CN106947475A - Al in fluorescent carbon quantum dot preparation method and its detection water3+Ion application - Google Patents
Al in fluorescent carbon quantum dot preparation method and its detection water3+Ion application Download PDFInfo
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Abstract
The present invention relates to a kind of fluorescent carbon quantum dot preparation method, method and step is as follows：S1：Electrolysis：Under 25 degrees celsius, NaOH solution is taken to be placed in 100mL beakers, using calomel electrode as reference electrode, two graphite rods ensure the distance between two graphite rods, control voltage and electrolysis time as positive and negative working electrode, to graphite rod electrolytic etching, brown solution is obtained；S2：Removal of impurities：After S1 steps terminate, the brown solution is subjected to centrifugal treating；S3：Purifying：After S2 steps terminate, the yellowish-brown carbon dots solution is put into bag filter, 24h is dialysed in ultra-pure water to remove alkali sodium hydroxide to neutrality.The present invention prepares fluorescent carbon quantum dot method simply, and the step of electrochemistry formated one is completed, and raw materials used is graphite rod, and electrolyte is NaOH solution, and toxicity, contaminative are all small.Compared to more other synthetic methods, the carbon quantum dot purity of electrochemistry formated is high, good crystallinity, no other impurities, without complicated purification and purification process after synthesis.
Description
Technical field
The present invention relates to a kind of carbon quantum dot preparing technical field, more particularly to a kind of fluorescent carbon quantum dot preparation method and
Its Al3+ ion application in detection water.
Background technology
Quantum dot is the nano material of the emerging quasi-zero dimension of a class, and this small size imparts its strong size limitation effect
Should and edge effect, so that stronger fluorescence can be produced, have widely in fields such as material science, electronic device, biochemistries
Application prospect.Earliest quantum dot is generally the sulfide or tellurides of some transition metal, such as cadmium sulfide, cadmium telluride,
But it is due to that these transition metal have certain toxicity, and their synthesis condition requires higher, and technique is also relative complex,
These defects significantly limit the application of quantum dot.Thus, it is controllable using the simple and environmentally-friendly extensive synthesis performance of method
Quantum dot has attracted the concern of numerous researchers, particularly the quantum dot based on carbon and silicon.
From researcher in 2004 since carbon quantum dot is had been surprisingly found that during purifying CNT, the system of carbon quantum dot
Preparation Method has obtained very big development, such as arc process, laser method, microwave method, but these methods often complex operation, equipment phase
To costliness, technique is cumbersome, and cost is higher, and yield is relatively low, significantly limit the application and development of carbon quantum dot.
Aluminium is metallic element most abundant in the earth's crust, is widely used in terms of food additives, medicine and Water warfare.
However, excessive aluminium is all harmful to environment and human body, as aluminium ion can damage the nervous system and immune system of people, cause
The diseases such as senile dementia, encephalopathic, senile dementia, chronic renal failure.In addition, aluminium ion excessive in environment is also harmful to
In the growth of plant.Accordingly, it would be desirable to develop quick and reliable method, come determine and assess the content of aluminium ion in the environment and
It is potentially hazardous.
Compared with other detection aluminium ion technologies, fluorescence analysis have unique advantage, such as high sensitivity, high selection
Property, quick response speed and low cost and enjoy favor.But by aluminium ion coordination ability is poor, lack transition metal ions institute
The spectral characteristic having, makes to be used for detecting that aluminum ions fluorescent optical sensor is more rare at present.At present it has been reported that lack
Amount is all based on organic fluorescence probe, such as 2- hydroxyl-1-naphthalene Formaldehydes fluorescence probe, 4- (diethyls on aluminium ion fluorescent optical sensor
Amino) -2- hydroxyls fluorescence and Rhodamine Derivatives fluorescence probe etc..The organo-aluminium ion fluorescence sensor of these reports is all needed
Complicated building-up process is wanted, various organic reagents all have potential toxicity and environmental pollution, and the organic fluorescence of these synthesis
Probe is most of water insoluble, it is impossible to detect the aluminium ion in water body, greatly limit their applications in practice.
