CN105419794A - Orange light emitting carbon nano dot, preparation method and applications thereof - Google Patents
Orange light emitting carbon nano dot, preparation method and applications thereof Download PDFInfo
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Abstract
The invention provides an orange light emitting carbon nano dot, which comprises a nitrogen-enriched carbon based core and a cation passivation layer that wraps the surface of the nitrogen-enriched carbon based core. The provided orange light emitting carbon nano dot has a specific core-shell structure, which improves the light emitting efficiency of the orange light emitting carbon nano dot in the wave band of orange light. The provided orange light emitting carbon nano dot can be used to prepare fluorescent ink, fluorescence powder, and light emitting diode (LED) giving off white light. The fluorescent ink and fluorescence powder prepared from the orange light emitting carbon nano dot both have high fluorescence radiation quantum efficiency. The fluorescence powder can be used to prepare LED giving off white light and the LED can be applied to illumination equipment.
Description
Technical field
The invention belongs to carbon nano dot technical field, be specifically related to a kind of orange light emission carbon nano dot and its preparation method and application.
Background technology
Carbon nano dot (Carbondots, CDs) be a kind of carbon nanomaterial that can be luminous, compare with organic dye with semiconductor-quantum-point, have fluorescent stability good, without optical flare, good biocompatibility, low toxin, have broad application prospects in fields such as biomolecular labeling, living imaging, sensing, photoelectricity.
At present, carbon nano dot has realized the High Efficiency Luminescence at blue light and green light band, and fluorescence quantum efficiency reaches more than 50%.But carbon nano dot is in long-wave band, and particularly the luminous efficiency of orange optical band is still very low.Major cause lacks the carbon nano dot that effective fixture has orange optical band High Efficiency Luminescence, hinders development and the Application Areas of carbon nano dot greatly.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of orange light emission carbon nano dot and its preparation method and application, and orange light emission carbon nano dot provided by the invention has efficient orange light emission.
The invention provides a kind of orange light emission carbon nano dot, comprise rich nitrogen carbon back kernel and the positively charged ion passivation layer being coated on described rich nitrogen carbon back core surface.
Preferably, the positively charged ion in described positively charged ion passivation layer is one or more in sodium ion, potassium ion and lithium ion.
Preferably, described rich nitrogen carbon back kernel is prepared as follows:
Urea and multi-carboxy compound are dissolved in high boiling organic solvent, reacting by heating under airtight condition, obtain rich nitrogen carbon back kernel.
Present invention also offers a kind of preparation method of orange light emission carbon nano dot, comprise the following steps:
Urea and multi-carboxy compound are dissolved in high boiling organic solvent, reacting by heating under airtight condition, obtain rich nitrogen carbon back kernel;
Described rich nitrogen carbon back kernel is scattered in basic solution and processes, obtain orange light emission carbon nano dot.
Preferably, described high boiling organic solvent is selected from N, N '-dimethyl methane amide, N, one or more in N '-dimethyl ethanamide and dimethyl sulfoxide (DMSO).
Preferably, described multi-carboxy compound is selected from one or more in citric acid, oxalic acid and tartrate.
Preferably, the mass ratio of described urea and multi-carboxy compound is (0.1 ~ 4): 1.
Preferably, described basic solution is aqueous sodium hydroxide solution, potassium hydroxide aqueous solution or lithium hydroxide aqueous solution.
Present invention also offers a kind of fluorescent ink, comprise organic solvent and be scattered in the orange light emission carbon nano dot in water or organic solvent;
Described orange light emission carbon nano dot is selected from the orange light emission carbon nano dot that above-mentioned orange light emission carbon nano dot or above-mentioned preparation method prepare.
Present invention also offers a kind of orange light emission carbon nanodot fluorescence powder, comprise biological products powder and orange light emission carbon nano dot;
Described orange light emission carbon nano dot is selected from the orange light emission carbon nano dot that above-mentioned orange light emission carbon nano dot or above-mentioned preparation method prepare.
Compared with prior art, the invention provides a kind of orange light emission carbon nano dot, comprise rich nitrogen carbon back kernel and the positively charged ion passivation layer being coated on described rich nitrogen carbon back core surface.Orange light emission carbon nano dot provided by the invention has specific nucleocapsid structure, and described orange light emission carbon nano dot is improved in the luminous efficiency of orange optical band.In addition, orange light emission carbon nano dot provided by the invention may be used for the photodiode preparing fluorescent ink, fluorescent material and white light emission.Wherein, the present invention passes through with orange light emission carbon nano dot for raw material, and the fluorescent ink prepared and fluorescent material have high fluorescence radiation quantum yield.Further, with above-mentioned fluorescent material for the photodiode of white light emission prepared by raw material, and be applied in set lights.
