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
- Publication number
- CN103663412A CN103663412A CN201310652713.1A CN201310652713A CN103663412A CN 103663412 A CN103663412 A CN 103663412A CN 201310652713 A CN201310652713 A CN 201310652713A CN 103663412 A CN103663412 A CN 103663412A
- Authority
- CN
- China
- Prior art keywords
- citrate
- citric acid
- solution
- carbon quantum
- quantum dots
- 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.)
- Pending
Links
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000003086 colorant Substances 0.000 title 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 185
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 64
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 230000005284 excitation Effects 0.000 claims abstract description 27
- 239000007864 aqueous solution Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005121 nitriding Methods 0.000 claims abstract 11
- 239000007800 oxidant agent Substances 0.000 claims abstract 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract 4
- 239000000243 solution Substances 0.000 claims description 84
- 238000000502 dialysis Methods 0.000 claims description 41
- 239000011259 mixed solution Substances 0.000 claims description 36
- 239000012043 crude product Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 21
- 239000001509 sodium citrate Substances 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 13
- -1 nitrogen-containing compound Chemical class 0.000 claims description 13
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- 239000001508 potassium citrate Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 7
- 238000000197 pyrolysis Methods 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims 2
- 239000001099 ammonium carbonate Substances 0.000 claims 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 235000012501 ammonium carbonate Nutrition 0.000 claims 1
- 235000013877 carbamide Nutrition 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 229960002635 potassium citrate Drugs 0.000 claims 1
- 235000011082 potassium citrates Nutrition 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 24
- 229910052799 carbon Inorganic materials 0.000 abstract description 24
- 239000000463 material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 210000004881 tumor cell Anatomy 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000002372 labelling Methods 0.000 abstract 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 2
- 238000010859 live-cell imaging Methods 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 235000015165 citric acid Nutrition 0.000 description 42
- 229910001220 stainless steel Inorganic materials 0.000 description 18
- 239000010935 stainless steel Substances 0.000 description 18
- 210000004027 cell Anatomy 0.000 description 17
- 239000003643 water by type Substances 0.000 description 14
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 13
- 235000019263 trisodium citrate Nutrition 0.000 description 13
- 229940038773 trisodium citrate Drugs 0.000 description 12
- 235000015870 tripotassium citrate Nutrition 0.000 description 11
- 150000003839 salts Chemical class 0.000 description 10
- 238000000695 excitation spectrum Methods 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 238000002189 fluorescence spectrum Methods 0.000 description 5
- 239000002096 quantum dot Substances 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000005424 photoluminescence Methods 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 238000006862 quantum yield reaction Methods 0.000 description 3
- 239000000090 biomarker Substances 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002953 phosphate buffered saline Substances 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Images
Landscapes
