CN107189777A - The preparation method of water-soluble nitrogen doping carbon quantum dot - Google Patents
The preparation method of water-soluble nitrogen doping carbon quantum dot Download PDFInfo
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- CN107189777A CN107189777A CN201710619687.0A CN201710619687A CN107189777A CN 107189777 A CN107189777 A CN 107189777A CN 201710619687 A CN201710619687 A CN 201710619687A CN 107189777 A CN107189777 A CN 107189777A
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Abstract
A kind of preparation method for carbon quantum dot of being adulterated the invention discloses water-soluble nitrogen, comprises the following steps：Precursor solution I is made Step 1: citric acid is dissolved in ultra-pure water, Para Amino Benzamide is dissolved in ultra-pure water precursor solution II is made, by volume 1~10:1 uniform mixing precursor solution I and precursor solution II, obtain mixed solution；Step 2: mixed solution made from step one is carried out into hydro-thermal reaction, you can obtain water-soluble nitrogen doping carbon quantum dot.The present invention uses one step hydro thermal method to prepare water-soluble nitrogen doping carbon quantum dot, and carbon source is abundant, cheap, and preparation process is simple, and preparation overall process is pollution-free, nontoxic, environmental protection, can largely prepare.
Description
Technical field
The present invention relates to the preparation field of nano material.It is more particularly related to a kind of water-soluble nitrogen doped carbon
The preparation method of quantum dot.
Background technology
In recent years, fluorescence carbon nanomaterial there is good optical characteristics and cell hypotoxicity to cause research work because of it
Persons' is widely studied.It has preferable photostability, and the presence of nontoxic secondary ion, it is adaptable to detects and shows for a long time
The experiment of track, has broad application prospects in terms of biomarker and analysis detection.Carbon quantum dot (CQDs) shows
The excellent properties such as hydrophily, low cytotoxicity, chemistry and photostability, make it be learned and photoelectron in chemistry, biomedical, sensing
Field has obtained extensive concern and application.
The preparation method of carbon quantum dot mainly has two kinds at present：Method and from bottom to top method from top to bottom.It is top-down to close
Into method, i.e., the physical method of carbon nano-particle, then the side being passivated by polymer surfaces are prepared from larger carbon structure peeling
Formula makes it effectively light, mainly including arc discharge, laser ablation, electrochemical oxidation, e-book radiation etc..This method is often needed
Strict experiment condition and the special energy are wanted, cost is high, and the carbon quantum productivity ratio obtained is relatively low.Synthesis from bottom to top
Method, i.e., directly synthesize fluorescent carbon quantum dot, method includes by the suitable predecessor that is pyrolyzed or is carbonized：Combustion method, hydrothermal solution carbon
Change method, ultrasonic method etc., but this kind of method used be all often non-renewable energy resources and need strict post-processing, so
Also it is unfavorable for continuing and large-scale production fluorescent carbon quantum dot.Therefore, cheap and easy to get, Nantural non-toxic raw material is found, using simple
The effective quick processability of method is excellent and carbon quantum dot of high quantum production rate seems is even more important.
The content of the invention
It is an object of the present invention to provide a kind of raw material is cheap and easy to get, preparation method is simple effectively, carbon quantum dot performance
The preparation method of the high water-soluble nitrogen doping carbon quantum dot of good yield.
In order to realize that there is provided a kind of water-soluble nitrogen doping carbon quantum dot according to object of the present invention and further advantage
Preparation method, comprise the following steps：
Precursor solution I is made Step 1: citric acid is dissolved in ultra-pure water, Para Amino Benzamide is dissolved in ultra-pure water
Precursor solution II, by volume 1~10 is made:1 uniform mixing precursor solution I and precursor solution II, obtain mixed solution；
Step 2: mixed solution made from step one is carried out into hydro-thermal reaction, you can obtain water-soluble nitrogen doping carbon quantum
Point.
Preferably, 1.0g citric acids are dissolved in 20mL ultra-pure waters in step one and precursor solution I is made.
Preferably, 0.1g Para Amino Benzamides are dissolved in 20mL ultra-pure waters in step one and precursor solution II is made.
Preferably, mixed solution also filtered successively after hydro-thermal reaction, dialyses, evaporates in step 2.