The content of the invention
In view of the deficiency that prior art is present, one of the object of the invention is to provide a kind of fluorescent carbon quantum dot preparation side
Method.
Another purpose of the invention is the fluorescent carbon quantum dot prepared using the above method Al in detection water3+Contain
Amount.
The technical proposal of the invention is realized in this way：
A kind of fluorescent carbon quantum dot preparation method, it is characterised in that：Method and step is as follows：
S1：Electrolysis：Under 25 degrees celsius, NaOH solution is taken to be placed in 100mL beakers, it is electric by reference of calomel electrode
Pole, two graphite rods ensure the distance between two graphite rods as positive and negative working electrode, control voltage and electrolysis time,
To graphite rod electrolytic etching, brown solution is obtained；
S2：Removal of impurities：After S1 steps terminate, the brown solution is subjected to centrifugal treating；
S3：Purifying：After S2 steps terminate, the yellowish-brown carbon dots solution is put into bag filter, in ultra-pure water thoroughly
24h is analysed to remove alkali sodium hydroxide to neutrality.
In some preferred embodiments, the concentration of the S1 steps NaOH is 0.5-5.5moL/L, and volume is 20-
60mL。
In some preferred embodiments, the electrolytic condition of the S1 steps is：The distance between described graphite rod is
0.5-2cm, the voltage is respectively 1.5-2.5v, electrolysis time is set to 140-200h.
In some preferred embodiments, the rotating speed 5500-8500rpm centrifuged described in S2 steps, centrifugation time 5-
20min。
In some preferred embodiments, bag filter specification described in S3 steps is 3500Da, and is dialysed in ultra-pure water
18-72h。
Fluorescent carbon quantum dot is made present invention also offers above-mentioned preparation method.
Due to the presence of oxygen, during carbon quantum dot electrochemistry formated, edge carbons are oxidized to carboxyl simultaneously
With the group such as carbonyl so that prepared quantum dot has good hydrophily, it can disperse for a long time in aqueous without rolling into a ball
It is poly-, with stable photoluminescent property；The groups such as substantial amounts of carboxyl and carbonyl exist and can had with part heavy metal ion
Good coordination, so as to be used as the detection probe of heavy metal ion.
The present invention optionally detects the aluminium ion in water using the carbon quantum of electrochemistry formated, with other fluoroscopic examinations
Aluminum ions organic fluorescence fluorescence probe is compared, and carbon quantum dot small toxicity, building-up process are simple, and a step is completed, and good water solubility is pure
Degree is high, without purifying and purifying, and raw materials used is graphite rod, and electrolyte is NaOH solution, and toxicity, contaminative are all small.While with
Other methods for preparing carbon quantum dots are compared, carbon quantum dot purity height of electrochemistry formated, good crystallinity, without other impurities, electric
Chemical synthesis process will be synthesized and the modification of its surface oxidation functional group is synchronously completed, and carbon quantum prepared by other various methods
Point, prepared by carbon point and surface modification will be carried out step by step, and process is complicated.
Present invention also offers described fluorescent carbon quantum dot detection water in Al3+Application in ion.
Present invention also offers described fluorescent carbon quantum dot detection river in Al3+Application in ion.
In some embodiments, a kind of fluorescent carbon quantum dot Al in detection river3+The method of ion, method and step is such as
Under：a：Filtering：By the river membrane filtration of collection；b：Add the Al of various concentrations3+Standard liquid；c：Utilize prepared carbon
Its levels of quantum point analysis.
In some preferred embodiments, the aperture of filter membrane is described in gained step a：0.25-0.55μm.
Compared with prior art, the device have the advantages that：
1st, fluorescent carbon quantum dot method is prepared simple, the step of electrochemistry formated one is completed, raw materials used is graphite rod, electrolyte
For NaOH solution, toxicity, contaminative are all small.
2nd, compared to more other synthetic methods, the carbon quantum dot purity of electrochemistry formated is high, and good crystallinity is miscellaneous without other
Matter, without complicated purification and purification process after synthesis.
