CN108179009A - A kind of europium ion-doped carbon quantum dot and preparation method thereof - Google Patents
A kind of europium ion-doped carbon quantum dot and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of europium ion-doped carbon quantum dot and preparation method thereof, the carbon quantum dot is using citric acid as presoma carbon source, and europium ion-doped ion concentration is 0.5~5%, and pattern is spherical, a diameter of 1~10nm.Preparation method includes the following steps：It weighs citric acid to be placed in beaker, adds in water and be stirred to dissolve to obtain citric acid solution；It weighs rare-earth oxidation europium, instills concentrated nitric acid, treat rare earth oxide the reaction was complete rare earth nitrate solution；Citric acid solution and rare earth europium nitrate solution are mixed, stir the hydro-thermal reaction that 2~15h is then carried out under the conditions of 100~240 DEG C, obtained yellow transparent liquid is europium ion-doped citric acid carbon quantum dot.The present invention has the advantages that high synthetic product purity, product photism and has good stability, carbon quantum dot Color tunable, overcome conventional carbon quantum dot light emitting unicity, it is moved so that shining to red light region, in the fields such as optical device and biomedicine, application prospect is good.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of europium ion-doped carbon quantum dot and its preparation side
Method.
Background technology
A kind of Novel Carbon Nanomaterials that carbon quantum dot (CDs) is got up as this new development in several years, not only with carbon skeleton
Peculiar property, also have characteristic more more superior than traditional quantum dot.With the fluorescence similar with conventional metals quantum dot
Outside performance, also with molecular weight and grain size are small, fluorescent stability is high, without optical flare, exciting light spectrum width and continuous, launch wavelength can
The advantages that tuning, good biocompatibility, hypotoxicity.In addition to this, also because of the quantum limitation effect of carbon quantum dot and boundary effect
And show many special properties, it is considered to be a kind of that traditional quantum point is replaced to carry out screen display, biomarker and fluorescence
The ideal material of the research such as imaging.
But the fluorescence quantum yield of carbon quantum dot prepared at present, fluorescence intensity cannot reach conventional metals quantum dot
Level, the application in the fields such as LED display technique and biomedicine is also immature, therefore, to high quantum production rate and shine
The preparation of the carbon quantum dot of intensity and the exploration of method seem and its important.Research finds that carbon quantum dot prepared by oxidizing process contains
The defects of a large amount of, the functional groups such as the carboxyl contained in addition to surface, hydroxyl, internal also there are a series of scission of links.If to carbon quantum dot
The structure that carbon quantum dot can not only be changed by carrying out a degree of modification can also enhance its quantum yield and photoluminescent property.In order to
The advantage of carbon dots in itself is not influenced, and doping method is the method for modifying carbon dots overriding concern.
2014, Hailong Dong etc. were in Polyol-mediated C-dot formation showing
efficient Tb3+/Eu3+In mono- texts of emission on the basis of carbon quantum dot doping metals zinc, magnesium metal, greatly improve
The fluorescence intensity and fluorescence quantum yield of carbon quantum dot.On the basis of alkali metal, Hailong Dong et al. are again in carbon
Using polyethylene glycol as carbon source on the basis of quantum dot, it is doped with rare-earth europium, rare earth terbium is prepared for rear-earth-doped carbon quantum dot, carbon
The energy transfer to rare earth ion is shown inside quantum dot.But due to the combination of polyethylene glycol and rare earth ion in this method
Weaker, therefore, it is difficult to ensure that rare earth ion is uniformly dispersed in carbon quantum dot.
2012, Yongqiang Dong et al. were carbon source using citric acid, were successfully prepared using pyrolysismethod with relatively strong
The carbon quantum dot of blue emission, citric acid are easy to chelated metal ions as a kind of organic acid, have it is at low cost, it is soluble easily in water
Etc. advantages, in addition to this, for this report using high temperature pyrolytic cracking (HTP), the pattern and Properties Control of carbon quantum dot are more difficult.
Invention content
The technical problems to be solved by the invention are：There is the monistic deficiency that shines in traditional carbon quantum dot, the present invention carries
A kind of europium ion-doped carbon quantum dot to solve the above problems and preparation method thereof has been supplied, there is synthetic product purity height, product
It photism and has good stability, carbon quantum dot Color tunable, preparation process is simple, synthesis condition is mild, the advantages such as at low cost.Europium
The successful preparation of the citric acid carbon quantum dot of ion doping overcomes conventional carbon quantum dot light emitting unicity so that shine to red
Light region is moved, and in the fields such as optical device and biomedicine, application prospect is good.
