CN105858638B - A kind of multi-functional carbon dots material and its preparation method and application - Google Patents
A kind of multi-functional carbon dots material and its preparation method and application Download PDFInfo
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- CN105858638B CN105858638B CN201610243556.2A CN201610243556A CN105858638B CN 105858638 B CN105858638 B CN 105858638B CN 201610243556 A CN201610243556 A CN 201610243556A CN 105858638 B CN105858638 B CN 105858638B
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The present invention provides a kind of multi-functional carbon dots materials and its preparation method and application.The preparation method includes the following steps：Dry soft-boiled eggs Huang is carbonized；The soft-boiled eggs Huang concentrated sulfuric acid after carbonization and the mixed liquor of concentrated nitric acid are cracked, oil bath reflux, centrifugal drying obtains carbon material crude product；Dry carbon material crude product is soluble in water, obtain the solution of the multi-functional carbon dots material after hydro-thermal reaction.The present invention provides the multi-functional carbon dots materials being prepared by above-mentioned preparation method.On the one hand above-mentioned multi-functional carbon dots material can be used as lithium or anode material of lithium-ion battery；On the other hand, which also has strong photoluminescent property, has potential application foreground in fields such as bio-imaging, FPD.
Description
Technical field
The present invention relates to a kind of carbon material and preparation method thereof more particularly to a kind of multi-functional carbon dots material and its preparation sides
Method belongs to carbon material and its preparing technical field.
Background technology
In recent years, carbon dots due to building-up process it is simple, it is of low cost, there is good water-soluble, biocompatibility and excellent
Different chemical stability etc. and cause people's extensive concern.It is latent that these excellent performances of carbon dots so that they have in many fields
It is applying, including as pharmaceutical carrier, realizing the fields such as cell imaging, photocatalytic water.However, the raw material of synthesis carbon dots are mostly to change
Reagent is learned, does not meet economic and environment-friendly green chemical concept；Also, most of carbon dots are difficult to preserve, can only be in a manner of solution
Storage.
In addition, also bringing new energy crisis while economy is rapidly developed in recent years, it is high to develop a kind of green
The energy storage device of effect is the key that solve the above problems.Lithium ion battery is high, environmental-friendly and recyclable by its energy density
Many advantages, such as use, receives researcher's favor, and is widely used in every field, such as mobile phone, computer portable power are set
The systems such as standby, electric vehicle and power transmission.So far, it is graphite to realize commercialized carbon negative pole material, but graphite
Theoretical capacity only has 372mAhg-1, it is therefore desirable to seek a kind of new carbon material improve the capacity of lithium (sodium) ion battery and
Cyclical stability, to meet the needs of current people are growing.
In view of the above problems, providing a kind of method for preparing multi-functional carbon dots material, such carbon dots material can not only be used
In the preparation of fluorescent carbon point, and can be used as lithium or anode material of lithium-ion battery.
Invention content
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of multi-functional carbon dots material, the carbon dots
The fluorescence quantum yield of material is high, and stability is good, can be used as fluorescent material；The carbon dots material is born as lithium or sodium-ion battery
Pole material has higher capacity and preferable cyclical stability.
In order to realize above-mentioned technical purpose, the present invention provides a kind of preparation method of multi-functional carbon dots material, the preparations
Method includes the following steps：
By dry soft-boiled eggs Huang carbonization 1h-5h；
The soft-boiled eggs Huang concentrated sulfuric acid after carbonization and the mixed liquor of concentrated nitric acid are cracked, the oil bath at 100 DEG C -120 DEG C
Flow back 12h-24h, and centrifugal drying obtains carbon material crude product；
Dry carbon material crude product is soluble in water, form a concentration of 25mgmL-1-60mg·mL-1Solution,
To get to the solution of multi-functional carbon dots material after 150 DEG C of -350 DEG C of hydro-thermal reaction 6h-24h.
In the preparation method of the multi-functional carbon dots material of the present invention, soft-boiled eggs Huang uses after smashing to pieces.
In the preparation method of the multi-functional carbon dots material of the present invention, carried out in tube furnace when being carbonized.
In the preparation method of the multi-functional carbon dots material of the present invention, it is preferable that the concentrated sulfuric acid of use and mixing for concentrated nitric acid
Closing liquid refers to the concentrated sulfuric acid with concentrated nitric acid with 1-5：The mixed solution that 1 volume ratio is prepared.
