CN109957398A - Nitrogen-doped carbon quantum dot and preparation method thereof - Google Patents
Nitrogen-doped carbon quantum dot and preparation method thereof Download PDFInfo
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- CN109957398A CN109957398A CN201711427000.XA CN201711427000A CN109957398A CN 109957398 A CN109957398 A CN 109957398A CN 201711427000 A CN201711427000 A CN 201711427000A CN 109957398 A CN109957398 A CN 109957398A
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Abstract
The present invention provides a kind of preparation methods of nitrogen-doped carbon quantum dot, comprising the following steps: provides hair and/or hair as carbon matrix precursor, the carbon matrix precursor is carried out carbonization treatment in inert environments, obtains carbon source；The carbon source is mixed with nitric acid, nitrogen-doped carbon quantum dot is prepared through hydro-thermal reaction.
Description
Technical field
The invention belongs to quantum dot synthesis technical fields more particularly to a kind of nitrogen-doped carbon quantum dot and preparation method thereof.
Background technique
Due to the excellent properties with unique electricity, optics, mechanics etc., quantum dot is passed in photoelectric display, biology
The fields such as sense, solar battery have a wide range of applications, and have become a hot topic of research.Contain a huge sum of money in traditional fluorescence quantum
Belong to element, such as Cd, Te, not only preparation cost is high for these traditional quantum dots, and has stronger bio-toxicity.In addition, system
Standby conventional fluorescent quantum dot needs water and oxygen in strict control preparation process, this is proposed very to equipment and synthesis technology
High requirement.Defect of traditional quantum dot in terms of these limits its application and development.
For carbon quantum dot as a kind of fluorescent nano material, contained substance is mainly carbon, and carbon is that nature is most rich
Rich one of element, therefore cost is relatively low for carbon quantum dot.Carbon quantum dot has lower conversion, upper conversion photoluminescent property, chemical stability
It is good, there is good biocompatibility and hypotoxicity, have in terms of bio-imaging, medical diagnosis, catalysis and photovoltaic device wide
General application prospect.At present there are many ways to synthesis carbon quantum dot, but mostly preparation process is complicated, and the period is long, product purity
Low, there is also more drawbacks.
Summary of the invention
The purpose of the present invention is to provide a kind of nitrogen-doped carbon quantum dots and preparation method thereof, it is intended to solve existing carbon amounts
Son point preparation process is complicated, and the period is long, the low problem of product purity.
For achieving the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of nitrogen-doped carbon quantum dot, comprising the following steps:
Hair and/or hair are provided as carbon matrix precursor, the carbon matrix precursor is subjected to carbonization treatment in inert environments,
Obtain carbon source；
The carbon source is mixed with nitric acid, nitrogen-doped carbon quantum dot is prepared through hydro-thermal reaction.
And a kind of nitrogen-doped carbon quantum dot, the nitrogen-doped carbon quantum dot are prepared by the above method.
The preparation method of nitrogen-doped carbon quantum dot provided by the invention, firstly, using hair and/or hair as carbon forerunner
Body, the hair, hair are the common substances of nature, not only from a wealth of sources, are highly susceptible to obtaining, advantageously reduce N doping
The preparation cost of carbon quantum dot；And the carbon content in the hair, hair is up to 45%, is highly suitable as carbon matrix precursor use
In preparation carbon quantum dot.Secondly, using after carbonization treatment the hair and/or hair as preparation carbon quantum dot carbon
Source mixes with nitric acid and prepares through hydro-thermal reaction with nitrogen-doped carbon quantum dot.On the one hand, the nitric acid is as nitrogen-doped carbon quantum dot
Nitrogen source, that is, nitro is provided, the nitrogen-oxygen bond in the hydro-thermal reaction of continuous high temperature, the nitro is easily broken off, to form N doping
It on the surface of carbon quantum dot, combines closely with carbon quantum dot, forms nitrogen-doped carbon quantum dot, be obviously improved the fluorescence of carbon quantum dot
Quantum yield and fluorescence intensity.On the other hand, the nitric acid simultaneously be used as passivator, oxidant, to carbon quantum dot surface into
Row oxidation, passivation, increase the content of carbon quantum dot surface oxygen functional group, reduce the defect on carbon quantum dot surface, improve fluorescence
Intensity.In addition, the preparation method of nitrogen-doped carbon quantum dot provided by the invention, need to only use two kinds of raw materials (raw material is few), not allow
It is easily introduced impurity, preparation method is easy to operate, and repeatability is very high, and the nitrogen-doped carbon quantum dot material that the present invention prepares
Material, will not introduce the pollution sources such as heavy metal, bio-toxicity can be greatly lowered, and is environment friendly and pollution-free in preparation process, be a kind of
Green safe preparation method.