3rd, electrochemical method for synthesizing will be synthesized and the modification of its surface oxidation functional group is synchronously completed, and other various methods
The carbon quantum dot of preparation, prepared by carbon point and surface modification will be carried out step by step, and process is complicated.
4th, prepared carbon quantum dot has unique high selectivity, highly sensitive enhancement effect of fluorescence to aluminium ion, can
For the aluminium composition in detection water body.
Brief description of the drawings
Fig. 1 is the transmission electron microscope phenogram of the carbon quantum dot prepared by embodiment 1 (A, B), and (C) particle diameter distribution and (D) are drawn
Graceful spectrogram.
Fig. 2 is infrared spectrogram and (B) ultraviolet spectrogram (a, the respectively day of the carbon quantum dot prepared by embodiment 1 (A)
The color of carbon quantum dot solution under light etc. time and 365nm uviol lamps).
The fluorescence spectra of carbon quantum dot prepared by Fig. 3, embodiment 1 (A), the carbon quantum dot prepared by (B) is to difference
The fluorescence response situation of metal ion, (wherein a is Al to (C) photoluminescent property with electrolysis time relation3+After carbon quantum dot effect
Fluorescence Increasing property and electrolysis time relation, photoluminescent property and electrolysis time relation when b is without Al3+ after carbon quantum dot effect；
Fluorescence condition：Excitation wavelength, 434nm, launch wavelength 510nm), (D) solution ph is to prepared carbon quantum dot photoluminescent property shadow
Ring (a) and add Al3+Fluorescence Increasing property influence (b) afterwards.
Carbon bright spot is to various concentrations Al prepared by Fig. 4, embodiment 1 (A)3+Fluorescence response figure, (B) corresponding linear relationship
Figure.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, but does not constitute to any of the present invention
Limitation.
Main agents, raw material sources explanation：
Graphite rod：Purchased from AlfaAesar (China) Chemical Co., Ltd., purity 99.99%；Calomel electrode is purchased from Shanghai occasion
Magnificent Instrument Ltd..
Embodiment 1：
It is prepared by fluorescent carbon quantum dot
Under 25 degrees celsius, take the NaOH solution of 50mL2 mol/Ls to be placed in 100mL beakers, using calomel electrode as
Reference electrode, two business high purity graphite rods ensure that the distance between two graphite rods are 1cm as positive and negative working electrode,
Control voltage is respectively 2.0V, carries out continuous electrolytic oxidation to graphite rod using potentiostatic method, electrolysis time is set to 170h.
As electrolysis time increases, otherwise transparent solution slowly becomes yellow solution, and final color is deepened until yellowish-brown
Color solution.After electrolysis terminates, above-mentioned brown solution is subjected to centrifugal treating, centrifuged 10 minutes in the case where rotating speed is 7500 turn, with
Go out large granular impurity, continuously repeat centrifugally operated 2 times.Yellowish-brown carbon dots solution after centrifugation is put into bag filter, specification：
3500Da, dialyses 24h to remove alkali sodium hydroxide to neutrality in ultra-pure water.
Due to the presence of oxygen, during carbon quantum dot electrochemistry formated, edge carbons are oxidized to carboxyl simultaneously
With the group such as carbonyl so that prepared quantum dot has good hydrophily, it can disperse for a long time in aqueous without rolling into a ball
It is poly-, with stable photoluminescent property；The groups such as substantial amounts of carboxyl and carbonyl exist and can had with part heavy metal ion
Good coordination, so as to be used as the detection probe of heavy metal ion.
Pattern such as Fig. 1 (A and B) after made carbon quantum dot is characterized under transmission electron microscope (TEM) is shown, and its particle diameter exists
Between 4.0-8.0nm, average grain diameter is that spacing of lattice is 0.24nm between 5.0nm or so (Fig. 1 C), atom, correspondence graphitic carbon
020 crystal face.
The prepared carbon point D bands of Raman Characterization (Fig. 1 D) determination and G bands are located at 1339 and 1594cm-1 respectively, and
Raman spectrum strength ID/IG=0.920, illustrates the carbon atom of part aromatic ring sp2 hydridization of the carbon quantum dot prepared by oxygen
It is melted into the carbon oxygen groups of sp3 hydridization.