- Luminescent Compositions (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明涉及一种荧光光色可调碳量子点的制备方法，属于纳米材料技术领域。本方法以柠檬酸或柠檬酸盐为碳源，以含氮化合物为氮化剂，过氧化氢为氧化剂，通过水热合成法得到在紫外光激发下发蓝色或绿色荧光的碳量子点水溶液，反应条件容易控制，适宜规模化生产；制备得到的碳量子点具有荧光光色可调、产率高、量子效率高、结果重复性好等诸多优点。产物可以直接用于肿瘤细胞标记及活细胞成像标记。本发明方法仅需一种反应物即可，并且原料易得、无毒，生产过程无需特殊防护，反应条件容易控制，所得到的碳量子点具有产率高、量子效率高、结果重复性好等优点。本发明方法具有产率高、制备工艺简单、成本低、易于规模化生产等特点。
The invention relates to a preparation method of carbon quantum dots with adjustable fluorescent light and color, belonging to the technical field of nanometer materials. The method uses citric acid or citrate as a carbon source, nitrogen-containing compounds as a nitriding agent, and hydrogen peroxide as an oxidizing agent to obtain an aqueous solution of carbon quantum dots that emits blue or green fluorescence under ultraviolet light excitation through a hydrothermal synthesis method. , the reaction conditions are easy to control, and are suitable for large-scale production; the prepared carbon quantum dots have many advantages such as adjustable fluorescent light color, high yield, high quantum efficiency, and good repeatability of results. The product can be directly used for tumor cell labeling and live cell imaging labeling. The method of the invention only needs one reactant, and the raw material is easy to obtain and non-toxic, the production process does not need special protection, the reaction conditions are easy to control, and the obtained carbon quantum dots have high yield, high quantum efficiency, and good repeatability of results Etc. The method of the invention has the characteristics of high yield, simple preparation process, low cost, easy large-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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310652713.1A CN103663412A (en) | 2013-12-05 | 2013-12-05 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310652713.1A CN103663412A (en) | 2013-12-05 | 2013-12-05 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103663412A true CN103663412A (en) | 2014-03-26 |
Family
ID=50302322
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310652713.1A Pending CN103663412A (en) | 2013-12-05 | 2013-12-05 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103663412A (en) |
Cited By (39)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017576A (en) * | 2014-06-20 | 2014-09-03 | 上海交通大学 | Method for synthesizing nitrogen-doped carbon quantum dots based on calcium citrate and urea microwave reaction |
| CN104017577A (en) * | 2014-06-20 | 2014-09-03 | 上海交通大学 | Method for directly synthesizing nitrogen doped carbon quantum dot on basis of direct heating of diacetone and ammonia |
| CN104403664A (en) * | 2014-11-07 | 2015-03-11 | 山西大学 | Preparation method of green fluorescent carbon spot and application of green fluorescent carbon spot in cell imaging |
| CN104655604A (en) * | 2015-02-13 | 2015-05-27 | 安徽理工大学 | Fluorescence sensor for detecting fluorine ions, and preparation method of fluorescence sensor |
| CN104694120A (en) * | 2014-09-24 | 2015-06-10 | 北京大学 | Preparation method of fluorescent nitrogen-enriched quantum dots as well as products and application of quantum dots |
| CN104752591A (en) * | 2015-04-13 | 2015-07-01 | 吉林大学 | Color panel display film with function of concentration regulation of carbon quantum dots and manufacturing method of color panel display film |
| CN104830328A (en) * | 2015-05-12 | 2015-08-12 | 太原理工大学 | Preparation method of single-matrix carbon quantum dot white light fluorescent powder |
| CN105236383A (en) * | 2015-09-14 | 2016-01-13 | 复旦大学 | Wavelength adjustable carbon quantum dots, preparation method and applications thereof |
| CN105542762A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Preparation method of nitrogen-doped fluorescence carbon dots |
| CN105647527A (en) * | 2016-01-22 | 2016-06-08 | 南京工业大学 | Preparation method of yellow fluorescent carbon quantum dots |