The present invention is achieved through the following technical solutions：
A kind of europium ion-doped carbon quantum dot, the carbon quantum dot using citric acid as presoma carbon source, it is europium ion-doped from
Son a concentration of 0.5~5%, pattern is spherical, a diameter of 1~10nm.
Preferably, under 393nm excitation wavelengths in 400-750nm sections all there is transmitting in the carbon quantum dot, wherein
The broad peak of 400-575nm belongs to the characteristic emission of carbon quantum dot, and wherein 597nm, 623, the narrow peak at 702nm belong to europium ion
Characteristic emission.
The method for preparing above-mentioned europium ion-doped carbon quantum dot, includes the following steps：
Step 1, the preparation of citric acid solution：It weighs citric acid to be placed in beaker, adds in water and be stirred to dissolve to obtain citric acid
Solution；
Step 2, the preparation of rare earth europium nitrate solution：Rare-earth oxidation europium is weighed, instills concentrated nitric acid, treats that rare earth oxide reacts
Rare earth nitrades europium solution is obtained completely；
Step 3, the preparation of europium ion-doped carbon quantum dot：Citric acid solution and step 2 prepared by step 1 prepares dilute
Native europium nitrate solution mixing, stirring and then the hydro-thermal reaction that 2~15h is carried out under the conditions of 100~240 DEG C, what is obtained is faint yellow
Transparency liquid is europium ion-doped carbon quantum dot.
Preferably, in the step 1, a concentration of 0.1~2mol/L of the citric acid solution of preparation.
Preferably, in the step 2, a concentration of 0.0044~0.176mol/ml of the rare earth europium nitrate solution of preparation.
Preferably, in the step 3, citric acid solution and rare earth europium nitrate solution are molten according to citric acid solute and europium nitrate
The molar ratio of matter is 20：1~200:1 mixing is stirred 10~20min and is reacted again after mixing.
Preferably, the temperature of the hydro-thermal reaction is 150~220 DEG C.
Preferably, the hydro-thermal reaction time is 3~8h.
The present invention has the advantage that and advantageous effect：
1st, the present invention uses citric acid rare-earth europium ion to be introduced with the mode of doping, using hydro-thermal method for presoma carbon source
Success prepares europium ion-doped carbon quantum dot.Citric acid can chelate europium ion, can be embedded in europium ion during carbonization
Carbon quantum dot skeleton by carbon quantum dot and the energy transmission of europium ion, obtains on the basis of pure carbon quantum dot blue emission
Characteristic emission with strong europium ion.By the introducing of citric acid huge legendary turtle and rare earth ion, changed inside carbon quantum dot after carbonization
Structure, and successfully combined using the excellent biocompatibility of carbon quantum dot and special optical property with rare earth ion, it realizes
The assembling of multi-functional compound carbon quantum dot can be imaged and sense in polychrome, the fields such as identification realize application；
2nd, the present invention has high synthetic product purity, product photism and has good stability, carbon quantum dot Color tunable, system
It is standby it is simple for process, synthesis condition is mild, the advantages such as at low cost.The successful preparation of europium ion-doped citric acid carbon quantum dot, gram
Conventional carbon quantum dot light emitting unicity is taken so that shine and moved to red light region, in the fields such as optical device and biomedicine
Application prospect is good.
Description of the drawings
Attached drawing described herein is used for providing further understanding the embodiment of the present invention, forms one of the application
Point, do not form the restriction to the embodiment of the present invention.In the accompanying drawings：
Fig. 1 is the TEM collection of illustrative plates of europium ion-doped citric acid carbon quantum dot prepared by the embodiment of the present invention 1；
Fig. 2 is the luorescence excitation spectrogram of europium ion-doped citric acid carbon quantum dot prepared by the embodiment of the present invention 1；
Fig. 3 is the fluorescent emission spectrogram of europium ion-doped citric acid carbon quantum dot prepared by the embodiment of the present invention 1；
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiment and attached drawing, to this
Invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining the present invention, do not make
For limitation of the invention.
Embodiment 1
Step 1, the preparation of citric acid solution：2.1g citric acid solid particles are weighed to be placed in beaker, add in 40ml go from
Sub- water is stirred to dissolve under normal temperature condition to get required citric acid solution；
Step 2, the preparation of europium nitrate solution：0.0352g (2%) rare-earth oxidation europium is weighed, concentrated nitric acid is instilled, treats rare earth oxygen
The reaction was complete for compound, obtains required europium nitrate solution；
Step 3, the preparation of europium ion-doped citric acid carbon quantum dot：Citric acid solution is mixed with europium nitrate solution,
10min is reacted under room temperature part, is then transferred to the hydro-thermal reaction for carrying out 3h in reaction kettle under the conditions of 200 DEG C, what is obtained is faint yellow
Transparency liquid is europium ion-doped citric acid carbon quantum dot.Its transmission electron microscope figure (TEM) is as shown in Figure 1, fluorescence swashs
Spectrogram shine as shown in Fig. 2, fluorescence emission spectrum is as shown in Figure 3.