In the preparation method of the multi-functional carbon dots material of the present invention, it is preferable that the temperature of the carbonization is 300 DEG C.
The present invention also provides a kind of multi-functional carbon dots materials, which is by above-mentioned multifunctional C
What the preparation method of point material was prepared.
Multi-functional carbon dots material provided by the invention, it is preferable that the fluorescence quantum yield of the multi-functional carbon dots material is
15%-28%.
Multi-functional carbon dots material provided by the invention, the carbon dots solution obtained by the multi-functional carbon dots material is in refrigerator (0
DEG C -6 DEG C) it preserves and will not occur to sink poly- phenomenon to 6 months.
The above-mentioned multi-functional carbon dots material of the present invention can both be used as lithium or anode material of lithium-ion battery can also be used as
Fluorescence carbon material.
In the application of multi-functional carbon dots material provided by the invention, it is preferable that the multi-functional carbon dots material as lithium or
Anode material of lithium-ion battery using when be that the multi-functional carbon dots material is carbonized at 600 DEG C -800 DEG C after 1h-5h to use.
In the application of multi-functional carbon dots material provided by the invention, it is preferable that the multi-functional carbon dots material as lithium from
Sub- cell negative electrode material, in 100mAg-1The lower capacity after 100 cycles is maintained at 711mAhg-1；In 500mAg-1Under, the capacity after 500 cycles is maintained at 702.9mAhg-1。
In the application of multi-functional carbon dots material provided by the invention, it is preferable that the multi-functional carbon dots material as sodium from
Sub- cell negative electrode material, in 100mAg-1The lower capacity after 100 cycles is 150mAhg-1；In 500mAg-1Under,
Capacity after 500 cycles is 121mAhg-1。
In the application of multi-functional carbon dots material provided by the invention, it is preferable that the multi-functional carbon dots material is as fluorescence
Carbon material using when be to take supernatant liquor for use after the solution of the multi-functional carbon dots material is centrifuged.
In the application of multi-functional carbon dots material provided by the invention, which makes as fluorescence carbon material
Used time is supernatant liquor after the solution of the multi-functional carbon dots material is centrifuged as fluorescent carbon materials'use；The multi-functional carbon dots
Precipitation after the solution centrifugation of material is dissolved in water, forms a concentration of 80mgmL-1-120mg·mL-1Solution, 150 DEG C-
At 350 DEG C after hydro-thermal reaction 6h-24h, centrifuging and taking supernatant liquor obtains second of carbon dots material, so repeats, gained after centrifugation
Solution is respectively provided with very strong luminosity, and centrifuges gained and precipitate the luminous carbon dots material that can be recycled to prepare high quality
Material.
The above-mentioned multi-functional carbon dots material of the present invention, mainly utilizing in this protein macromolecule of yolk to be rich in has nitrogen member
Element directly forms the carbon dots material of the i.e. nitrogen atom doping of hetero atom in heat treatment process.And no matter N doping is for gained material
The photoluminescent property or lithium of material or the electrochemical properties of anode material of lithium-ion battery all have important influence.
The above-mentioned multi-functional carbon dots material of the present invention, presents its good cyclical stability and high rate performance so that its
Lithium or anode material of lithium-ion battery can be used as.In addition, the multi-functional carbon dots material also has stronger photoluminescent property (quantum
28%) yield reaches as high as, have potential application foreground in fields such as bio-imaging, FPD.
The multi-functional carbon dots material of the present invention can not only be used as the carbon source of carbon quantum dot but also lithium or sodium ion can be used as electric
Pond negative material uses.The fluorescence quantum yield of carbon quantum dot obtained using the multi-functional carbon dots material is high, and stability is good, can
Using as fluorescent material, and centrifuge gained precipitation and can recycle luminous carbon dots material to prepare high quality, biology into
The fields such as picture, FPD have potential application foreground；Have using lithium made from the multi-functional carbon dots material or sodium-ion battery
There are higher capacity and preferable cyclical stability so that it can as lithium or anode material of lithium-ion battery.
The preparation process of the multi-functional carbon dots material of the present invention is simple, and synthesis condition is mild, and manufacturing cost is low.