Preferably, hydro-thermal reaction is carried out in isoperibol in step 2, and temperature is 160 DEG C, and the reaction time is 4h.
Preferably, precursor solution I and precursor solution II by volume 5 in step one:1 is mixed.
Preferably, dialysis, using the bag filter of shearing molecular weight 1000, is dialysed 72 hours in step 2.
Preferably, evaporation uses constant temperature rotary evaporation in step 2, and temperature is 60 DEG C.
Preferably, also carried out between step one and step 2：
Step a, mixed solution made from step one is carried out to ultrasonic disperse, ultrasonic frequency is 28~33KHz, and the time is
20~35min, then will be ultrasonically treated after mixed solution carry out infrared heating processing, programming rate be 2 DEG C/min, final temperature is 54
~58 DEG C, bipolar electrode system is put into heating process in mixed solution, anode is graphite electrode, and negative electrode is platinum electrode, simultaneously
It is powered, size of current presses 0.01A/min speed increase, at the end of temperature-rise period, electric current also stops increase, maintains temperature
Degree and current condition 30min, then rise to 78~84 DEG C, size of current is pressed with 3 DEG C/min programming rate by temperature
0.02A/min speed increase, after assigned temperature is reached, maintains temperature and current condition 50min, finally with 4 DEG C/min's
Cooling rate and 0.04A/min electric current reduce speed and cool the temperature to room temperature, and electric current also is down into 0A, in addition, for the first time
In insulating process, ammonia is passed through into mixed solution with 100ml/min speed, with 80ml/min in second of insulating process
Speed ammonia is passed through into mixed solution.
The present invention at least includes following beneficial effect：
1st, the present invention prepares water-soluble nitrogen doping carbon quantum dot using one step hydro thermal method, and carbon source is abundant, cheap, prepares
Journey is simple, and preparation overall process is pollution-free, nontoxic, environmental protection, can largely prepare.
2nd, the water-soluble nitrogen doping carbon quantum dot that the present invention is prepared has that good water solubility, excitation-emission be adjustable, fluorescence is steady
The fixed, advantage of good biocompatibility, in biomarker, bio-sensing, bio-imaging, fluorescence probe, anti-fake mark and immune
Chromatography product scope has important application value.
3rd, the water-soluble nitrogen doped carbon quantum dot size that the present invention is prepared is controllable, and exciting light spectrum is wider, to different ripples
Long exciting light can be detected without adjustment, and detection rising limit is low, and detection is accurate sensitive.
4th, the water-soluble nitrogen doped carbon quantum dot quantum yield that prepared by the present invention is higher.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings
Fig. 1 is the fluorescence excitation and fluorescent emission collection of illustrative plates of water-soluble nitrogen doping carbon quantum dot prepared by embodiment 5；
Fig. 2 is fluorescent emission collection of illustrative plates of the water-soluble nitrogen doping carbon quantum dot of the preparation of embodiment 5 under different excitation wavelengths；
Fig. 3 is the fluorescence quantum yield figure of water-soluble nitrogen doping carbon quantum dot prepared by embodiment 5.
Embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
It should be noted that experimental method described in following embodiments, is conventional method unless otherwise specified, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
<Embodiment 1>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, comprises the following steps：
Precursor solution I is made Step 1: 1.0g citric acids are dissolved in 20mL ultra-pure waters, by 0.1g Para Amino Benzamides
It is dissolved in 20mL ultra-pure waters and precursor solution II is made, by volume 1:1 uniform mixing precursor solution I and precursor solution II, obtain mixed
Close solution；
Step 2: mixed solution made from step one is stirred, the polytetrafluoroethylene (PTFE) of hydrothermal synthesis reaction kettle is put into
In inner bag, then hydrothermal synthesis reaction kettle be placed in insulating box heated, obtain yellow solution, calorstat temperature is 160 DEG C,
Reaction time is 4h；
Step 3: yellow solution made from filtration step two obtains filtrate, then filtrate is dialysed, using shearing point
The bag filter of son amount 1000, dialysis obtains dialyzate in 72 hours, dialyzate finally is carried out into constant temperature rotary evaporation, temperature is 60
DEG C, obtain water-soluble nitrogen doping carbon quantum dot.