Result shows, orange light emission carbon nano dot provided by the invention has efficient orange light emission, and the fluorescence quantum efficiency in ethanolic soln can reach 47%.Fluorescence quantum efficiency under efficient orange of the present invention photoemissive bio-based carbon nanodot fluorescence powder is solid-state can reach 21%.
Accompanying drawing explanation
Fig. 1 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 1;
Fig. 2 is the Fourier transform infrared spectroscopy figure of orange light emission carbon nano dot prepared by embodiment 1;
Fig. 3 is transmission electron microscope and the high resolution transmission electron microscopy photo of orange light emission carbon nano dot prepared by embodiment 1;
Fig. 4 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 2;
Fig. 5 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 3;
Fig. 6 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 4;
Fig. 7 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 5;
Fig. 8 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 6;
Fig. 9 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 7;
Figure 10 is the pattern that the orange light carbon nanodot fluorescence ink of embodiment 8 preparation is under ultraviolet light write;
Figure 11 is the photo of starch base orange light emission carbon nanodot fluorescence powder under ultraviolet lighting prepared by embodiment 10;
Figure 12 is the photo of the LED prepared based on starch base orange light emission carbon nanodot fluorescence powder prepared by embodiment 11.
Embodiment
The invention provides a kind of orange light emission carbon nano dot, comprise rich nitrogen carbon back kernel and the positively charged ion passivation layer being coated on described rich nitrogen carbon back core surface.
In described orange light emission carbon nano dot, interacted by chemical bond between carbon nitrogen and can form rich nitrogen carbon back kernel, and described rich nitrogen carbon back core surface is connected with carboxyl functional group.
Described orange light emission carbon nano dot also comprises one deck positively charged ion passivation layer being coated on described rich nitrogen carbon back core surface.
The kind of the present invention to described positively charged ion passivation layer cationic does not have particular restriction, is preferably one or more in sodium ion, potassium ion and lithium ion.
In the present invention, described rich nitrogen carbon back kernel is preferably prepared as follows:
Urea and multi-carboxy compound are dissolved in high boiling organic solvent, reacting by heating under airtight condition, obtain rich nitrogen carbon back kernel.
First urea and multi-carboxy compound are dissolved in high boiling organic solvent by the present invention.In the present invention, described multi-carboxy compound is preferably citric acid.Described high boiling organic solvent is preferably N, N '-dimethyl methane amide (DMF), N, one or more in N '-dimethyl ethanamide (DMAC) and dimethyl sulfoxide (DMSO) (DMSO).
Wherein, the source of the present invention to described urea, multi-carboxy compound and high boiling organic solvent does not have particular restriction, generally commercially available.
In the present invention, the mass ratio (0.1 ~ 4) of described urea and multi-carboxy compound: 1, is preferably (0.5 ~ 3): 1.In some embodiments of the invention, the mass ratio of described urea and multi-carboxy compound is 2:1.
The total mass of described urea and multi-carboxy compound and the volume ratio of high boiling organic solvent are (2 ~ 7) g:(5 ~ 30) ml, be preferably (3 ~ 5) g:(10 ~ 20) ml.In some embodiments of the invention, the total mass of described urea and multi-carboxy compound and the volume ratio of high boiling organic solvent are 3g:10ml, in other embodiments of the present invention, the total mass of described urea and multi-carboxy compound and the volume ratio of high boiling organic solvent are 4g:10ml.
The present invention obtains mixing solutions after urea and multi-carboxy compound are dissolved in high boiling organic solvent.Described mixing solutions is reacted in confined conditions.In the present invention, preferably described mixing solutions is placed in autoclave.The concrete kind of the present invention to described autoclave does not have particular restriction, for preparing the reaction conditions that carbon nano dot provides airtight, and can bear the reaction unit of certain high pressure.The present invention preferably adopts tetrafluoroethylene autoclave.
After described mixing solutions is placed in autoclave, closes autoclave, carry out reacting by heating.Wherein, the temperature of described reacting by heating is 160 ~ 200 DEG C, is preferably 170 ~ 190 DEG C.In embodiments more of the present invention, the temperature of described reacting by heating is 160 DEG C, and in other embodiments of the present invention, the temperature of described reacting by heating is 200 DEG C.The time of described reacting by heating is 4 ~ 24h, is preferably 5 ~ 20h.In embodiments more of the present invention, the time of described reacting by heating is 4h, and in other embodiments of the present invention, the time of described reacting by heating is 6h, and in other embodiments of the present invention, the time of described reacting by heating is 10h.