Nitrogen-doped carbon quantum dot provided by the invention, is prepared by the above method, and obtained nitrogen-doped carbon quantum dot is not
Only size uniformity, purity is high, and quantum dot rate is high, luminous efficiency is good, can be widely used for preparing nanocomposite, light
The fields such as electrical part and biosensor.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
The embodiment of the invention provides a kind of preparation methods of nitrogen-doped carbon quantum dot, comprising the following steps:
S01. hair and/or hair are provided as carbon matrix precursor, the carbon matrix precursor is carbonized in inert environments
Processing, obtains carbon source；
S02. the carbon source is mixed with nitric acid, nitrogen-doped carbon quantum dot is prepared through hydro-thermal reaction.
The preparation method of nitrogen-doped carbon quantum dot provided in an embodiment of the present invention, firstly, using hair and/or hair conduct
Carbon matrix precursor, the hair, hair are the common substances of nature, not only from a wealth of sources, are highly susceptible to obtaining, advantageously reduce
The preparation cost of nitrogen-doped carbon quantum dot；And the carbon content in the hair, hair is up to 45%, before being highly suitable as carbon
It drives body and is used to prepare carbon quantum dot.Secondly, using after carbonization treatment the hair and/or hair as preparation carbon quantum dot
Carbon source, mix with nitric acid and prepare through hydro-thermal reaction with nitrogen-doped carbon quantum dot.On the one hand, the nitric acid is as N doping carbon amounts
Son point provides nitrogen source, that is, nitro, and the nitrogen-oxygen bond in the hydro-thermal reaction of continuous high temperature, the nitro is easily broken off, to form nitrogen
It is entrained in the surface of carbon quantum dot, is combined closely with carbon quantum dot, nitrogen-doped carbon quantum dot is formed, is obviously improved carbon quantum dot
Fluorescence quantum yield and fluorescence intensity.On the other hand, the nitric acid is used as passivator, oxidant simultaneously, to carbon quantum dot table
Face is aoxidized, is passivated, and the content of carbon quantum dot surface oxygen functional group is increased, and reduces the defect on carbon quantum dot surface, is improved
Fluorescence intensity.In addition, the preparation method of nitrogen-doped carbon quantum dot provided in an embodiment of the present invention, only need to use two kinds of raw materials (former
Material is few), it is not easy to impurity is introduced, preparation method is easy to operate, repeatability is very high, and the embodiment of the present invention prepares
Nitrogen-doped carbon quanta point material will not introduce the pollution sources such as heavy metal, and bio-toxicity, and preparation process middle ring can be greatly lowered
It protects pollution-free, is a kind of green safe preparation method.
Specifically, in above-mentioned steps S01, the hair, hair phosphorus content be up to 45%, and ingredient is relatively single, warp
High temperature cabonization processing can obtain the carbon source of carbon content superelevation, be highly suitable as carbon precursor preparation carbon quantum dot.In addition, institute
Hair, hair abundance are stated, cost is relatively low, can reduce cost of manufacture.
It further include that the carbon source is subjected to cleaning treatment, to remove surface before the hair, hair are carried out carbonization treatment
Oily matter and other impurities.It is specific preferred, the method that the carbon source is subjected to cleaning treatment are as follows: the hair that will be provided
And/or hair successively uses dish washing liquid, acetone, alcohol, ultrapure water to be cleaned.Using specific cleaning reagent according to it is above-mentioned into
Row cleaning, can substantially effectively remove the oily matter and other miscellaneous, carbon sources for being of hair and/or hair surface
Carbon content is more secure.
Further, the carbon matrix precursor is subjected to carbonization treatment in inert environments, removes extra non-carbon element, mentions
The phosphorus content of high carbon source.Preferably, the temperature of the carbonization treatment is 600-800 DEG C, and the time is 1-3 hours, with this condition,
Hair and/or hair are sufficiently carbonized.If the temperature of the carbonization treatment is too low and/or the time is too short, carbonization is not exclusively, unfavorable
Carbon content is too low in carbon source after the preparation of carbon quantum dot, or carbonization, the reduced performance of obtained carbon quantum dot；If the institute
State carbonization treatment temperature is excessively high and/or overlong time, then influence the dimensional homogeneity and fluorescence property of subsequent carbon quantum dot.More
Further, under the conditions of above-mentioned carbonization treatment, the carbon for the carbon source that the hair and/or hair obtain after carbonization treatment
Content is higher than 90%.