<Embodiment 2>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, comprises the following steps：
Precursor solution I is made Step 1: 1.0g citric acids are dissolved in 20mL ultra-pure waters, by 0.1g Para Amino Benzamides
It is dissolved in 20mL ultra-pure waters and precursor solution II is made, by volume 2:1 uniform mixing precursor solution I and precursor solution II, obtain mixed
Close solution；
Step 2: mixed solution made from step one is stirred, the polytetrafluoroethylene (PTFE) of hydrothermal synthesis reaction kettle is put into
In inner bag, then hydrothermal synthesis reaction kettle be placed in insulating box heated, obtain yellow solution, calorstat temperature is 160 DEG C,
Reaction time is 4h；
Step 3: yellow solution made from filtration step two obtains filtrate, then filtrate is dialysed, using shearing point
The bag filter of son amount 1000, dialysis obtains dialyzate in 72 hours, dialyzate finally is carried out into constant temperature rotary evaporation, temperature is 60
DEG C, obtain water-soluble nitrogen doping carbon quantum dot.
<Embodiment 3>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, comprises the following steps：
Precursor solution I is made Step 1: 1.0g citric acids are dissolved in 20mL ultra-pure waters, by 0.1g Para Amino Benzamides
It is dissolved in 20mL ultra-pure waters and precursor solution II is made, by volume 4:1 uniform mixing precursor solution I and precursor solution II, obtain mixed
Close solution；
Step 2: mixed solution made from step one is stirred, the polytetrafluoroethylene (PTFE) of hydrothermal synthesis reaction kettle is put into
In inner bag, then hydrothermal synthesis reaction kettle be placed in insulating box heated, obtain yellow solution, calorstat temperature is 160 DEG C,
Reaction time is 4h；
Step 3: yellow solution made from filtration step two obtains filtrate, then filtrate is dialysed, using shearing point
The bag filter of son amount 1000, dialysis obtains dialyzate in 72 hours, dialyzate finally is carried out into constant temperature rotary evaporation, temperature is 60
DEG C, obtain water-soluble nitrogen doping carbon quantum dot.
<Embodiment 4>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, comprises the following steps：
Precursor solution I is made Step 1: 1.0g citric acids are dissolved in 20mL ultra-pure waters, by 0.1g Para Amino Benzamides
It is dissolved in 20mL ultra-pure waters and precursor solution II is made, by volume 6:1 uniform mixing precursor solution I and precursor solution II, obtain mixed
Close solution；
Step 2: mixed solution made from step one is stirred, the polytetrafluoroethylene (PTFE) of hydrothermal synthesis reaction kettle is put into
In inner bag, then hydrothermal synthesis reaction kettle be placed in insulating box heated, obtain yellow solution, calorstat temperature is 160 DEG C,
Reaction time is 4h；
Step 3: yellow solution made from filtration step two obtains filtrate, then filtrate is dialysed, using shearing point
The bag filter of son amount 1000, dialysis obtains dialyzate in 72 hours, dialyzate finally is carried out into constant temperature rotary evaporation, temperature is 60
DEG C, obtain water-soluble nitrogen doping carbon quantum dot.
<Embodiment 5>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, comprises the following steps：
Precursor solution I is made Step 1: 1.0g citric acids are dissolved in 20mL ultra-pure waters, by 0.1g Para Amino Benzamides
It is dissolved in 20mL ultra-pure waters and precursor solution II is made, by volume 8:1 uniform mixing precursor solution I and precursor solution II, obtain mixed
Close solution；
Step 2: mixed solution made from step one is stirred, the polytetrafluoroethylene (PTFE) of hydrothermal synthesis reaction kettle is put into
In inner bag, then hydrothermal synthesis reaction kettle be placed in insulating box heated, obtain yellow solution, calorstat temperature is 160 DEG C,
Reaction time is 4h；
Step 3: yellow solution made from filtration step two obtains filtrate, then filtrate is dialysed, using shearing point
The bag filter of son amount 1000, dialysis obtains dialyzate in 72 hours, dialyzate finally is carried out into constant temperature rotary evaporation, temperature is 60
DEG C, obtain water-soluble nitrogen doping carbon quantum dot.