After heating terminates, obtain reaction solution.After described reaction solution rotary evaporation is removed solvent, through alcohol precipitation, obtain rich nitrogen carbon back kernel, described rich nitrogen carbon back core surface contains a large amount of carboxyl functional group.In the present invention, preferably adopt ethanol to carry out the operation of alcohol precipitation, the concrete grammar of the present invention to above-mentioned rotary evaporation, alcohol precipitation does not have particular restriction, well known to a person skilled in the art the method for rotary evaporation, alcohol precipitation.
Present invention also offers a kind of preparation method of orange light emission carbon nano dot, comprise the following steps:
Urea and multi-carboxy compound are dissolved in high boiling organic solvent, reacting by heating under airtight condition, obtain rich nitrogen carbon back kernel;
Described rich nitrogen carbon back kernel is scattered in basic solution and processes, obtain orange light emission carbon nano dot.
First urea and multi-carboxy compound are dissolved in high boiling organic solvent by the present invention.In the present invention, described multi-carboxy compound is preferably citric acid.Described high boiling organic solvent is preferably N, N '-dimethyl methane amide (DMF), N, one or more in N '-dimethyl ethanamide (DMAC) and dimethyl sulfoxide (DMSO) (DMSO).
Wherein, the source of the present invention to described urea, multi-carboxy compound and high boiling organic solvent does not have particular restriction, generally commercially available.
In the present invention, the mass ratio (0.1 ~ 4) of described urea and multi-carboxy compound: 1, is preferably (0.5 ~ 3): 1.In some embodiments of the invention, the mass ratio of described urea and multi-carboxy compound is 2:1.
The total mass of described urea and multi-carboxy compound and the volume ratio of high boiling organic solvent are (2 ~ 7) g:(5 ~ 30) ml, be preferably (3 ~ 5) g:(10 ~ 20) ml.In some embodiments of the invention, the total mass of described urea and multi-carboxy compound and the volume ratio of high boiling organic solvent are 3g:10ml, in other embodiments of the present invention, the total mass of described urea and multi-carboxy compound and the volume ratio of high boiling organic solvent are 4g:10ml.
The present invention obtains mixing solutions after urea and multi-carboxy compound are dissolved in high boiling organic solvent.Described mixing solutions is reacted in confined conditions.In the present invention, preferably described mixing solutions is placed in autoclave.The concrete kind of the present invention to described autoclave does not have particular restriction, for preparing the reaction conditions that carbon nano dot provides airtight, and can bear the reaction unit of certain high pressure.The present invention preferably adopts tetrafluoroethylene autoclave.
After described mixing solutions is placed in autoclave, closes autoclave, carry out reacting by heating.Wherein, the temperature of described reacting by heating is 160 ~ 200 DEG C, is preferably 170 ~ 190 DEG C.In embodiments more of the present invention, the temperature of described reacting by heating is 160 DEG C, and in other embodiments of the present invention, the temperature of described reacting by heating is 200 DEG C.The time of described reacting by heating is 4 ~ 24h, is preferably 5 ~ 20h.In embodiments more of the present invention, the time of described reacting by heating is 4h, and in other embodiments of the present invention, the time of described reacting by heating is 6h, and in other embodiments of the present invention, the time of described reacting by heating is 10h.
After heating terminates, obtain reaction solution.After described reaction solution rotary evaporation is removed solvent, through alcohol precipitation, obtain rich nitrogen carbon back kernel, described rich nitrogen carbon back core surface contains a large amount of carboxyl functional group.In the present invention, preferably adopt ethanol to carry out the operation of alcohol precipitation, the concrete grammar of the present invention to above-mentioned rotary evaporation, alcohol precipitation does not have particular restriction, well known to a person skilled in the art the method for rotary evaporation, alcohol precipitation.
After obtaining rich nitrogen carbon back kernel, described rich nitrogen carbon back kernel is scattered in basic solution and processes, obtain orange light emission carbon nano dot.
The kind of the present invention to described basic solution does not have particular restriction, is preferably aqueous sodium hydroxide solution, potassium hydroxide aqueous solution or lithium hydroxide aqueous solution.Wherein, the mass concentration of described basic solution is preferably 5wt% ~ 20wt%, is more preferably 10% ~ 15wt%.The mass volume ratio of described rich nitrogen carbon back kernel and described basic solution is (0.5 ~ 5) g:(5 ~ 30) ml), be more preferably (2 ~ 4) g:(10 ~ 15) and ml).