Description of the drawings
Fig. 1 is that the TEM of multi-functional carbon dots material made from embodiment 1 schemes；
Fig. 2 is fluorescent emission collection of illustrative plates of the multi-functional carbon dots material under different excitation wavelengths made from embodiment 1；
Fig. 3 is for multi-functional carbon dots material made from embodiment 1 as lithium ion battery in 100mAg-1Under current density
Cyclical stability and coulombic efficiency collection of illustrative plates；
Fig. 4 is for multi-functional carbon dots material made from embodiment 1 as lithium ion battery in 500mAg-1Under current density
Cyclical stability and coulombic efficiency collection of illustrative plates；
Fig. 5 is for multi-functional carbon dots material made from embodiment 1 as sodium-ion battery in 100mAg-1Under current density
Cyclical stability and coulombic efficiency collection of illustrative plates；
Fig. 6 is for multi-functional carbon dots material made from embodiment 1 as sodium-ion battery in 500mAg-1Under current density
Cyclical stability and coulombic efficiency collection of illustrative plates.
Specific embodiment
In order to which technical characteristic, purpose and the advantageous effect to the present invention are more clearly understood, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that the present invention can practical range restriction.
Embodiment 1
A kind of multi-functional carbon dots material is present embodiments provided, through the following steps that be prepared：
The yolk of cooked egg is smashed to pieces and is placed in beaker, it is dry, dried yolk is placed in tube furnace carbon at 300 DEG C
Change 2 hours；
The yolk of carbonization is placed in beaker, (volume ratio 3 is cracked with the mixed liquor of the concentrated sulfuric acid and concentrated nitric acid:1) it is, oily
Bath reflux, reflux finish, and centrifugation distillation water washing is dried to obtain carbon material；
Carbon material will be dried to obtain to be dissolved in the distilled water of 160mL, mixed to uniformly, hydro-thermal reaction 12 at 300 DEG C
Hour obtains the solution of multi-functional carbon dots material.
The solution of multi-functional carbon dots material is centrifuged, the supernatant being obtained by filtration is the carbon dots solution with photoluminescent property
(CD-1), fluorescence quantum efficiency 28%.
As can be seen from Figure 1 the grain size of the above-mentioned carbon dots with photoluminescent property is about 3nm.
Fig. 2 is the fluorescent emission collection of illustrative plates of the multi-functional carbon dots material under different excitation wavelengths of the present embodiment, can be with from Fig. 2
See the multi-functional carbon dots material of the present embodiment solution have apparent excitation wavelength dependence, with excitation wavelength from
350nm increases to 470nm, and fluorescence emission peak has been moved to 510nm from 452nm is red, and this feature causes carbon dots in bio-imaging, puts down
Plate shows etc. that there are potential applications in fields.
The preparation of lithium or Carbon negative electrode material of sodium ion battery：The solution removal of obtained multi-functional carbon dots material is molten
Agent, with borax (mass ratio 1:3) grinding is uniform, the high temperature cabonization 2h at 700 DEG C in tube furnace.Then 1molL is used-1Hydrochloric acid
Washing, centrifugal drying obtain carbon material (CD-2) and are used to prepare ion battery.
The preparation of lithium ion battery：By carbon material (CD-2) (80wt%), acetylene black (10wt%), polyvinylidene fluoride
(10wt%) is mixed, and the NMP for adding in 15 μ L forms the mixed liquor of glutinous pulpous state, is uniformly coated on copper sheet, is dried in vacuo at 60 DEG C
24h.Pour lithium slice is used as to electrode, and diethyl carbonate (DEC)-ethylene carbonate ester (EC) is as electrolyte, then in glove box
Middle assembling button cell.
The preparation of sodium-ion battery：By carbon material (CD-2) (80wt%), acetylene black (10wt%), polyvinylidene fluoride
(10wt%) is mixed, and the NMP for adding in 15 μ L forms the mixed liquor of glutinous pulpous state, is uniformly coated on copper sheet, is dried in vacuo at 120 DEG C
24h.Pure sodium piece is used as to electrode, and diethyl carbonate (DEC)-ethylene carbonate ester (EC) is as electrolyte, then in glove box
Middle assembling button cell.