The prepared carbon quantum dot of infrared spectrum characterization (Fig. 2A) display is in 1751,1598 and 1361cm-1Place has bright respectively
Aobvious absworption peak, corresponding should be C=O stretching vibration absworption peak, COO-Flexible and symmetric vibration absworption peak.Exist simultaneously
910 and 631cm-1It should be aromatic ring Ar-H vibration absorption peak that place is corresponding.C=O present in infrared spectrum and COO-It is special
Levy absworption peak and further demonstrate the carbon atom of part aromatic ring sp2 hydridization in prepared carbon quantum dot and be oxidized to oxygen containing carboxylic
The group such as base and carbonyl.
Ultraviolet spectra characterizes (Fig. 2 B) and shows that prepared carbon quantum dot has absorption in larger wave-length coverage,
There is a most strong absworption peak at 288nm, corresponding should be the n-π * energy level transition absworption peaks of C=O in carboxyl.Prepared is yellowish-brown
Dark green fluorescence (Fig. 2 B) is presented in color carbon quantum dot under 365nm uviol lamps.
600 μ L carbon dots solutions are diluted to 3mL with redistilled water, characterized for photoluminescent property.As a result (Fig. 3 A) is shown,
Prepared carbon point has the photoluminescent property of multi-point shooting.In the case where 330 and 434nm wavelength is excited, respectively in 448 Hes
Fluorescence emission peak is produced at 510nm, and the fluorescence emission peak at 448nm wavelength is most strong.Prepared carbon quantum dot is simultaneously
Also have upper converting photoluminescent property, when excitation wavelength increases to 900nm from 600nm, corresponding maximum emission wavelength from
396nm red shifts are at 491nm, wherein in the case where 700nm wavelength is excited, having most hyperfluorescence emission peak at 423nm, illustrating made
Standby carbon quantum dot has multi-point shooting and up-conversion luminescence property.
The effect of prepared fluorescent carbon quantum dot and heavy metal ion：
600 μ L carbon dots solutions are diluted to 3mL with redistilled water, different metal ions, Al are then added3+、Ag+、As3 +、Hg2+、Ca2+、Zn2+、Pb2+、Cu2+、Cd2+、Fe3+And Co2+, after heavy metal ion and carbon dots solution are fully acted on, record it
Change in fluorescence situation at 510nm (excitation wavelength 434nm) place, experimental result (Fig. 3 B) display only has Al3+To prepared carbon
There is quantum dot solution obvious Fluorescence Increasing to respond, and fluorescent quenching effect or glimmering is presented in the heavy metal ion of other experiments
Light change is not obvious.It these results suggest that Al3+The fluorescence intensity to prepared carbon quantum dot with high selectivity is responded, so
Can be using the carbon quantum dot come Al in selective detection water-outlet body using this feature3+。
Electrolysis time Optimal Experimental (Fig. 3 C) shows, Al3+Fluorescence intensity response and carbon amounts to prepared carbon quantum dot
Electrolysis time in son point preparation process has certain corresponding relation, before electrolysis time is less than 130h, Al3+To carbon quantum
Point has fluorescent quenching effect, after electrolysis time is more than 140h, starts with obvious enhancement effect of fluorescence, and arrives 170h
There is a maximum enhancement value.
Aqueous solution acid-base value Optimal Experimental (Fig. 3 D) shows, is in the range of 4-8 in pH value, prepared carbon quantum dot and
Itself and Al3+Photoluminescent property during effect is all hardly influenceed by acid-base value, illustrates prepared carbon quantum dot in very wide pH
In the range of detect Al3+, the pH value without adjusting solution, therefore this experiment solvent for use is two adjusted without cushioning liquid
Secondary distilled water.