The present invention does not have particular restriction to the mode that described rich nitrogen carbon back kernel processes in basic solution, is preferably scattered in basic solvent by rich nitrogen carbon back kernel and stirs.
After described rich nitrogen carbon back kernel processes in basic solution, described rich nitrogen carbon back core surface carboxyl functional group is transformed into carboxylic acid ion, and then make this carbon nano dot surface form positively charged ion passivation layer, the time that described rich nitrogen carbon back kernel carries out processing in basic solution is preferably 0.1 ~ 5min, is more preferably 0.5 ~ 1min.
After basic solution process terminates, obtain reaction solution.Described reaction solution carries out centrifugal by the present invention, after solid-liquid separation, obtains solid matter.
The present invention does not have particular restriction to described centrifugal method, well known to a person skilled in the art centrifugal method.In the present invention, described centrifugal rotating speed is preferably 16000rmin
-1, the centrifugal time is preferably 10min.
The solid matter obtained is washed, dry, obtain orange light emission carbon nano dot.
Wherein, the method for the present invention to described washing does not have particular restriction, preferably carries out twice washing, carries out centrifugal after washing, after removing supernatant liquid, described lower floor solid matter is carried out drying.In the present invention, preferably freeze drying.The present invention does not have particular restriction to described cryodesiccated method, well known to a person skilled in the art cryodesiccated method.
Present invention also offers a kind of application of orange light emission carbon nano dot, the Application Areas of the present invention to described orange light emission carbon nano dot is not particularly limited, and the Application Areas of nano luminescent material of the prior art can realize.In the present invention, described orange light emission carbon nano dot can be used for preparing fluorescent ink and fluorescent material.
Concrete, the invention provides a kind of fluorescent ink, comprise solvent and be scattered in the orange light emission carbon nano dot in solvent.Wherein, described orange light emission carbon nano dot is orange light emission carbon nano dot described above.Described solvent is selected from water or organic solvent, and described organic solvent is preferably ethanol, DMF, dimethylsulfoxide or tetrahydrofuran (THF).
Present invention also offers a kind of preparation method of fluorescent ink, comprise the following steps:
Described orange light emission carbon nano dot is dissolved in solvent, obtains fluorescent ink.
In the present invention, described solvent is selected from water or organic solvent, and described organic solvent is preferably ethanol, DMF, dimethylsulfoxide or tetrahydrofuran (THF).The mass volume ratio of described orange light emission carbon nano dot and solvent is preferably (0.001 ~ 0.01) g:(5 ~ 50) ml), be more preferably (0.005 ~ 0.001) g:(20 ~ 30) and ml).
Fluorescent ink provided by the invention can be drawn on the substrate such as paper, plastics, after band solvent evaporates, under described substrate is placed in ultraviolet lamp, obtains fluorescent orange pattern.Therefore, described fluorescent ink can be applicable to the field such as anti-fake mark, indoor decoration.
Present invention also offers a kind of orange light emission carbon nanodot fluorescence powder, comprise biological products powder and orange light emission carbon nano dot; Wherein, described orange light emission carbon nano dot is orange light emission carbon nano dot described above.
The preferred of described biological products powder is starch, agar powder, paper pulp or cellulose powder, is more preferably starch.In the present invention, the mass ratio of described biological products powder and described orange light emission carbon nano dot is preferably (50 ~ 1000): 1, is more preferably (300 ~ 500): 1.
Present invention also offers a kind of preparation method of orange light emission carbon nanodot fluorescence powder, comprise the following steps:
By biological products powder and orange light emission carbon nano dot mixed dissolution in water, obtain mixing solutions;
Described mixing solutions is filtered, obtains solid matter;
Described solid matter is obtained orange light emission carbon nanodot fluorescence powder through lyophilize and grinding successively.
First biological products powder and orange light emission carbon nano dot are dissolved in the water mix and blend by the present invention, obtain mixing solutions, its objective is the biological products powder obtaining being adsorbed with orange light emission carbon nano dot.
After obtaining mixing solutions, described mixing solutions is filtered.Wherein, the method for the present invention to described filtration does not have particular restriction, can realize the carbon nano dot not being adsorbed onto biological products powder particle surface and the filter method of object of biological products powder separation being adsorbed with orange light emission carbon nano dot.
Undertaken obtaining orange light emission carbon nanodot fluorescence powder through lyophilize and grinding successively by filtering the solid matter obtained.The present invention does not have particular restriction to described cryodesiccated method, well known to a person skilled in the art freezing method.In the present invention, after grinding, the particle size range of the orange light emission carbon nanodot fluorescence powder obtained is 5 ~ 100 microns.