Fig. 3 is lithium ion battery made from the present embodiment in 100mAg-1Current density under the lithium ion battery that measures
Cyclical stability and coulombic efficiency collection of illustrative plates, from collection of illustrative plates it can be seen that the battery have good cyclical stability, by 100 times
It is still 711mAhg to recycle later capacity-1。
Fig. 4 is lithium ion battery made from the present embodiment in 500mAg-1Current density under the lithium ion battery that measures
Cyclical stability and coulombic efficiency collection of illustrative plates, from collection of illustrative plates it can be seen that the battery under high magnification have good cyclical stability
Higher coulombic efficiency, the capacity after 500 cycles are still 702.9mAhg-1.Fig. 4 illustrates that the present embodiment obtains
Multi-functional carbon dots material high rate performance especially high rate capability it is good, this for its practical application be significantly,
It can greatly shorten the time used in material charging.
Fig. 5 is sodium-ion battery made from the present embodiment in 100mAg-1Current density under the sodium-ion battery that measures
Cyclical stability and coulombic efficiency collection of illustrative plates, from collection of illustrative plates it can be seen that the battery have good cyclical stability, by 300
It is still 150mAhg to recycle later capacity-1。
Fig. 6 is sodium-ion battery made from the present embodiment in 500mAg-1Current density under the sodium-ion battery that measures
Cyclical stability and coulombic efficiency collection of illustrative plates, from collection of illustrative plates it can be seen that the battery under high magnification have good cyclical stability
Higher coulombic efficiency, the charge specific capacity after 500 cycles are still 121mAhg-1。
Embodiment 2
A kind of multi-functional carbon dots material is present embodiments provided, through the following steps that be prepared：
The preparation of carbon material is the same as embodiment 1；
Carbon material will be dried to obtain to be dissolved in the distilled water of 160mL, mix to uniformly, solution is then divided into four
Part, hydro-thermal reaction 12 hours at 185 DEG C, 200 DEG C, 250 DEG C, 300 DEG C, take supernatant liquor to obtain four kinds of carbon dots respectively after centrifugation
Material is respectively CD-3, CD-4, CD-5, CD-6, and fluorescence quantum yield is respectively 17.29%, 21.75%, 24.53%,
28.36%.
Embodiment 3
A kind of multi-functional carbon dots material is present embodiments provided, through the following steps that be prepared：
The preparation of carbon material is the same as embodiment 1；
Carbon material will be dried to obtain to be dissolved in the distilled water of 160mL, mixed to uniformly, then solution is divided into four parts,
Hydro-thermal reaction 6h, 12h, 18h at 200 DEG C respectively, it is respectively CD- that supernatant liquor is taken to obtain four kinds of carbon dots materials for 24 hours, after centrifugation
7, CD-8, CD-9, CD-10, fluorescence quantum yield are respectively 18.19%, 18.99%, 21.97%, 22.00%.
Embodiment 4
A kind of multi-functional carbon dots material is present embodiments provided, through the following steps that be prepared：
The preparation of carbon material is the same as embodiment 1；
Carbon material will be dried to obtain to be dissolved in the distilled water of 50mL, mixed to uniformly, then solution water at 300 DEG C
The carbon material being obtained by filtration is continued to be dissolved in the distilled water of 50mL, be mixed to by thermal response 12h, centrifuging and taking supernatant liquor
Uniformly, then solution hydro-thermal reaction 12h at 300 DEG C, second of carbon dots material that centrifuging and taking supernatant liquor obtains are CD-11；
Precipitation is dissolved in the distilled water of 50mL again, is mixed to uniformly, then solution hydro-thermal reaction at 300 DEG C
12h, centrifuging and taking supernatant liquor obtain carbon dots material C D-12；Precipitation is dissolved in the distilled water of 50mL again, is mixed to
Even, then solution hydro-thermal reaction 12h at 300 DEG C, centrifuging and taking supernatant liquor obtain carbon dots material C D-13；Precipitation is dissolved in again
In the distilled water of 50mL, mix to uniformly, then solution hydro-thermal reaction 12h at 300 DEG C, centrifuging and taking supernatant liquor obtain
Carbon dots material C D-14；Precipitation is dissolved in the distilled water of 50mL again, is mixed to uniformly, then solution hydro-thermal at 300 DEG C
12h is reacted, centrifuging and taking supernatant liquor obtains carbon dots material C D-15；The fluorescence quantum yield of five kinds of carbon dots materials is respectively
20.46%, 25.06%, 26.42%, 18.98%, 20.82%.