<Embodiment 6>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, comprises the following steps：
Precursor solution I is made Step 1: 1.0g citric acids are dissolved in 20mL ultra-pure waters, by 0.1g Para Amino Benzamides
It is dissolved in 20mL ultra-pure waters and precursor solution II is made, by volume 10:1 uniform mixing precursor solution I and precursor solution II, obtain mixed
Close solution；
Step 2: mixed solution made from step one is stirred, the polytetrafluoroethylene (PTFE) of hydrothermal synthesis reaction kettle is put into
In inner bag, then hydrothermal synthesis reaction kettle be placed in insulating box heated, obtain yellow solution, calorstat temperature is 160 DEG C,
Reaction time is 4h；
Step 3: yellow solution made from filtration step two obtains filtrate, then filtrate is dialysed, using shearing point
The bag filter of son amount 1000, dialysis obtains dialyzate in 72 hours, dialyzate finally is carried out into constant temperature rotary evaporation, temperature is 60
DEG C, obtain water-soluble nitrogen doping carbon quantum dot.
<Embodiment 7>
The water-soluble nitrogen doping carbon quantum dot that the present invention is prepared can carry out immunochromatographiassays assays with antibody binding.It is anti-
The fluorescent carbon quantum dot that body is combined is more, and corresponding fluorescence intensity is stronger, can be quantified using the power of its fluorescence signal
Analysis.
The water-soluble nitrogen doping carbon quantum dot prepared now to embodiment 5 carries out following immunochromatographiassays assays experiment：
(1) under buffer solution system, two cyclohexyl diimines (DCC) or DIC (DIC) place are passed through
Reason can be crosslinked with streptavidin, then with the antibody binding of biotin labeling, obtained and combined water-soluble nitrogen doping carbon quantum
The antibody of point.
(2) immuno-chromatographic test paper strip includes sample application zone, conjugate release area, reaction zone and the suction zones set gradually；Institute
State the conjugate release pad that conjugate release area is combined with the antibody of water-soluble nitrogen doping carbon quantum dot for coating；The reaction zone
To be divided into test section and control zone, the reaction zone is antigen, control zone coating anti-mouse IgG of the test section coating with antibody binding
The solid support of antibody.
(3) antibody for combining water-soluble nitrogen doping carbon quantum dot is sprayed in conjugate release pad and obtains conjugate release
Area；
Antigen and dynamics are sprayed on the solid support of reaction zone, test section, control zone is formed respectively and obtains
Obtain reaction zone；
Being pasted onto on backing of mutually overlapping successively of sample application zone, conjugate release area, reaction zone and suction zones is produced.
Wherein, the antigen sprayed in immune chromatography reagent kit of the present invention on immuno-chromatographic test paper strip is directed to different detections
Thing can select the antigen being adapted with detectable substance.
<Embodiment 8>
Water-soluble nitrogen doping carbon quantum dot prepared by embodiment 5 is added in pure water, and it is 2mg/mL water-soluble to prepare concentration
Nitrogen-doped carbon quantum dot aqueous solution 2mL, it is mixed with 5mL polyvinyl alcohol (5.0wt%), and mixed solution is equal with brush
It is even to be applied on sheet glass, sheet glass is placed in 65 DEG C of baking ovens 1 hour afterwards, sheet glass is taken out and takes pictures, understood by contrast,
Sheet glass does not have any color under natural light, and the visible bright blue-fluorescence under 365nm uviol lamps, therefore carbon quantum dot can
As anti-fake mark.
<Embodiment 9>
Fluorescence standard material is done using quinine sulfate, at the same to embodiment 5 prepare water-soluble nitrogen adulterate carbon quantum dot and
Quinine sulfate carries out fluorescent absorbance determining, and its result such as Fig. 3 is straight according to water-soluble nitrogen-doped carbon quantum dot structure in Fig. 3
Slope and quinine sulfate select the straight slope of structure ratio be multiplied by quinine sulfate quantum yield (quinine sulfate is standard volume,
Its quantum yield is 88% for the fluorescence quantum yield that 54%) can calculate the carbon quantum dot of the present invention.