Present invention also offers a kind of photodiode of white light emission, concrete:
By the above-mentioned orange light emission carbon nanodot fluorescence powder for preparing and mixed with resin, obtain compo;
Described mixed slurry is coated on the LED surface of cold white light, obtains the photodiode that warm white is launched.
Fluorescent material prepared by the present invention has good fluorescence quantum efficiency, when being applied on photodiode, makes photodiode have good fluorescence quantum efficiency.
Orange light emission carbon nano dot provided by the invention has specific nucleocapsid structure, and described orange light emission carbon nano dot is improved in the luminous efficiency of orange optical band.In addition, orange light emission carbon nano dot provided by the invention may be used for the photodiode preparing fluorescent ink, fluorescent material and white light emission.Wherein, the present invention passes through with orange light emission carbon nano dot for raw material, and the fluorescent ink prepared and fluorescent material have high fluorescence radiation quantum yield.Further, with above-mentioned fluorescent material for the photodiode of white light emission prepared by raw material, and be applied in set lights.
Result shows, orange light emission carbon nano dot provided by the invention has efficient orange light emission, and the fluorescence quantum efficiency in ethanolic soln can reach 47%.Fluorescence quantum efficiency under efficient orange of the present invention photoemissive bio-based carbon nanodot fluorescence powder is solid-state can reach 21%.
In order to understand the present invention further, be described orange light emission carbon nano dot provided by the invention and its preparation method and application below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
(1) 2g urea and 1g citric acid are made into 10mL dimethyl formamide (DMF) solution, are placed in tetrafluoroethylene autoclave, react 4 hours at 160 DEG C.The solution of gained being removed most of DMF by rotary evaporation, adds a large amount of ethanol and be precipitated, is rich nitrogen carbon back kernel, the carbon nano dot of surface containing a large amount of carboxyl functional group.
(2) the carbon nano dot of (1) gained is dissolved in the 20mLNaOH aqueous solution (50mg/mL) solution stirring 1min, at 16000rmin
-1under speed, centrifugal 10min. centrifugal gained solid is through washing, centrifugal (16000rmin
-1, 10min) and twice, wash excessive alkali and salt impurity off, obtain orange light emission carbon nano dot-40 DEG C of lyophilizes.
Ultraviolet-ray visible absorbing and fluorescence emission spectrum analysis are carried out to carbon nano dot prepared by embodiment 1, result as shown in Figure 1, Fig. 1 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 1, in Fig. 1, the uv-visible absorption spectra figure of the orange light emission carbon nano dot that (a) is prepared for embodiment 1; The fluorescence emission spectrogram of b orange light emission carbon nano dot that () prepares for embodiment 1.As can be seen from Figure 1, carbon nano dot has emission peak in Cheng Guang district, and calculating fluorescence quantum efficiency is 47%.Described have efficient orange photoemissive carbon nano dot, and launch peak position 580nm, fluorescence quantum efficiency 47%, surperficial positively charged ion is Na+.
Carry out ftir analysis to carbon nano dot prepared by embodiment 1, as shown in Figure 2, Fig. 2 is the Fourier transform infrared spectroscopy figure of orange light emission carbon nano dot prepared by embodiment 1 to result.As shown in Figure 2, the charateristic avsorption band ν in Fig. 2
as(COO) (1580cm
-1) demonstrate the existence of carbon nano dot surface carbonyl salt groups.
Electronic microscope photos is carried out to carbon nano dot prepared by embodiment 1, the results are shown in Figure 3, Fig. 3 is transmission electron microscope and the high resolution transmission electron microscopy photo of orange light emission carbon nano dot prepared by embodiment 1, in Fig. 3, the transmission electron microscope photo of the orange light emission carbon nano dot that (a) is prepared for embodiment 1; The high resolution transmission electron microscopy photo of b orange light emission carbon nano dot that () prepares for embodiment 1.As seen in Figure 3, carbon nano-dot size at 4-10nm, and has good crystallinity.
Embodiment 2
(1) 4g urea and 1g citric acid are made into 10mL dimethyl formamide (DMF) solution, are placed in tetrafluoroethylene autoclave, react 10 hours at 160 DEG C.The solution of gained being removed most of DMF by rotary evaporation, adds a large amount of ethanol and be precipitated, is rich nitrogen carbon back kernel, the carbon nano dot of surface containing a large amount of carboxyl functional group.
(2) the carbon nano dot of (1) gained is dissolved in the 20mLNaOH aqueous solution (50mg/mL) solution stirring 1min, at 16000rmin
-1under speed, centrifugal 10min. centrifugal gained solid is through washing, centrifugal (16000rmin
-1, 10min) and twice, wash excessive alkali and salt impurity off, obtain orange light emission carbon nano dot-40 DEG C of freeze-drying.