Above example illustrates that multi-functional carbon dots material provided by the invention has dual application value, the carbon dots material
The fluorescence quantum yield of material is high, and stability is good, can be used as fluorescent material；It, can be with the cyclical stability that high power capacity is become reconciled
As lithium or anode material of lithium-ion battery.
Claims (9)
1. a kind of preparation method of multi-functional carbon dots material, which is characterized in that the preparation method includes the following steps：
By dry soft-boiled eggs Huang carbonization 1h-5h；
The soft-boiled eggs Huang concentrated sulfuric acid after carbonization and the mixed liquor of concentrated nitric acid are cracked, the oil bath reflux at 100 DEG C -120 DEG C
12h-24h, centrifugal drying obtain carbon material crude product；
Dry carbon material crude product is soluble in water, form a concentration of 25mgmL-1-60mg·mL-1Solution, 150 DEG C-
At 350 DEG C after hydro-thermal reaction 6h-24h, the solution of the multi-functional carbon dots material is obtained.
2. the preparation method of multi-functional carbon dots material according to claim 1, which is characterized in that the concentrated sulfuric acid and dense nitre
The mixed liquor of acid refers to the mixed solution that the concentrated sulfuric acid is prepared with concentrated nitric acid with 1-5: 1 volume ratio.
3. the preparation method of multi-functional carbon dots material according to claim 1, which is characterized in that the temperature of the carbonization is
300℃。
4. a kind of multi-functional carbon dots material, which is characterized in that the multi-functional carbon dots material is by any one of claim 1-3 institutes
What the preparation method of multi-functional carbon dots material stated was prepared；The fluorescence quantum yield of the multi-functional carbon dots material is 15%-
28%.
5. the application of the multi-functional carbon dots material described in claim 4, which is characterized in that the multi-functional carbon dots material as lithium or
Anode material of lithium-ion battery and fluorescence carbon material.
6. the application of multi-functional carbon dots material according to claim 5, which is characterized in that the multi-functional carbon dots material conduct
Lithium or anode material of lithium-ion battery using when be that the multi-functional carbon dots material is carbonized at 600 DEG C -800 DEG C after 1h-5h to make
With.
7. the application of multi-functional carbon dots material according to claim 5 or 6, which is characterized in that the multi-functional carbon dots material
As lithium ion battery negative material, in 100mAg-1Under, the capacity after 100 cycles is maintained at 711mAhg-1；
In 500mAg-1Under, the capacity after 500 cycles is maintained at 702.9mAhg-1。
8. the application of multi-functional carbon dots material according to claim 5 or 6, which is characterized in that the multi-functional carbon dots material
As anode material of lithium-ion battery, in 100mAg-1Under, the capacity after 100 cycles is 150mAhg-1；
500mA·g-1Under, the capacity after 500 cycles is 121mAhg-1。
9. the application of multi-functional carbon dots material according to claim 5, which is characterized in that the multi-functional carbon dots material conduct
It is to take supernatant liquor for use after the solution of the multi-functional carbon dots material is centrifuged during fluorescent carbon materials'use.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101973541A (en) * | 2010-10-11 | 2011-02-16 | 福州大学 | Method for extracting carbon quantum dots from activated carbon |
| CN103588189A (en) * | 2013-07-04 | 2014-02-19 | 上海交通大学 | Egg-based method for realizing hydrothermal synthesis of carbon quantum dots |
| WO2014193089A1 (en) * | 2013-05-30 | 2014-12-04 | 부경대학교 산학협력단 | Method for preparation of carbon quantum dots |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973541A (en) * | 2010-10-11 | 2011-02-16 | 福州大学 | Method for extracting carbon quantum dots from activated carbon |
| WO2014193089A1 (en) * | 2013-05-30 | 2014-12-04 | 부경대학교 산학협력단 | Method for preparation of carbon quantum dots |
| CN103588189A (en) * | 2013-07-04 | 2014-02-19 | 上海交通大学 | Egg-based method for realizing hydrothermal synthesis of carbon quantum dots |
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