%, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes ammonium citrate and ammoniacal liquor fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 200 degrees Celsius, react 2 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 500 through molecular weight cut-off is dialysed and obtain launching the carbon quantum dot aqueous solution of blue light under the ultraviolet lamp of 365 nanometers.
Embodiment five, prepare the carbon quantum dot that ultraviolet excitation issues blue-fluorescence:
(1) take 0.04 gram of citric acid is carbon source, adds in 20 ml waters and dissolves;
(2) take 0.3 gram of volatile salt, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Trisodium Citrate and volatile salt fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 120 degrees Celsius, react 24 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 3500 through molecular weight cut-off is dialysed and obtain launching the carbon quantum dot aqueous solution of blue light under the ultraviolet lamp of 365 nanometers.
Embodiment six, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 0.4 gram of Trisodium Citrate is carbon source, adds in 20 ml waters and dissolves;
(2) take 3.2 grams of bicarbonate of ammonia, and 3 milliliters containing 30% aqueous hydrogen peroxide solution, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Trisodium Citrate, and bicarbonate of ammonia and hydrogen peroxide fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 170 degrees Celsius, react 12 hours, obtain the yellow solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 3000 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution.
The photoluminescent property of the carbon quantum dot of the green-emitting fluorescence of these embodiment six preparations characterizes: with the ultraviolet lamp of wavelength 365 nanometers, carbon quantum dot aqueous sample is irradiated, can be observed obvious green glow, as Fig. 1, wherein C is sample photo under white light, and D is that hand-held ultraviolet lamp 365 nano-ultraviolet lights irradiate lower fluorescent photo; With spectrophotofluorometer, obtain the photoluminescence spectrogram of carbon quantum dot and excite accordingly spectrogram, further proved is invented prepared carbon quantum dot and send green fluorescence under burst of ultraviolel, as shown in Figure 3, fluorescence spectrum (solid line, 372 nanometers excite, peak position is set to 560 nanometers) and corresponding excitation spectrum (excitation spectrum peak position is set to 372 nanometers for dotted line, 560 nanometer transmittings)).
Embodiment seven, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 0.4 gram of Tripotassium Citrate is carbon source, adds in 20 ml waters and dissolves;
(2) take 3 grams of urea, and 5 milliliters containing 30% aqueous hydrogen peroxide solution, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Tripotassium Citrate, and urea and hydrogen peroxide fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 180 degrees Celsius, react 4 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 10000 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution of transmitting green light under the ultraviolet lamp of 365 nanometers.
Embodiment eight, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 0.4 gram of ammonium citrate is carbon source, adds in 20 ml waters and dissolves;
(2) pipette the ammoniacal liquor of 3 milliliter 50%, and 10 milliliters containing 30% aqueous hydrogen peroxide solution, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes ammonium citrate, and ammoniacal liquor and hydrogen peroxide fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 170 degrees Celsius, react 12 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 8000 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution of transmitting green light under the ultraviolet lamp of 365 nanometers.
Embodiment nine, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 2 grams of Trisodium Citrates is carbon source, adds in 20 ml waters and dissolves;
(2) take 3 grams of volatile salts, and 10 milliliters containing 30% aqueous hydrogen peroxide solution, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Trisodium Citrate, and volatile salt and hydrogen peroxide fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into 200 degrees Celsius, baking oven 2 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 8000 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution of transmitting green light under the ultraviolet lamp of 365 nanometers.
Embodiment ten, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 0.4 gram of citric acid is carbon source, adds in 20 ml waters and dissolves;
(2) take 3 grams of urea, and 10 milliliters containing 30% aqueous hydrogen peroxide solution, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Trisodium Citrate, and urea and hydrogen peroxide fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put under 160 degrees Celsius, baking oven, react 24 hours, obtain the solution that contains carbon quantum dot.
(4) dialysis tubing that solution step 3 being obtained is 100 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution of transmitting green light under the ultraviolet lamp of 365 nanometers.
Embodiment 11, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 0.4 gram of Trisodium Citrate is carbon source, adds in 20 ml waters and dissolves;
(2) take 2.8 grams of bicarbonate of ammonia, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Trisodium Citrate and bicarbonate of ammonia fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 180 degrees Celsius, react 3 hours, obtain brown solution.