In the embodiment of the present invention, the carbonization carries out under an inert atmosphere, to guarantee in carbonisation not by external environment
Interference, guarantee that the purity of carbon content and carbon source (reduces the introducing of impurity, finally obtains the nitrogen-doped carbon quantum of purity is high
Point).The inert atmosphere includes but is not limited to nitrogen.The heating device of the carbonization treatment does not limit strictly, it is preferred to use
High temperature cabonization processing is carried out in tube furnace.
In above-mentioned steps S02, nitric acid is provided, on the one hand the nitric acid is used as the carbon source of nitrogen-doped carbon quantum dot, another party
Face, the nitric acid has excellent oxidation, passivation effect to obtained carbon quantum dot, therefore the nitric acid is used as passivator simultaneously
And oxidant, oxidation, passivation carbon quantum dot surface, and then increase the content of its surface oxygen functional group, reduce carbon quantum dot table
The defect in face improves fluorescence intensity.Preferably, the concentration of the nitric acid is 2-6mol/L, to give full play to above-mentioned two aspect
Performance, and avoid corrosion of the excessive concentrations to the carbon quantum dot.
As another implementation situation, the nitric acid mainly as nitrogen-doped carbon quantum dot nitrogen source, meanwhile, be added it is other
Substance carries out surface oxidation to carbon quantum dot as oxidant, passivator, reduces the surface defect of carbon quantum dot.At this point, institute
The concentration and/or content for stating nitric acid can be reduced suitably.Specifically, being carried out using sulfuric acid as oxidant, passivator to carbon quantum dot
Surface oxidation reduces the surface defect of carbon quantum dot.But the type of oxidant, passivator is not limited to sulfuric acid.
Further, the carbon source is mixed with nitric acid.Preferably, by the carbon source and the nitric acid according to quality volume
Than the ratio mixing for 1g:(1-3) ml, to control reasonable carbon doping, be conducive to obtain fluorescent quantum quantum yield and
Fluorescence intensity more preferably nitrogen-doped carbon quantum dot, the quantum dot light emitting layer material being suitable in light emitting diode with quantum dots (QLED)
Material.
The carbon source and nitric acid are subjected to continuous high temperature hydro-thermal reaction, the nitrogen-oxygen bond fracture in reaction process in nitro, shape
It at N doping on the surface of the carbon quantum dot of formation, combines closely with carbon quantum dot, nitrogen-doped carbon quantum dot is formed, thus significantly
Promote the fluorescence quantum yield and fluorescence intensity of carbon quantum dot.Preferably, the temperature of the hydro-thermal reaction is 150-200 DEG C,
Reaction time is 4-8 hours.If reaction temperature is too low, react insufficient, be both unfavorable for doping of the nitrogen in carbon quantum dot,
It is unfavorable for passivation, oxidation of the nitric acid to carbon quantum dot；If reaction temperature is excessively high, the carbon quantum dot generated is easy to happen reunion.
In the embodiment of the present invention, the hydro-thermal reaction carries out preferably in pyroreaction kettle, due to nitric acid or other oxidations
Agent, the corrosivity of passivator are higher, and the reaction kettle of the hydro-thermal reaction is preferably the pyroreaction with polytetrafluoroethylliner liner
In kettle.
After hydro-thermal reaction, mixed system is cooled to room temperature (10-30 DEG C), is successively centrifuged, dialysed, drying place
Reason collects nitrogen-doped carbon quantum dot.
Carbon quantum dot size uniformity that the above method of the embodiment of the present invention prepares, can be directly dispersing in purity is high
It is used in water, can also be prepared into using after solid, can be widely used for preparing nanocomposite, photoelectric device
And biosensor etc..
And the embodiment of the invention also provides a kind of nitrogen-doped carbon quantum dots, the nitrogen-doped carbon quantum dot is by above-mentioned
Method prepares.
Nitrogen-doped carbon quantum dot provided in an embodiment of the present invention, is prepared by the above method, obtained N doping carbon amounts
Son puts not only size uniformity, purity is high, but also quantum dot rate is high, luminous efficiency is good, can be widely used for preparing nano combined
The fields such as material, photoelectric device and biosensor.
It is illustrated combined with specific embodiments below.
Embodiment 1
The embodiment of the invention provides a kind of preparation methods of nitrogen-doped carbon quantum dot, comprising the following steps:
S11. the hair come will be collected and be used as carbon source, it is once purged, it is put into tube furnace, annealing is 3 small under the conditions of 600 DEG C
When, the carbon source after then taking out carbonization；
S12. 3g carbon source is weighed, is uniformly mixed with the nitric acid that concentration is 3mol/L, mixed liquor is put into hydrothermal reaction kettle,
160 DEG C are heated to, 4 hours are reacted.To after reaction, be cooled to room temperature, then successively it is centrifuged, is dialysed, is done
After dry processing, nitrogen-doped carbon quantum dot is obtained.