<Embodiment 10>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, specific implementation process is same as Example 5, difference
It is between step one and step 2 also to carry out：
Step a, mixed solution made from step one is subjected to ultrasonic disperse, ultrasonic frequency is 28KHz, and the time is
20min, then will be ultrasonically treated after mixed solution carry out infrared heating processing, programming rate be 2 DEG C/min, final temperature be 54 DEG C,
Bipolar electrode system is put into heating process in mixed solution, anode is graphite electrode, and negative electrode is platinum electrode, while being led to
Electricity, size of current presses 0.01A/min speed increase, at the end of temperature-rise period, and electric current also stops increase, maintains temperature and electricity
Stream condition 30min, then rises to 78 DEG C, size of current presses 0.02A/min speed with 3 DEG C/min programming rate by temperature
It is incremented by, after assigned temperature is reached, temperature and current condition 50min is maintained, finally with 4 DEG C/min cooling rate and 0.04A/
Min electric current reduces speed and cools the temperature to room temperature, and electric current also is down into 0A, in addition, in first time insulating process, with
100ml/min speed is passed through ammonia into mixed solution, with 80ml/min speed to mixing in second of insulating process
Ammonia is passed through in solution.
It is 90% to determine its yield to the use of this embodiment and the identical detection method of embodiment 9, compared to embodiment 5
88% yield increases.
<Embodiment 11>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, specific implementation process is same as Example 5, difference
It is between step one and step 2 also to carry out：
Step a, mixed solution made from step one is subjected to ultrasonic disperse, ultrasonic frequency is 33KHz, and the time is
35min, then will be ultrasonically treated after mixed solution carry out infrared heating processing, programming rate be 2 DEG C/min, final temperature be 58 DEG C,
Bipolar electrode system is put into heating process in mixed solution, anode is graphite electrode, and negative electrode is platinum electrode, while being led to
Electricity, size of current presses 0.01A/min speed increase, at the end of temperature-rise period, and electric current also stops increase, maintains temperature and electricity
Stream condition 30min, then rises to 84 DEG C, size of current presses 0.02A/min speed with 3 DEG C/min programming rate by temperature
It is incremented by, after assigned temperature is reached, temperature and current condition 50min is maintained, finally with 4 DEG C/min cooling rate and 0.04A/
Min electric current reduces speed and cools the temperature to room temperature, and electric current also is down into 0A, in addition, in first time insulating process, with
100ml/min speed is passed through ammonia into mixed solution, with 80ml/min speed to mixing in second of insulating process
Ammonia is passed through in solution.
It is 91% to determine its yield to the use of this embodiment and the identical detection method of embodiment 9, compared to embodiment 5
88% yield increases.
<Embodiment 12>
A kind of preparation method of water-soluble nitrogen doping carbon quantum dot, specific implementation process is same as Example 5, difference
It is between step one and step 2 also to carry out：
Step a, mixed solution made from step one is subjected to ultrasonic disperse, ultrasonic frequency is 30KHz, and the time is
28min, then will be ultrasonically treated after mixed solution carry out infrared heating processing, programming rate be 2 DEG C/min, final temperature be 56 DEG C,
Bipolar electrode system is put into heating process in mixed solution, anode is graphite electrode, and negative electrode is platinum electrode, while being led to
Electricity, size of current presses 0.01A/min speed increase, at the end of temperature-rise period, and electric current also stops increase, maintains temperature and electricity
Stream condition 30min, then rises to 81 DEG C, size of current presses 0.02A/min speed with 3 DEG C/min programming rate by temperature
It is incremented by, after assigned temperature is reached, temperature and current condition 50min is maintained, finally with 4 DEG C/min cooling rate and 0.04A/
Min electric current reduces speed and cools the temperature to room temperature, and electric current also is down into 0A, in addition, in first time insulating process, with
100ml/min speed is passed through ammonia into mixed solution, with 80ml/min speed to mixing in second of insulating process
Ammonia is passed through in solution.
It is 93% to determine its yield to the use of this embodiment and the identical detection method of embodiment 9, compared to embodiment 5
88% yield increases.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the embodiment with description.
Claims (9)
- The preparation method of carbon quantum dot 1. a kind of water-soluble nitrogen adulterates, it is characterised in that comprise the following steps：Precursor solution I is made Step 1: citric acid is dissolved in ultra-pure water, Para Amino Benzamide is dissolved in ultra-pure water and is made Precursor solution II, by volume 1~10:1 uniform mixing precursor solution I and precursor solution II, obtain mixed solution；Step 2: mixed solution made from step one is carried out into hydro-thermal reaction, you can obtain water-soluble nitrogen doping carbon quantum dot.