(4) pipette 3 milliliters of aqueous hydrogen peroxide solutions containing 30% and join obtaining in solution of step 3, room temperature condition lower magnetic force stirs and makes to mix.
(5) the resulting mixed solution of step 4 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 180 degrees Celsius, react 3 hours, obtain pale yellow solution.
(6) dialysis tubing that solution step 5 being obtained is 500 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution.
The ultraviolet excitation of the present embodiment 11 preparations issues the carbon quantum dot light photoluminescence property representation of green fluorescence: with the ultraviolet lamp of wavelength 365 nanometers, carbon quantum dot aqueous sample is irradiated, can be observed obvious green glow, as shown in Figure 1, wherein E is sample photo under white light, and F is that hand-held ultraviolet lamp 365 nano-ultraviolet lights irradiate lower fluorescent photo; With spectrophotofluorometer, obtain the photoluminescence spectrogram of carbon quantum dot and excite accordingly spectrogram, further proved is invented prepared carbon quantum dot and send green fluorescence under burst of ultraviolel, as shown in Figure 4, fluorescence spectrum (solid line, 413 nanometers excite, peak position is set to 563 nanometers) and corresponding excitation spectrum (excitation spectrum peak position is set to 413 nanometers for dotted line, 563 nanometer transmittings).
Embodiment 12, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 2 grams of Tripotassium Citrates is carbon source, adds in 20 ml waters and dissolves;
(2) take 3 grams of urea, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Tripotassium Citrate and urea fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into 180 degrees Celsius, baking oven 5 hours, obtain brown solution.
(4) pipette 5 milliliters of aqueous hydrogen peroxide solutions containing 30% and join obtaining in solution of step 3, room temperature condition lower magnetic force stirs and makes to mix.
(5) the resulting mixed solution of step 4 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 180 degrees Celsius, react 3 hours, obtain pale yellow solution.
(6) dialysis tubing that solution step 5 being obtained is 500 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution of transmitting green light under the ultraviolet lamp of 365 nanometers.
Embodiment 13, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 2 grams of ammonium citrates is carbon source, adds in 20 ml waters and dissolves;
(2) pipette the ammoniacal liquor of 3 milliliter 50%, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes ammonium citrate and ammoniacal liquor fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 150 degrees Celsius, react 24 hours, obtain brown solution.
(4) pipette 5 milliliters of aqueous hydrogen peroxide solutions containing 30% and join obtaining in solution of step 3, room temperature condition lower magnetic force stirs and makes to mix.
(5) the resulting mixed solution of step 4 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 190 degrees Celsius, react 2 hours, obtain pale yellow solution.
(6) dialysis tubing that solution step 5 being obtained is 5000 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution of transmitting green light under the ultraviolet lamp of 365 nanometers.
Embodiment 14, prepare the carbon quantum dot that ultraviolet excitation issues green fluorescence:
(1) take 2 grams of citric acids is carbon source, adds in 20 ml waters and dissolves;
(2) take 3 grams of urea, join in the solution of step 1, room temperature condition lower magnetic force stirs and makes Trisodium Citrate and urea fully dissolve and mix;
(3) the resulting mixed solution of step 2 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 160 degrees Celsius, react 10 hours, obtain brown solution.
(4) pipette 10 milliliters of aqueous hydrogen peroxide solutions containing 30% and join obtaining in solution of step 3, room temperature condition lower magnetic force stirs and makes to mix.
(5) the resulting mixed solution of step 4 is transferred in 50 milliliters of polytetrafluoroethyllining lining tanks, packs in stainless steel hydrothermal reaction kettle, put into baking oven, under 180 degrees Celsius, react 4 hours, obtain pale yellow solution.
(6) dialysis tubing that solution step 5 being obtained is 1000 through molecular weight cut-off is dialysed and is obtained the carbon quantum dot aqueous solution of transmitting green light under the ultraviolet lamp of 365 nanometers.