Embodiment 2
The embodiment of the invention provides a kind of preparation methods of nitrogen-doped carbon quantum dot, comprising the following steps:
S21. the hair come will be collected and be used as carbon source, it is once purged, it is put into tube furnace, annealing is 1 small under the conditions of 800 DEG C
When, the carbon source after then taking out carbonization；
S22. 8g carbon source is weighed, is uniformly mixed with the nitric acid that concentration is 6mol/L, mixed liquor is then put into hydro-thermal reaction
In kettle, 200 DEG C are heated to, reacts 8 hours.To after reaction, be cooled to room temperature, then successively it is centrifuged, thoroughly
After being dried, the carbon quantum dot of N doping is can be obtained in analysis.
Embodiment 3
The embodiment of the invention provides a kind of preparation methods of nitrogen-doped carbon quantum dot, comprising the following steps:
S31. the hair come will be collected and be used as carbon source, it is once purged, it is put into tube furnace, annealing is 2 small under the conditions of 700 DEG C
When, the carbon source after then taking out carbonization；
S32. 5g carbon source is weighed, is uniformly mixed with the nitric acid that concentration is 4.5mol/L, it is anti-that mixed liquor is then put into hydro-thermal
It answers in kettle, is heated to 180 DEG C, react 6 hours.To after reaction, be cooled to room temperature, be then successively centrifuged,
After being dried, the carbon quantum dot of N doping is can be obtained in dialysis.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of preparation method of nitrogen-doped carbon quantum dot, which comprises the following steps:
Hair and/or hair are provided as carbon matrix precursor, the carbon matrix precursor is subjected to carbonization treatment in inert environments, is obtained
Carbon source；
The carbon source is mixed with nitric acid, nitrogen-doped carbon quantum dot is prepared through hydro-thermal reaction.
2. the preparation method of nitrogen-doped carbon quantum dot as described in claim 1, which is characterized in that the temperature of the hydro-thermal reaction
It is 150-200 DEG C, the reaction time is 4-8 hours.
3. the preparation method of nitrogen-doped carbon quantum dot as described in claim 1, which is characterized in that the concentration of the nitric acid is 2-
6mol/L。
4. the preparation method of nitrogen-doped carbon quantum dot as claimed in claim 3, which is characterized in that mix the carbon source with nitric acid
In the step of conjunction, the carbon source and the nitric acid are mixed according to mass volume ratio for the ratio of 1g:(1-3) ml.
5. the preparation method of nitrogen-doped carbon quantum dot according to any one of claims 1-4, which is characterized in that at the carbonization
The temperature of reason is 600-800 DEG C, and the time is 1-3 hours.
6. the preparation method of nitrogen-doped carbon quantum dot as claimed in claim 5, which is characterized in that the carbon content of the carbon source is high
In 90%.
7. as claim seeks the preparation method of the described in any item nitrogen-doped carbon quantum dots of 1-4, which is characterized in that by the carbon
It further include that the carbon source is subjected to cleaning treatment before presoma carries out carbonization treatment.
8. the preparation method of the nitrogen-doped carbon quantum dot as described in claim asks 7, which is characterized in that carry out the carbon source clear
The method of clean processing are as follows: successively use dish washing liquid, acetone, alcohol, ultrapure water to clean in the hair provided and/or hair.
9. as claim seeks the preparation method of the described in any item nitrogen-doped carbon quantum dots of 1-4, which is characterized in that will be through hydro-thermal
After mixed system cooling after reaction, successively it is centrifuged, is dialysed, is dried, collect nitrogen-doped carbon quantum dot.
10. a kind of nitrogen-doped carbon quantum dot, which is characterized in that the nitrogen-doped carbon quantum dot is any described by claim 1-9
Method prepares.
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| CN113089015A (en) * | 2021-03-29 | 2021-07-09 | 西北大学 | Nitrogen-doped carbon quantum dot and preparation method thereof, reduced graphene oxide and preparation method and application thereof |
| CN115043393A (en) * | 2022-07-15 | 2022-09-13 | 武汉纺织大学 | Ultralong phosphorescent keratin derived carbon quantum dot and preparation method thereof |
| CN117187617A (en) * | 2023-09-21 | 2023-12-08 | 上海理工大学 | High-heat-conductivity composite material and preparation method thereof |
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Application publication date: 20190702 |