Embodiment 2
Step 1, the preparation of citric acid solution：2.1g citric acid solid particles are weighed to be placed in beaker, add in 40ml go from
Sub- water is stirred to dissolve under normal temperature condition to get required citric acid solution；
Step 2, the preparation of europium nitrate solution：0.0088g (0.5%) rare-earth oxidation europium is weighed, instills concentrated nitric acid, it is to be oxidized
The reaction was complete for europium, obtains required europium nitrate solution；
Step 3, the preparation of europium ion-doped citric acid carbon quantum dot：Citric acid solution is mixed with europium nitrate solution,
10min is reacted under room temperature part, is then transferred to the hydro-thermal reaction for carrying out 6h in reaction kettle under the conditions of 150 DEG C, what is obtained is faint yellow
Transparency liquid is europium ion-doped citric acid carbon quantum dot.
Embodiment 3
Step 1, the preparation of citric acid solution：2.1g citric acid solid particles are weighed to be placed in beaker, add in 40ml go from
Sub- water is stirred to dissolve under normal temperature condition to get required citric acid solution；
Step 2, the preparation of europium nitrate solution：0.086g (5%) rare-earth oxidation europium is weighed, instills concentrated nitric acid, europium to be oxidized
The reaction was complete, obtains required europium nitrate solution；
Step 3, the preparation of europium ion-doped citric acid carbon quantum dot：Citric acid solution is mixed with europium nitrate solution,
10min is reacted under room temperature part, is then transferred to the hydro-thermal reaction for carrying out 2h in reaction kettle under the conditions of 240 DEG C, what is obtained is faint yellow
Transparency liquid is europium ion-doped citric acid carbon quantum dot.
Above-described specific embodiment has carried out the purpose of the present invention, technical solution and advantageous effect further
It is described in detail, it should be understood that the foregoing is merely the specific embodiment of the present invention, is not intended to limit the present invention
Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (8)
1. a kind of europium ion-doped carbon quantum dot, which is characterized in that the carbon quantum dot using citric acid as presoma carbon source, europium from
Sub- Doped ions a concentration of 0.5~5%, pattern is spherical, a diameter of 1~10nm.
2. a kind of europium ion-doped carbon quantum dot according to claim 1, which is characterized in that the carbon quantum dot exists
Under 393nm excitation wavelengths, all there is transmitting in 400-750nm sections, wherein the broad peak of 400-575nm belongs to the spy of carbon quantum dot
It levys and penetrates, wherein 597nm, 623, the narrow peak at 702nm belong to the characteristic emission of europium ion.
3. based on a kind of preparation method of europium ion-doped carbon quantum dot of claims 1 or 2 any one of them, feature exists
In including the following steps：
Step 1, the preparation of citric acid solution：It weighs citric acid to be placed in beaker, adds in water and be stirred to dissolve to obtain citric acid solution；
Step 2, the preparation of rare earth europium nitrate solution：Rare-earth oxidation europium is weighed, instills concentrated nitric acid, treating rare earth oxide, the reaction was complete
Obtain rare earth europium nitrate solution；
Step 3, the preparation of europium ion-doped carbon quantum dot：Rare earth nitre prepared by citric acid solution and step 2 prepared by step 1
Sour europium solution mixing, stirring and then the hydro-thermal reaction that 2~15h is carried out under the conditions of 100~240 DEG C, obtained pale yellow transparent
Liquid is europium ion-doped carbon quantum dot.
A kind of 4. preparation method of europium ion-doped carbon quantum dot according to claim 3, which is characterized in that the step
In 1, a concentration of 0.1~2mol/L of the citric acid solution of preparation.
A kind of 5. preparation method of europium ion-doped carbon quantum dot according to claim 3, which is characterized in that the step
In 2, a concentration of 0.0044~0.176mol/ml of the rare earth europium nitrate solution of preparation.
A kind of 6. preparation method of europium ion-doped carbon quantum dot according to claim 1, which is characterized in that the step
In 3, citric acid solution and rare earth europium nitrate solution are 20 according to the molar ratio of citric acid solute and europium nitrate solute：1~200:1
Mixing is stirred 10~20min and is reacted again after mixing.