Under the experiment condition of optimization, (by 600 μ L carbon dots solution redistilled waters in prepared carbon quantum dot solution
It is diluted to 3mL) to the Al in 0.1-7.2 μM of annual scope3+With Linear-phase relation, minimal detectable concentration is 0.05 μM of (figure
4A、B)。
Embodiment 2：
Under 25 degrees celsius, the NaOH solution of the mol/Ls of 60mL 0.5 is taken to be placed in 100mL beakers, with calomel electricity
Extremely reference electrode, two business high purity graphite rods ensure that the distance between two graphite rods are as positive and negative working electrode
2cm, control voltage is respectively 2.5V, carries out continuous electrolytic oxidation to graphite rod using potentiostatic method, electrolysis time is set to
200h。
Embodiment 3
A kind of fluorescent carbon quantum dot preparation method, it is characterised in that：Method and step is as follows：
S1：Electrolysis：Under 25 degrees celsius, NaOH solution is taken to be placed in 100mL beakers, it is electric by reference of calomel electrode
Pole, two graphite rods ensure the distance between two graphite rods as positive and negative working electrode, control voltage and electrolysis time,
To graphite rod electrolytic etching, brown solution is obtained；
S2：Removal of impurities：After S1 steps terminate, the brown solution is subjected to centrifugal treating；
S3：Purifying：After S2 steps terminate, the yellowish-brown carbon dots solution is put into bag filter, in ultra-pure water thoroughly
24h is analysed to remove alkali sodium hydroxide to neutrality.
The concentration of the S1 steps NaOH is 1.0moL/L, and volume is 30mL.
The electrolytic condition of the S1 steps is：The distance between described graphite rod is 0.5-2cm, and the voltage is respectively
1.2v, makes electrolysis time be set to 160h.
In some preferred embodiments, the rotating speed 6500rpm centrifuged described in S2 steps, centrifugation time 10min.
In some preferred embodiments, bag filter specification described in S3 steps is 3500Da, and is dialysed in ultra-pure water
18h。
Embodiment 4
A kind of fluorescent carbon quantum dot preparation method, it is characterised in that：Method and step is as follows：
S1：Electrolysis：Under 25 degrees celsius, NaOH solution is taken to be placed in 100mL beakers, it is electric by reference of calomel electrode
Pole, two graphite rods ensure the distance between two graphite rods as positive and negative working electrode, control voltage and electrolysis time,
To graphite rod electrolytic etching, brown solution is obtained；
S2：Removal of impurities：After S1 steps terminate, the brown solution is subjected to centrifugal treating；
S3：Purifying：After S2 steps terminate, the yellowish-brown carbon dots solution is put into bag filter, in ultra-pure water thoroughly
24h is analysed to remove alkali sodium hydroxide to neutrality.
In some preferred embodiments, the concentration of the S1 steps NaOH is 1.5moL/L, and volume is 35mL.
In some preferred embodiments, the electrolytic condition of the S1 steps is：The distance between described graphite rod is
01.4cm, the voltage is respectively 1.5v, electrolysis time is set to 180h.
In some preferred embodiments, the rotating speed 7500rpm centrifuged described in S2 steps, centrifugation time 150min.
In some preferred embodiments, bag filter specification described in S3 steps is 3500Da, and is dialysed in ultra-pure water
36h。
Embodiment 5
A kind of fluorescent carbon quantum dot preparation method, it is characterised in that：Method and step is as follows：
S1：Electrolysis：Under 25 degrees celsius, NaOH solution is taken to be placed in 100mL beakers, it is electric by reference of calomel electrode
Pole, two graphite rods ensure the distance between two graphite rods as positive and negative working electrode, control voltage and electrolysis time,
To graphite rod electrolytic etching, brown solution is obtained；
S2：Removal of impurities：After S1 steps terminate, the brown solution is subjected to centrifugal treating；
S3：Purifying：After S2 steps terminate, the yellowish-brown carbon dots solution is put into bag filter, in ultra-pure water thoroughly
24h is analysed to remove alkali sodium hydroxide to neutrality.
In some preferred embodiments, the concentration of the S1 steps NaOH is 3.0moL/L, and volume is 45mL.
In some preferred embodiments, the electrolytic condition of the S1 steps is：The distance between described graphite rod is
1.6cm, the voltage is respectively 3.0v, electrolysis time is set to 190h.