Application example: the viable cell imaging applications of blueness or green fluorescence carbon quantum dot:
(1) s is inoculated in culture dish of the quartzy end, in 37 degrees Celsius, 5% CO2gas incubator, cultivates;
(2) after cell attachment, suck original fluid, join respectively and contain in example one, six of the present invention, 11 bluenesss of preparation or three substratum of green fluorescence carbon quantum dot, at 37 degrees Celsius, gas concentration lwevel is in 5% incubator, to hatch altogether 24 hours;
(3) take out culture dish, by phosphate buffered saline buffer buffer solution for cleaning, fall nutrient solution, use the phosphate buffered saline buffer damping fluid fixed cell of paraformaldehyde;
(4) under inverted fluorescence microscope, observe carbon quantum dot to Hela cell marking situation, as shown in Figure 5, wherein A, B are the shows fluorescent microscopy images of the quantum dot-labeled Hela cell of blue-fluorescence carbon that obtains of embodiment mono-, A is cell pattern under halogen light, and B is cell fluorescence figure under mercury lamp UV-irradiation; C, D are the shows fluorescent microscopy images of the quantum dot-labeled Hela cell of blue-fluorescence carbon that obtains of example six, and C is cell pattern under halogen light, and D is cell fluorescence figure under mercury lamp blue light illumination; E, F are the shows fluorescent microscopy images of the quantum dot-labeled Hela cell of blue-fluorescence carbon that obtains of example 11, and E is cell pattern under halogen light, and F is cell fluorescence figure under mercury lamp blue light illumination.
Claims (5)
1. a preparation method for the photochromic adjustable carbon quantum dot of fluorescence, is characterized in that the method comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, nitridizing agent is joined in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, under room temperature, use magnetic agitation, Citrate trianion and nitridizing agent are fully dissolved, obtain mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains crude product;
(4) crude product of step (3) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues blue-fluorescence.
2. a preparation method for the photochromic adjustable carbon quantum dot of fluorescence, is characterized in that the method comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, using hydrogen peroxide as oxygenant, join in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, oxygenant: citric acid or citrate solution=1:5～25, room temperature lower magnetic force stirs, and makes citric acid or Citrate trianion, nitrogenous compound and hydrogen peroxide fully dissolve and mix, and obtains mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains crude product;
(4) crude product of step (3) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues green fluorescence.
3. a preparation method for the photochromic adjustable carbon quantum dot of fluorescence, is characterized in that the method comprises the following steps:
(1) citric acid or Citrate trianion are added to the water, making the mass percent concentration of citric acid or Citrate trianion is 0.2%～30%, obtains citric acid or citrate solution;
(2) using nitrogenous compound as nitridizing agent, nitridizing agent is joined in the citric acid or citrate solution of step (1), the mol ratio adding is: nitridizing agent: citric acid or citrate solution=1:2～50, under room temperature, use magnetic agitation, citric acid or Citrate trianion and nitridizing agent are fully dissolved, obtain mixed solution;
(3) mixed solution of step (2) is put into hydrothermal reaction kettle, move in baking oven and carry out pyrolytic reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains the first crude product;
(4) using hydrogen peroxide as oxygenant, join in the first crude product of step (4), add mol ratio ratio to be: oxygenant: citric acid or Citrate trianion=1:5～25 mix mixed solution under magnetic stirrer;
(5) mixed solution of step (4) is moved in hydrothermal reaction kettle, put into immigration baking oven and carry out hydrothermal oxidization reaction, temperature of reaction is 120 ℃～200 ℃, and the reaction times is 2～24 hours, obtains the second crude product;
(6) the second crude product of step (5) is dialysed with dialysis tubing, the molecular weight that dams of dialysis tubing is 100-10000, and dialysis time is 6～72 hours, obtains the carbon quantum dot aqueous solution that ultraviolet excitation issues green fluorescence.
4. the preparation method of the photochromic adjustable carbon quantum dot of fluorescence as described in claim 1,2 or 3, is characterized in that wherein said Citrate trianion is any in Trisodium Citrate, Tripotassium Citrate or ammonium citrate.
5. the preparation method of the photochromic adjustable carbon quantum dot of fluorescence as described in claim 1,2 or 3, is characterized in that wherein said nitrogenous compound is any in bicarbonate of ammonia, volatile salt, ammoniacal liquor or urea.
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