A kind of 7. preparation method of europium ion-doped carbon quantum dot according to claim 3, which is characterized in that the hydro-thermal
The temperature of reaction is 150~220 DEG C.
A kind of 8. preparation method of europium ion-doped carbon quantum dot according to claim 3, which is characterized in that the hydro-thermal
Reaction time is 3~8h.
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Cited By (16)
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|---|---|---|---|---|
| CN108822840A (en) * | 2018-08-29 | 2018-11-16 | 济南大学 | A kind of fiber crops are the preparation method of carbon source neodymium doped carbon quantum dot composite material |
| CN109054829A (en) * | 2018-08-29 | 2018-12-21 | 济南大学 | A kind of palm bark is the preparation method of carbon source praseodymium doped carbon quantum dot composite material |
| CN109097034A (en) * | 2018-08-29 | 2018-12-28 | 济南大学 | It is a kind of using cotton stalk skins as the preparation method of carbon source La doped carbon quantum dot composite material |
| CN109181686A (en) * | 2018-07-12 | 2019-01-11 | 安徽师范大学 | Cerium dopping carbon dots and preparation method thereof and the application in catalyzing hydrolysis phosphate compounds |
| CN109181693A (en) * | 2018-08-29 | 2019-01-11 | 济南大学 | It is a kind of using luffa as the preparation method of carbon source Er ions carbon quantum dot composite material |
| CN109370576A (en) * | 2018-11-12 | 2019-02-22 | 许昌学院 | Chemical method for preparing carbon quantum dots |
| CN109852373A (en) * | 2019-01-07 | 2019-06-07 | 温州大学 | A kind of boric acid functional fluorescence nano material and the application for detecting glucose |
| CN112079892A (en) * | 2020-08-18 | 2020-12-15 | 华东理工大学 | Preparation method and application of carbon quantum dot doped rare earth ratio type fluorescent probe |
| CN112266391A (en) * | 2020-11-16 | 2021-01-26 | 华东理工大学 | Preparation method and application of rare earth porous fluorescent micro-grid material |
| CN112961669A (en) * | 2021-02-01 | 2021-06-15 | 苏州星烁纳米科技有限公司 | Preparation method of solid-phase carbon quantum dot, solid-phase carbon quantum dot prepared by same and light-emitting device |
| CN113834802A (en) * | 2021-09-18 | 2021-12-24 | 上海交通大学 | Preparation method and application of lanthanide metal-doped carbon quantum dot and lanthanide metal-doped carbon quantum dot-aptamer conjugate probe |
| CN113861971A (en) * | 2021-10-12 | 2021-12-31 | 青岛农业大学 | Rare earth element doped carbon quantum dot ratiometric fluorescent probe, and preparation method and application thereof |
| CN113884476A (en) * | 2021-10-12 | 2022-01-04 | 青岛农业大学 | Sensor for detecting aluminum ions and method for detecting aluminum ions by using sensor |
| CN113884475A (en) * | 2021-10-12 | 2022-01-04 | 青岛农业大学 | Tetracycline detection method based on europium-doped carbon quantum dot ratio fluorescent probe |
| CN116179198A (en) * | 2023-02-27 | 2023-05-30 | 河北大学 | Method for preparing solid rare earth doped fluorescent carbon dots by one-step hydrothermal method |
| CN116179197A (en) * | 2023-02-27 | 2023-05-30 | 河北大学 | Preparation of Eu by one-step hydrothermal method 3+ Method for doping fluorescent carbon dots |
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| CN109181686A (en) * | 2018-07-12 | 2019-01-11 | 安徽师范大学 | Cerium dopping carbon dots and preparation method thereof and the application in catalyzing hydrolysis phosphate compounds |
| CN109097034A (en) * | 2018-08-29 | 2018-12-28 | 济南大学 | It is a kind of using cotton stalk skins as the preparation method of carbon source La doped carbon quantum dot composite material |
| CN109181693A (en) * | 2018-08-29 | 2019-01-11 | 济南大学 | It is a kind of using luffa as the preparation method of carbon source Er ions carbon quantum dot composite material |
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| CN116179198B (en) * | 2023-02-27 | 2023-12-05 | 河北大学 | Method for preparing solid rare earth doped fluorescent carbon dots by one-step hydrothermal method |
| CN116179197B (en) * | 2023-02-27 | 2024-04-05 | 河北大学 | Preparation of Eu by one-step hydrothermal method 3+ Method for doping fluorescent carbon dots |
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