| CN105670617A (en) * | 2016-01-14 | 2016-06-15 | 中国石油大学(华东) | Simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots |
| CN105860972A (en) * | 2016-05-11 | 2016-08-17 | 四川省人民医院 | Preparation method of P-doped carbon dots and application of P-doped carbon dots to cell imaging |
| CN106092984A (en) * | 2016-06-07 | 2016-11-09 | 广东省汕头市质量计量监督检测所 | A kind of fluorescence analysis method based on passivation carbon quantum dot and application thereof |
| CN106433632A (en) * | 2016-10-08 | 2017-02-22 | 哈尔滨师范大学 | Preparation method and application of carbon quantum dot |
| CN106525806A (en) * | 2017-01-13 | 2017-03-22 | 中国农业大学 | Method for detecting ethrel by using fluorescent nitrogen doped carbon quantum dot |
| CN107118768A (en) * | 2017-06-11 | 2017-09-01 | 哈尔滨师范大学 | A kind of fluorescent carbon quantum dot and application |
| CN107189777A (en) * | 2017-07-26 | 2017-09-22 | 广西师范学院 | The preparation method of water-soluble nitrogen doping carbon quantum dot |
| CN107681042A (en) * | 2017-09-29 | 2018-02-09 | 广州正农照明科技有限公司 | A kind of quantum dot LED light source for plant growth |
| CN108164458A (en) * | 2018-02-08 | 2018-06-15 | 浙江师范大学 | A kind of synthetic method of citrazinic acid |
| CN108394885A (en) * | 2018-03-26 | 2018-08-14 | 大连理工大学 | A kind of method of Gaseous Detonation composite solid state carbon quantum dot |
| CN108483422A (en) * | 2018-04-03 | 2018-09-04 | 武汉轻工大学 | The carbon quantum dot and preparation method thereof of excited by visible light fluorescence |
| CN108728086A (en) * | 2018-06-01 | 2018-11-02 | 陕西科技大学 | A kind of method of simple synthesis green fluorescence carbon quantum dot |
| CN108732152A (en) * | 2018-06-01 | 2018-11-02 | 陕西科技大学 | A method of formaldehyde is detected as fluorescence probe based on amino functional carbon quantum dot |
| CN109336087A (en) * | 2018-12-26 | 2019-02-15 | 南京林业大学 | Preparation of Quercus Quercus shell-based carbon quantum dots using Quercus Quercus and its application in fluorescent inks |
| CN109502569A (en) * | 2018-12-27 | 2019-03-22 | 南京林业大学 | A kind of method and application of microwave synthesis green fluorescence biomass carbon dots |
| CN109607512A (en) * | 2019-01-31 | 2019-04-12 | 吉林大学 | A carbon quantum dot prepared by pyrolysis of molecular sieve and its application in hydrogen peroxide detection |
| CN110044861A (en) * | 2019-05-09 | 2019-07-23 | 南宁师范大学 | The detection method of concentration of hydrogen peroxide |
| TWI674100B (en) * | 2018-05-02 | 2019-10-11 | 國立中山大學 | Method for manufacturing clathrate-like carbon dot |
| CN110342490A (en) * | 2019-07-02 | 2019-10-18 | 武汉纺织大学 | A preparation process of seven-color fluorescent carbon quantum dots |
| CN110846031A (en) * | 2019-11-27 | 2020-02-28 | 重庆医科大学 | A kind of self-assembled composite nanoparticle and preparation method thereof |
| CN111073638A (en) * | 2019-12-19 | 2020-04-28 | 东华大学 | Method for preparing controllable photoluminescence carbon dots by changing temperature |
| CN111139064A (en) * | 2019-12-20 | 2020-05-12 | 自然资源部天津海水淡化与综合利用研究所 | Carbon nano-fluorescent material suitable for seawater medium, preparation method and application thereof |
| CN111377430A (en) * | 2020-03-09 | 2020-07-07 | 广东省微生物研究所（广东省微生物分析检测中心） | A kind of nitrogen-doped carbon nanomaterial and preparation method thereof |
| CN111620314A (en) * | 2019-05-24 | 2020-09-04 | 中国医学科学院基础医学研究所 | Preparation method and application of phenylboronic acid modified carbon nitride quantum dots |
| CN111807323A (en) * | 2019-04-11 | 2020-10-23 | 中国石化工程建设有限公司 | Method for preparing hydrogen by steam conversion |
| CN112645293A (en) * | 2020-12-21 | 2021-04-13 | 重庆邮电大学 | Preparation method of narrow-band-gap carbon nitride material, product and application thereof |
| CN113604217A (en) * | 2021-07-21 | 2021-11-05 | 中钞印制技术研究院有限公司 | Quantum dot luminescent material, preparation method thereof, anti-counterfeiting element and security document |