- The preparation method of carbon quantum dot 2. water-soluble nitrogen as claimed in claim 1 adulterates, it is characterised in that will in step one 1.0g citric acids, which are dissolved in 20mL ultra-pure waters, is made precursor solution I.
- The preparation method of carbon quantum dot 3. water-soluble nitrogen as claimed in claim 2 adulterates, it is characterised in that will in step one 0.1g Para Amino Benzamides, which are dissolved in 20mL ultra-pure waters, is made precursor solution II.
- The preparation method of carbon quantum dot 4. water-soluble nitrogen as claimed in claim 1 adulterates, it is characterised in that mixed in step 2 Solution also filtered successively after hydro-thermal reaction, dialyses, evaporates.
- The preparation method of carbon quantum dot 5. water-soluble nitrogen as claimed in claim 1 adulterates, it is characterised in that hydro-thermal in step 2 Reaction is carried out in isoperibol, and temperature is 160 DEG C, and the reaction time is 4h.
- The preparation method of carbon quantum dot 6. water-soluble nitrogen as claimed in claim 3 adulterates, it is characterised in that precursor in step one Solution I and precursor solution II by volume 5:1 is mixed.
- The preparation method of carbon quantum dot 7. water-soluble nitrogen as claimed in claim 4 adulterates, it is characterised in that dialysed in step 2 Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
- The preparation method of carbon quantum dot 8. water-soluble nitrogen as claimed in claim 4 adulterates, it is characterised in that evaporated in step 2 Using constant temperature rotary evaporation, temperature is 60 DEG C.
- The preparation method of carbon quantum dot 9. water-soluble nitrogen as claimed in claim 1 adulterates, it is characterised in that in step one and step Also carried out between rapid two：Step a, by made from step one mixed solution carry out ultrasonic disperse, ultrasonic frequency be 28~33KHz, the time be 20~ 35min, then will be ultrasonically treated after mixed solution carry out infrared heating processing, programming rate be 2 DEG C/min, final temperature be 54~58 DEG C, bipolar electrode system is put into heating process in mixed solution, anode is graphite electrode, and negative electrode is platinum electrode, carried out simultaneously Be powered, size of current press 0.01A/min speed increase, at the end of temperature-rise period, electric current also stop increase, maintain temperature with Current condition 30min, then rises to 78~84 DEG C, size of current presses 0.02A/min with 3 DEG C/min programming rate by temperature Speed increase, after assigned temperature is reached, maintain temperature and current condition 50min, finally with 4 DEG C/min cooling rate and 0.04A/min electric current reduces speed and cools the temperature to room temperature, and electric current also is down into 0A, in addition, in first time insulating process, Ammonia is passed through into mixed solution with 100ml/min speed, with 80ml/min speed to mixed in second of insulating process Close in solution and be passed through ammonia.
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| Publication number | Priority date | Publication date | Assignee | Title |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497762A (en) * | 2013-06-26 | 2014-01-08 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN103642494A (en) * | 2013-12-27 | 2014-03-19 | 中国科学院上海微***与信息技术研究所 | Preparation method for fluorescence carbon-based quantum dot |
| CN103663412A (en) * | 2013-12-05 | 2014-03-26 | 中国科学院大学 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
| CN104927849A (en) * | 2015-07-08 | 2015-09-23 | 安徽工业大学 | Green synthetic method for blue fluorescence carbon quantum dots with high fluorescence quantum yield |
| CN105176528A (en) * | 2015-08-24 | 2015-12-23 | 中物院成都科学技术发展中心 | Preparation method of nitrogen doped carbon based quantum dot |
| CN106587007A (en) * | 2016-11-22 | 2017-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Nitrogen-sulfur-doped pH-sensitive carbon quantum dots and preparing method and application |
-
2017
- 2017-07-26 CN CN201710619687.0A patent/CN107189777A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497762A (en) * | 2013-06-26 | 2014-01-08 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN103663412A (en) * | 2013-12-05 | 2014-03-26 | 中国科学院大学 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
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