In some preferred embodiments, the rotating speed 7000rpm centrifuged described in S2 steps, centrifugation time 18min.
In some preferred embodiments, bag filter specification described in S3 steps is 3500Da, and is dialysed in ultra-pure water
60h。
Embodiment 6
A kind of fluorescent carbon quantum dot preparation method, it is characterised in that：Method and step is as follows：
S1：Electrolysis：Under 25 degrees celsius, NaOH solution is taken to be placed in 100mL beakers, it is electric by reference of calomel electrode
Pole, two graphite rods ensure the distance between two graphite rods as positive and negative working electrode, control voltage and electrolysis time,
To graphite rod electrolytic etching, brown solution is obtained；
S2：Removal of impurities：After S1 steps terminate, the brown solution is subjected to centrifugal treating；
S3：Purifying：After S2 steps terminate, the yellowish-brown carbon dots solution is put into bag filter, in ultra-pure water thoroughly
24h is analysed to remove alkali sodium hydroxide to neutrality.
In some preferred embodiments, the concentration of the S1 steps NaOH is 3.5moL/L, and volume is 55mL.
In some preferred embodiments, the electrolytic condition of the S1 steps is：The distance between described graphite rod is
1.8cm, the voltage is respectively 3.2v, electrolysis time is set to 170h.
In some preferred embodiments, the rotating speed 720rpm centrifuged described in S2 steps, centrifugation time 12min.
In some preferred embodiments, bag filter specification described in S3 steps is 3500Da, and is dialysed in ultra-pure water
58h。
Claims (10)
1. a kind of fluorescent carbon quantum dot preparation method, it is characterised in that：Method and step is as follows：
S1：Electrolysis：Under 25 degrees celsius, NaOH solution is taken to be placed in 100mL beakers, using calomel electrode as reference electrode,
Two graphite rods ensure the distance between two graphite rods, control voltage and electrolysis time, to stone as positive and negative working electrode
Inker electrolytic etching, obtains brown solution；
S2：Removal of impurities：After S1 steps terminate, the brown solution is subjected to centrifugal treating；
S3：Purifying：After S2 steps terminate, the yellowish-brown carbon dots solution is put into bag filter, dialyse 24h in ultra-pure water
To remove alkali sodium hydroxide to neutrality.
2. fluorescent carbon quantum dot preparation method according to claim 1, it is characterised in that：The concentration of the S1 steps NaOH
For 0.5-5.5moL/L, volume is 20-60mL.
3. fluorescent carbon quantum dot preparation method according to claim 1, it is characterised in that：The electrolytic condition of the S1 steps
For：The distance between described graphite rod is 0.5-2cm, and the voltage is respectively 0.5-2.5v, electrolysis time is set to 140-
200h。
4. fluorescent carbon quantum dot preparation method according to claim 1, it is characterised in that：What is centrifuged described in S2 steps turns
Fast 5500-8500rpm, centrifugation time 5-20min.
5. fluorescent carbon quantum dot preparation method according to claim 1, it is characterised in that：Bag filter described in S3 steps is advised
Lattice are 3500Da, and the 18-72h that dialyses in ultra-pure water.
6. fluorescent carbon quantum dot made from preparation method described in claim 1-5 any one.
7. the Al in detection water of the fluorescent carbon quantum dot described in claim 63+Application in ion.
8. the Al in detection river of the fluorescent carbon quantum dot described in claim 63+Application in ion.
9. a kind of fluorescent carbon quantum dot Al in detection river3+The method of ion, it is characterised in that：Method and step is as follows：a：Cross
Filter：By the river membrane filtration of collection；b：Add the Al3+ standard liquids of various concentrations；c：Utilize prepared carbon quantum dot
Analyze its levels.
10. the method for fluorescent carbon quantum dot according to claim 9 Al3+ ions in detection river, it is characterised in that：
The aperture of filter membrane is described in gained step a：0.25-0.55μm.