| CN115432693A (en) * | 2022-10-09 | 2022-12-06 | 中国石油大学(北京) | Nitrogen-doped carbon quantum dot corrosion inhibitor, preparation method thereof and application thereof in carbon steel metal pickling solution |
| CN116376362A (en) * | 2023-06-06 | 2023-07-04 | 江苏唐彩新材料科技股份有限公司 | Water-based ink and preparation method thereof |
-
2013
- 2013-12-05 CN CN201310652713.1A patent/CN103663412A/en active Pending
Cited By (54)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017577A (en) * | 2014-06-20 | 2014-09-03 | 上海交通大学 | Method for directly synthesizing nitrogen doped carbon quantum dot on basis of direct heating of diacetone and ammonia |
| CN104017576B (en) * | 2014-06-20 | 2016-01-13 | 上海交通大学 | A method for synthesizing nitrogen-doped carbon quantum dots based on the microwave reaction of calcium citrate and urea |
| CN104017577B (en) * | 2014-06-20 | 2016-07-06 | 上海交通大学 | A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia |
| CN104017576A (en) * | 2014-06-20 | 2014-09-03 | 上海交通大学 | Method for synthesizing nitrogen-doped carbon quantum dots based on calcium citrate and urea microwave reaction |
| CN104694120A (en) * | 2014-09-24 | 2015-06-10 | 北京大学 | Preparation method of fluorescent nitrogen-enriched quantum dots as well as products and application of quantum dots |
| CN104403664A (en) * | 2014-11-07 | 2015-03-11 | 山西大学 | Preparation method of green fluorescent carbon spot and application of green fluorescent carbon spot in cell imaging |
| CN104655604B (en) * | 2015-02-13 | 2017-11-03 | 安徽理工大学 | It is a kind of to be used to detect fluorescent optical sensor of fluorine ion and preparation method thereof |
| CN104655604A (en) * | 2015-02-13 | 2015-05-27 | 安徽理工大学 | Fluorescence sensor for detecting fluorine ions, and preparation method of fluorescence sensor |
| CN104752591B (en) * | 2015-04-13 | 2017-05-10 | 吉林大学 | Color panel display film with function of concentration regulation of carbon quantum dots and manufacturing method of color panel display film |
| CN104752591A (en) * | 2015-04-13 | 2015-07-01 | 吉林大学 | Color panel display film with function of concentration regulation of carbon quantum dots and manufacturing method of color panel display film |
| CN104830328A (en) * | 2015-05-12 | 2015-08-12 | 太原理工大学 | Preparation method of single-matrix carbon quantum dot white light fluorescent powder |
| CN105236383A (en) * | 2015-09-14 | 2016-01-13 | 复旦大学 | Wavelength adjustable carbon quantum dots, preparation method and applications thereof |
| CN105542762A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Preparation method of nitrogen-doped fluorescence carbon dots |
| CN105670617A (en) * | 2016-01-14 | 2016-06-15 | 中国石油大学(华东) | Simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots |
| CN105647527A (en) * | 2016-01-22 | 2016-06-08 | 南京工业大学 | Preparation method of yellow fluorescent carbon quantum dots |
| CN105860972A (en) * | 2016-05-11 | 2016-08-17 | 四川省人民医院 | Preparation method of P-doped carbon dots and application of P-doped carbon dots to cell imaging |
| CN105860972B (en) * | 2016-05-11 | 2018-05-04 | 四川省人民医院 | The preparation method of P doping carbon quantum dots and its application in cell imaging |
| CN106092984A (en) * | 2016-06-07 | 2016-11-09 | 广东省汕头市质量计量监督检测所 | A kind of fluorescence analysis method based on passivation carbon quantum dot and application thereof |
| CN106092984B (en) * | 2016-06-07 | 2019-04-26 | 广东省汕头市质量计量监督检测所 | A kind of fluorescence analysis method and its application based on passivation carbon quantum dot |
| CN106433632A (en) * | 2016-10-08 | 2017-02-22 | 哈尔滨师范大学 | Preparation method and application of carbon quantum dot |
| CN106433632B (en) * | 2016-10-08 | 2019-06-25 | 哈尔滨师范大学 | A kind of preparation method and applications of carbon quantum dot |
| CN106525806A (en) * | 2017-01-13 | 2017-03-22 | 中国农业大学 | Method for detecting ethrel by using fluorescent nitrogen doped carbon quantum dot |