Ultraviolet-ray visible absorbing and fluorescence emission spectrum analysis are carried out to carbon nano dot prepared by embodiment 2, result as shown in Figure 4, Fig. 4 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 2, in Fig. 4, the uv-visible absorption spectra figure of the orange light emission carbon nano dot that (a) is prepared for embodiment 2; The fluorescence emission spectrogram of b orange light emission carbon nano dot that () prepares for embodiment 2.As can be seen from Figure 4, carbon nano dot has emission peak in Cheng Guang district, and calculating fluorescence quantum efficiency is 42%.Described have efficient orange photoemissive carbon nano dot, and launch peak position 590nm, fluorescence quantum efficiency 42%, surperficial positively charged ion is Na
+.
Embodiment 3
(1) 2g urea and 1g citric acid are made into 10mL dimethyl formamide (DMF) solution, are placed in tetrafluoroethylene autoclave, react 4 hours at 160 DEG C.The solution of gained being removed most of DMF by rotary evaporation, adds a large amount of ethanol and be precipitated, is rich nitrogen carbon back kernel, the carbon nano dot of surface containing a large amount of carboxyl functional group.
(2) the carbon nano dot of (1) gained is dissolved in the 20mLKOH aqueous solution (50mg/mL) solution stirring 1min, at 16000rmin
-1under speed, centrifugal 10min. centrifugal gained solid is through washing, centrifugal (16000rmin
-1, 10min) and twice, wash excessive alkali and salt impurity off, obtain orange light emission carbon nano dot-40 DEG C of freeze-drying.
Ultraviolet-ray visible absorbing and fluorescence emission spectrum analysis are carried out to carbon nano dot prepared by embodiment 3, result as shown in Figure 5, Fig. 5 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 3, in Fig. 5, the uv-visible absorption spectra figure of the orange light emission carbon nano dot that (a) is prepared for embodiment 3; The fluorescence emission spectrogram of b orange light emission carbon nano dot that () prepares for embodiment 3.As can be seen from Figure 5, carbon nano dot has emission peak in Cheng Guang district, and calculating fluorescence quantum efficiency is 38%.Described have efficient orange photoemissive carbon nano dot, and launch peak position 580nm, fluorescence quantum efficiency 38%, surperficial positively charged ion is K
+.
Embodiment 4
(1) 2g urea and 1g citric acid are made into 10mL N,N-DIMETHYLACETAMIDE (DMAC) solution, are placed in tetrafluoroethylene autoclave, react 6 hours at 200 DEG C.The solution of gained being removed most of DMAC by rotary evaporation, adds a large amount of ethanol and be precipitated, is rich nitrogen carbon back kernel, the carbon nano dot of surface containing a large amount of carboxyl functional group.
(2) the carbon nano dot of (1) gained is dissolved in the 20mLKOH aqueous solution (50mg/mL) solution stirring 1min, at 16000rmin
-1under speed, centrifugal 10min. centrifugal gained solid is through washing, centrifugal (16000rmin
-1, 10min) and twice, wash excessive alkali and salt impurity off ,-40 DEG C of freeze-drying obtain orange light emission carbon nano dot.
Ultraviolet-ray visible absorbing and fluorescence emission spectrum analysis are carried out to carbon nano dot prepared by embodiment 4, result as shown in Figure 6, Fig. 6 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 4, in Fig. 6, the uv-visible absorption spectra figure of the orange light emission carbon nano dot that (a) is prepared for embodiment 4; The fluorescence emission spectrogram of b orange light emission carbon nano dot that () prepares for embodiment 4.As can be seen from Figure 6, carbon nano dot has emission peak in Cheng Guang district, and calculating fluorescence quantum efficiency is 40%.Described have efficient orange photoemissive carbon nano dot, and launch peak position 582nm, fluorescence quantum efficiency 40%, surperficial positively charged ion is Na
+.
Embodiment 5
(1) 2g urea and 1g citric acid are made into 10mL N,N-DIMETHYLACETAMIDE (DMF) solution, are placed in tetrafluoroethylene autoclave, react 6 hours at 200 DEG C.The solution of gained being removed most of DMF by rotary evaporation, adds a large amount of ethanol and be precipitated, is rich nitrogen carbon back kernel, the carbon nano dot of surface containing a large amount of carboxyl functional group.