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| CN107694605A (en) * | 2017-11-01 | 2018-02-16 | 中国科学院福建物质结构研究所 | Carbon quantum dot@porphyryl metal organic framework catalyst and preparation method and application |
| CN107974249A (en) * | 2017-12-06 | 2018-05-01 | 南京工业大学 | Preparation method and application of polydopamine quantum dot-based fluorescent probe for detecting glutamic acid and aluminum ions |
| CN108033437A (en) * | 2017-12-08 | 2018-05-15 | 中国矿业大学 | A kind of quick method for preparing carbon dots of salt auxiliary |
| CN109975253A (en) * | 2017-12-27 | 2019-07-05 | 中国科学院宁波材料技术与工程研究所 | Fluorescence indicator combination, fluorescence sensor array, preparation method and application |
| CN112095113A (en) * | 2020-09-07 | 2020-12-18 | 太原理工大学 | Method for preparing carbon quantum dots by taking coal as raw material |
| CN112408362A (en) * | 2019-08-21 | 2021-02-26 | 中国石油大学(北京) | Carbon quantum dot and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402858A (en) * | 2008-11-19 | 2009-04-08 | 武汉大学 | Process for producing low-toxicity fluorescent carbon point |
| CN104934232A (en) * | 2015-05-13 | 2015-09-23 | 东南大学 | Titanium dioxide or titanium nitride supported carbon quantum dot modification polypyrrole nanometer array material and preparation method and application thereof |
| CN105714323A (en) * | 2016-03-01 | 2016-06-29 | 常州大学 | Method for rapidly preparing fluorescent carbon quantum dot by using direct-current pulse process |
| CN106398693A (en) * | 2016-08-31 | 2017-02-15 | 山西大学 | Preparation method and application of nitrogen doped yellow fluorescent carbon dots |
-
2017
- 2017-03-30 CN CN201710200189.2A patent/CN106947475B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402858A (en) * | 2008-11-19 | 2009-04-08 | 武汉大学 | Process for producing low-toxicity fluorescent carbon point |
| CN104934232A (en) * | 2015-05-13 | 2015-09-23 | 东南大学 | Titanium dioxide or titanium nitride supported carbon quantum dot modification polypyrrole nanometer array material and preparation method and application thereof |
| CN105714323A (en) * | 2016-03-01 | 2016-06-29 | 常州大学 | Method for rapidly preparing fluorescent carbon quantum dot by using direct-current pulse process |
| CN106398693A (en) * | 2016-08-31 | 2017-02-15 | 山西大学 | Preparation method and application of nitrogen doped yellow fluorescent carbon dots |
Non-Patent Citations (1)
| Title |
|---|
| 李腾飞，等: "荧光可调控的碳量子点的电化学制备及性质研究", 《ACTA CHIM.SINICA》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107694605A (en) * | 2017-11-01 | 2018-02-16 | 中国科学院福建物质结构研究所 | Carbon quantum dot@porphyryl metal organic framework catalyst and preparation method and application |
| CN107974249A (en) * | 2017-12-06 | 2018-05-01 | 南京工业大学 | Preparation method and application of polydopamine quantum dot-based fluorescent probe for detecting glutamic acid and aluminum ions |
| CN107974249B (en) * | 2017-12-06 | 2020-03-27 | 南京工业大学 | Preparation method and application of polydopamine quantum dot-based fluorescent probe for detecting glutamic acid and aluminum ions |
| CN108033437A (en) * | 2017-12-08 | 2018-05-15 | 中国矿业大学 | A kind of quick method for preparing carbon dots of salt auxiliary |
| CN109975253A (en) * | 2017-12-27 | 2019-07-05 | 中国科学院宁波材料技术与工程研究所 | Fluorescence indicator combination, fluorescence sensor array, preparation method and application |
| CN109975253B (en) * | 2017-12-27 | 2022-05-31 | 中国科学院宁波材料技术与工程研究所 | Fluorescent indicator composition, fluorescent array sensor, preparation method and application thereof |
| CN112408362A (en) * | 2019-08-21 | 2021-02-26 | 中国石油大学(北京) | Carbon quantum dot and preparation method and application thereof |
| CN112095113A (en) * | 2020-09-07 | 2020-12-18 | 太原理工大学 | Method for preparing carbon quantum dots by taking coal as raw material |
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