| CN106525806B (en) * | 2017-01-13 | 2019-05-21 | 中国农业大学 | A method of utilizing fluorescence nitrogen-doped carbon quantum dots characterization ethephon (CEPHA),2-(chloroethyl) phosphonic acid |
| CN107118768A (en) * | 2017-06-11 | 2017-09-01 | 哈尔滨师范大学 | A kind of fluorescent carbon quantum dot and application |
| CN107189777A (en) * | 2017-07-26 | 2017-09-22 | 广西师范学院 | The preparation method of water-soluble nitrogen doping carbon quantum dot |
| CN107681042A (en) * | 2017-09-29 | 2018-02-09 | 广州正农照明科技有限公司 | A kind of quantum dot LED light source for plant growth |
| CN108164458A (en) * | 2018-02-08 | 2018-06-15 | 浙江师范大学 | A kind of synthetic method of citrazinic acid |
| CN108164458B (en) * | 2018-02-08 | 2021-02-02 | 浙江师范大学 | Synthetic method of citrazinic acid |
| CN108394885A (en) * | 2018-03-26 | 2018-08-14 | 大连理工大学 | A kind of method of Gaseous Detonation composite solid state carbon quantum dot |
| CN108394885B (en) * | 2018-03-26 | 2021-03-26 | 大连理工大学 | A method for gas phase detonation synthesis of solid carbon quantum dots |
| CN108483422A (en) * | 2018-04-03 | 2018-09-04 | 武汉轻工大学 | The carbon quantum dot and preparation method thereof of excited by visible light fluorescence |
| TWI674100B (en) * | 2018-05-02 | 2019-10-11 | 國立中山大學 | Method for manufacturing clathrate-like carbon dot |
| CN108728086A (en) * | 2018-06-01 | 2018-11-02 | 陕西科技大学 | A kind of method of simple synthesis green fluorescence carbon quantum dot |
| CN108732152A (en) * | 2018-06-01 | 2018-11-02 | 陕西科技大学 | A method of formaldehyde is detected as fluorescence probe based on amino functional carbon quantum dot |
| CN109336087A (en) * | 2018-12-26 | 2019-02-15 | 南京林业大学 | Preparation of Quercus Quercus shell-based carbon quantum dots using Quercus Quercus and its application in fluorescent inks |
| CN109502569A (en) * | 2018-12-27 | 2019-03-22 | 南京林业大学 | A kind of method and application of microwave synthesis green fluorescence biomass carbon dots |
| CN109502569B (en) * | 2018-12-27 | 2020-07-31 | 南京林业大学 | Method for synthesizing green fluorescent biomass carbon dots by microwave and application |
| CN109607512A (en) * | 2019-01-31 | 2019-04-12 | 吉林大学 | A carbon quantum dot prepared by pyrolysis of molecular sieve and its application in hydrogen peroxide detection |
| CN111807323A (en) * | 2019-04-11 | 2020-10-23 | 中国石化工程建设有限公司 | Method for preparing hydrogen by steam conversion |
| CN110044861A (en) * | 2019-05-09 | 2019-07-23 | 南宁师范大学 | The detection method of concentration of hydrogen peroxide |
| CN111620314A (en) * | 2019-05-24 | 2020-09-04 | 中国医学科学院基础医学研究所 | Preparation method and application of phenylboronic acid modified carbon nitride quantum dots |
| CN110342490A (en) * | 2019-07-02 | 2019-10-18 | 武汉纺织大学 | A preparation process of seven-color fluorescent carbon quantum dots |
| CN110846031A (en) * | 2019-11-27 | 2020-02-28 | 重庆医科大学 | A kind of self-assembled composite nanoparticle and preparation method thereof |
| CN111073638A (en) * | 2019-12-19 | 2020-04-28 | 东华大学 | Method for preparing controllable photoluminescence carbon dots by changing temperature |
| CN111139064A (en) * | 2019-12-20 | 2020-05-12 | 自然资源部天津海水淡化与综合利用研究所 | Carbon nano-fluorescent material suitable for seawater medium, preparation method and application thereof |
| CN111139064B (en) * | 2019-12-20 | 2023-11-07 | 自然资源部天津海水淡化与综合利用研究所 | Carbon nano fluorescent material suitable for seawater medium and preparation method and application thereof |
| CN111377430A (en) * | 2020-03-09 | 2020-07-07 | 广东省微生物研究所（广东省微生物分析检测中心） | A kind of nitrogen-doped carbon nanomaterial and preparation method thereof |
| CN111377430B (en) * | 2020-03-09 | 2022-11-08 | 广东省微生物研究所（广东省微生物分析检测中心） | Nitrogen-doped carbon nano material and preparation method thereof |
| CN112645293A (en) * | 2020-12-21 | 2021-04-13 | 重庆邮电大学 | Preparation method of narrow-band-gap carbon nitride material, product and application thereof |