(2) the carbon nano dot of (1) gained is dissolved in the 20mLLiOH aqueous solution (50mg/mL) solution stirring 1min, at 16000rmin
-1under speed, centrifugal 10min. centrifugal gained solid is through washing, centrifugal (16000rmin
-1, 10min) and twice, wash excessive alkali and salt impurity off ,-40 DEG C of freeze-drying obtain orange light emission carbon nano dot.
Ultraviolet-ray visible absorbing and fluorescence emission spectrum analysis are carried out to carbon nano dot prepared by embodiment 5, result as shown in Figure 7, Fig. 7 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 5, in Fig. 7, the uv-visible absorption spectra figure of the orange light emission carbon nano dot that (a) is prepared for embodiment 5; The fluorescence emission spectrogram of b orange light emission carbon nano dot that () prepares for embodiment 5.As can be seen from Figure 7, carbon nano dot has emission peak in Cheng Guang district, and calculating fluorescence quantum efficiency is 38%.Described have efficient orange photoemissive carbon nano dot, and launch peak position 577nm, fluorescence quantum efficiency 38%, surperficial positively charged ion is Li
+.
Embodiment 6
(1) 5g urea and 0.5g citric acid are made into 10mL N,N-DIMETHYLACETAMIDE (DMF) solution, are placed in tetrafluoroethylene autoclave, react 6 hours at 200 DEG C.The solution of gained being removed most of DMF by rotary evaporation, adds a large amount of ethanol and be precipitated, is rich nitrogen carbon back kernel, the carbon nano dot of surface containing a large amount of carboxyl functional group.
(2) the carbon nano dot of (1) gained is dissolved in the 20mLNaOH aqueous solution (50mg/mL) solution stirring 1min, at 16000rmin
-1under speed, centrifugal 10min. centrifugal gained solid is through washing, centrifugal (16000rmin
-1, 10min) and twice, wash excessive alkali and salt impurity off ,-40 DEG C of freeze-drying obtain orange light emission carbon nano dot.
Ultraviolet-ray visible absorbing and fluorescence emission spectrum analysis are carried out to carbon nano dot prepared by embodiment 6, result as shown in Figure 8, Fig. 8 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 6, in Fig. 8, the uv-visible absorption spectra figure of the orange light emission carbon nano dot that (a) is prepared for embodiment 6; The fluorescence emission spectrogram of b orange light emission carbon nano dot that () prepares for embodiment 6.As can be seen from Figure 8, carbon nano dot has emission peak in Cheng Guang district, and calculating fluorescence quantum efficiency is 32%.Described have efficient orange photoemissive carbon nano dot, and launch peak position 579nm, fluorescence quantum efficiency 32%, surperficial positively charged ion is Na
+.
Embodiment 7
(1) 2g urea and 1g citric acid are made into 10mL N,N-DIMETHYLACETAMIDE (DMF) solution, are placed in tetrafluoroethylene autoclave, react 6 hours at 200 DEG C.The solution of gained being removed most of DMF by rotary evaporation, adds a large amount of ethanol and be precipitated, is rich nitrogen carbon back kernel, the carbon nano dot of surface containing a large amount of carboxyl functional group.
(2) the carbon nano dot of (1) gained is dissolved in the 20mLNaOH aqueous solution (50mg/mL) solution stirring 1min, at 16000rmin
-1under speed, centrifugal 10min. centrifugal gained solid is through washing, centrifugal (16000rmin
-1, 10min) and twice, wash excessive alkali and salt impurity off ,-40 DEG C of freeze-drying obtain orange light emission carbon nano dot.
Ultraviolet-ray visible absorbing and fluorescence emission spectrum analysis are carried out to carbon nano dot prepared by embodiment 7, result as shown in Figure 9, Fig. 9 is ultraviolet-ray visible absorbing and the fluorescence emission spectrogram of orange light emission carbon nano dot prepared by embodiment 7, in Fig. 9, the uv-visible absorption spectra figure of the orange light emission carbon nano dot that (a) is prepared for embodiment 7; The fluorescence emission spectrogram of b orange light emission carbon nano dot that () prepares for embodiment 7.As can be seen from Figure 9, carbon nano dot has emission peak in Cheng Guang district, and calculating fluorescence quantum efficiency is 35%.Described have efficient orange photoemissive carbon nano dot, and launch peak position 582nm, fluorescence quantum efficiency 35%, surperficial positively charged ion is Na
+.
Embodiment 8
The preparation of orange light carbon nanodot fluorescence ink:
The carbon nano dot getting preparation in 10mg embodiment 1 is dissolved in 100ml deionized water, is configured to the fluorescent ink of orange light carbon nano dot, dips fluorescent ink with pen, blank sheet of paper is write and obtains red-purple writing, after water is dry, under blank sheet of paper is placed in ultraviolet lamp, obtain fluorescent orange writing.The results are shown in Figure 10, Figure 10 is the pattern that the orange light carbon nanodot fluorescence ink of embodiment 8 preparation is under ultraviolet light write.