| CN112645293B (en) * | 2020-12-21 | 2023-05-12 | 重庆邮电大学 | Preparation method of narrow-band-gap carbon nitride material, and product and application thereof |
| CN113604217A (en) * | 2021-07-21 | 2021-11-05 | 中钞印制技术研究院有限公司 | Quantum dot luminescent material, preparation method thereof, anti-counterfeiting element and security document |
| CN115432693A (en) * | 2022-10-09 | 2022-12-06 | 中国石油大学(北京) | Nitrogen-doped carbon quantum dot corrosion inhibitor, preparation method thereof and application thereof in carbon steel metal pickling solution |
| CN116376362A (en) * | 2023-06-06 | 2023-07-04 | 江苏唐彩新材料科技股份有限公司 | Water-based ink and preparation method thereof |
| CN116376362B (en) * | 2023-06-06 | 2023-08-11 | 江苏唐彩新材料科技股份有限公司 | Water-based ink and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103663412A (en) | Preparation method of carbon quantum dots with adjustable fluorescence colors | |
| Zhang et al. | A review on carbon quantum dots: Synthesis, photoluminescence mechanisms and applications | |
| CN102277157B (en) | Near-infrared silver sulphide quantum dot as well as preparation method and application thereof | |
| CN105542764B (en) | A kind of yellow fluorescence carbon point of high quantum production rate and preparation method thereof | |
| CN108545715A (en) | A kind of preparation method for the red fluorescence carbon dots that transmitting does not change with excitation wavelength | |
| Xiao et al. | Porous carbon quantum dots: one step green synthesis via L-cysteine and applications in metal ion detection | |
| CN103232029B (en) | Preparation method and application of green fluorescent carbon dots | |
| CN105001861B (en) | A kind of composite quantum dot and its preparation method and application | |
| CN104528692A (en) | Synthesis method of nitrogen-doped fluorescent carbon dots | |
| CN104388082B (en) | A kind of orange nitrogen, the green synthesis method of sulfur codope carbon quantum dot | |
| CN105236383A (en) | Wavelength adjustable carbon quantum dots, preparation method and applications thereof | |
| Kayani et al. | Carbon dot as fluorescence sensor for glutathione in human serum samples: a review | |
| CN104987861A (en) | Method for preparing carbon dots with up-down conversion luminescence characteristic from maize straw | |
| CN103254890A (en) | Preparation method of hyperbranched poly-glycidyl ether grated rare earth up-conversion luminescence nanocrystal | |
| CN106590617A (en) | Synthetic method of nitrogen and sulfur co-doped cellulosic fluorescent carbon dots | |
| WO2022095131A1 (en) | Preparation method and application for carbon nanoparticle | |
| CN109438722A (en) | Based on manganese base luminescent metal organic framework material and its preparation method and application | |
| CN107529514B (en) | Preparation method and application of fluoride ion-doped carbon dots | |
| CN102911669B (en) | Preparation method for water-soluble chiral CdTe quantum dots | |
| CN109607512A (en) | A carbon quantum dot prepared by pyrolysis of molecular sieve and its application in hydrogen peroxide detection | |
| CN104610964A (en) | Preparation method of wavelength adjustable fluorescent carbon dot and application of fluorescent carbon dot in mercury ion detection | |
| CN108728090A (en) | A method of additive Mn perovskite quantum dot is quickly prepared based on ultrasound | |
| CN111057541B (en) | A nitrogen-doped orange fluorescent carbon quantum dot and its preparation method and application | |
| CN104555984A (en) | Carbon quantum dot fluorescence labeling material with egg white used as carbon source as well as preparation method and application of carbon quantum dot fluorescence labeling material | |
| CN103616357A (en) | Visual biosensor device and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140326 |