Embodiment 9
The preparation of orange light carbon nanodot fluorescence ink:
Get the carbon nano dot described in 1mg embodiment 1 to be dissolved in 30ml ethanol, be configured to the fluorescent ink of orange light carbon nano dot, dip fluorescent ink with pen, blank sheet of paper is write and obtains red-purple writing, after ethanol is dry, under blank sheet of paper is placed in ultraviolet lamp, obtain fluorescent orange writing.
Embodiment 10
The preparation of the photoemissive bio-based carbon nanodot fluorescence powder of orange:
The carbon nano dot (10mg) embodiment 1 prepared and starch (1g) mixed dissolution are in 10ml water, and Keep agitation 1min, by obtained mixed reaction solution after filtration, to separate the carbon nano dot not being adsorbed onto starch particle surface, by obtained permeate after the freeze-drying of vacuum-freeze-dry machine, fully pulverize, obtain the efficient orange photoemissive bio-based carbon nanodot fluorescence powder that particle diameter is 10-40 micron, the fluorescence quantum efficiency of fluorescent material is 21%.The results are shown in Figure 11, Figure 11 is the photo of starch base orange light emission carbon nanodot fluorescence powder under ultraviolet lighting prepared by embodiment 10.
Embodiment 11
The photoemissive bio-based carbon nanodot fluorescence powder of orange prepares white LED lamp.
The preparation method of above-mentioned LED:
The fluorescent material prepare embodiment 11 and epoxy silicone resin (being purchased from the model that Dow Corning Corporation produces is the epoxy silicone resin of sylgard184) are applied in the LED of cold white light, wherein cold white LED lamp is existing patent of invention (CN104263364A), obtain the LED with warm white transmitting, chromaticity coordinates is (0.41,0.45) and colour temperature is (3708K).Specifically see Figure 12, Figure 12 is the photo of the LED prepared based on starch base orange light emission carbon nanodot fluorescence powder prepared by embodiment 11.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. an orange light emission carbon nano dot, is characterized in that, comprises rich nitrogen carbon back kernel and the positively charged ion passivation layer being coated on described rich nitrogen carbon back core surface.
2. orange light emission carbon nano dot according to claim 1, is characterized in that, the positively charged ion in described positively charged ion passivation layer is one or more in sodium ion, potassium ion and lithium ion.
3. orange light emission carbon nano dot according to claim 1, is characterized in that, described rich nitrogen carbon back kernel is prepared as follows:
Urea and multi-carboxy compound are dissolved in high boiling organic solvent, reacting by heating under airtight condition, obtain rich nitrogen carbon back kernel.
4. a preparation method for orange light emission carbon nano dot, is characterized in that, comprise the following steps:
Urea and multi-carboxy compound are dissolved in high boiling organic solvent, reacting by heating under airtight condition, obtain rich nitrogen carbon back kernel;
Described rich nitrogen carbon back kernel is scattered in basic solution and processes, obtain orange light emission carbon nano dot.
5. preparation method according to claim 4, is characterized in that, described high boiling organic solvent is selected from N, N '-dimethyl methane amide, N, one or more in N '-dimethyl ethanamide and dimethyl sulfoxide (DMSO).
6. preparation method according to claim 4, is characterized in that, described multi-carboxy compound be selected from citric acid, oxalic acid and tartrate one or more.
7. preparation method according to claim 4, is characterized in that, the mass ratio of described urea and multi-carboxy compound is (0.1 ~ 4): 1.
8. preparation method according to claim 4, is characterized in that, described basic solution is aqueous sodium hydroxide solution, potassium hydroxide aqueous solution or lithium hydroxide aqueous solution.
9. a fluorescent ink, is characterized in that, comprises organic solvent and is scattered in the orange light emission carbon nano dot in water or organic solvent;
Described orange light emission carbon nano dot is selected from the orange light emission carbon nano dot that the orange light emission carbon nano dot described in claims 1 to 3 any one claim or the preparation method described in claim 4 ~ 8 any one claim prepare.
10. an orange light emission carbon nanodot fluorescence powder, is characterized in that, comprises biological products powder and orange light emission carbon nano dot;
Described orange light emission carbon nano dot is selected from the orange light emission carbon nano dot that the orange light emission carbon nano dot described in claims 1 to 3 any one claim or the preparation method described in claim 4 ~ 8 any one claim prepare.
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