CN106497551A - Pure organic room temperature phosphorimetry material of a kind of high-performance and its preparation method and application - Google Patents
Pure organic room temperature phosphorimetry material of a kind of high-performance and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to luminescent material technical field, and in particular to pure organic room temperature phosphorimetry material of a kind of high-performance and its preparation method and application.The preparation method is comprised the following steps：S1, the carbon quantum dot that will be enriched in N element and O elements and carbamide are by 1:100～100000 quality agitated uniformly obtains reaction mixture than mixed dissolution in water；S2, step S1 gained reaction mixture is heated 1～10 hour at 100～200 DEG C, then sequentially pass through cooling and grind, obtained final product.The method of the invention, raw material pure organic, nontoxic, cheap, be easy to get, synthetic route is simple, easy to operate, and reaction condition is gentle, is suitable for producing in enormous quantities；Prepared room temperature phosphorimetry material quantum yield under air at room temperature is high, and Decay is long, and there is great application value in fields such as white light LEDs, false proof, cell imaging or biochemical analysises.
Description
Technical field
The invention belongs to luminescent material technical field, and in particular to a kind of pure organic room temperature phosphorimetry material of high-performance and its system
Preparation Method and application.
Background technology
Room temperature phosphorimetry material refers to that at room temperature material after excitation light irradiation stopping remains to light, and when continuing one section
Between, there is the longer life-span relative to fluorescent material, therefore false proof, information encryption and display field have important application valency
Value.Existing most of room temperature phosphorimetry materials are organometallic complexs, and their preparation is typically required for poison, expensive
Heavy metal, great threat is caused to health.Pure organic room temperature phosphorimetry material is subject to cheap, environmental friendliness
The extensive attention of researcher, but their phosphorescence performance is unsatisfactory, usual phosphorescence intensity is weaker, and the life-span is shorter, to oxygen
Gas is very sensitive, it is easy to be quenched under air.In order to obtain the transmitting of effective phosphorescence, generally require design and synthesize specific point
Minor structure, building-up process are complicated, loaded down with trivial details, it usually needs high temperature, the condition of high pressure, synthesis material are rare, expensive, and dispersion solvent has
Malicious, volatile, therefore limit its popularization and application.
Carbon is the basis of all known life on the earth.As which has various electron orbit characteristic (sp1、sp2、
sp3), therefore form the peculiar material of many structures and property.Carbon quantum dot is with good stability, toxicity is low, be easy to functionalization etc.
Advantage, is expected to substitute organic dyestuff and contains mostly the semiconductor-quantum-point of heavy metal, have in fields such as cell imaging, biochemical analysises
Very big application prospect.At present, only there is the carbon quantum dot composite of preparation photoluminescent property, few people to prepare the phosphorus that sets out
The carbon quantum dot composite of light.There is phosphorescent characteristics carbon quantum dot composite to have widened significantly its range of application for exploitation.Existing
Method with high-performance pure organic room temperature phosphorimetry material is not also prepared in some technology.
Content of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of preparation side of the pure organic room temperature phosphorimetry material of high-performance
Method, its are comprised the following steps：
S1, the carbon quantum dot that will be enriched in N element and O elements and carbamide are by 1:100～100000 quality compares mixed dissolution
In water, agitated reaction mixture is uniformly obtained；
S2, step S1 gained reaction mixture is heated 1～10 hour at 100～200 DEG C, then sequentially pass through cooling and
Grinding, obtains final product.
The method of the invention, with carbamide and the carbon quantum dot rich in N element and O elements as raw material, the raw material is pure to be had
Machine, nontoxic, cheap, be easy to get, synthetic route is simple, easy to operate, and reaction condition is gentle, is suitable for producing in enormous quantities, solves existing
The problem that phosphor material complicated process of preparation, preparing raw material are rare in technology and optical property is poor；The carbon quantum dot with
The reasonable mixture ratio of carbamide, by the interaction of the two, effectively inhibits the triplet nonradiative transition of carbon quantum dot, so as to pole
The earth promotes triplet phosphorescent emissions；Prepared room temperature phosphorimetry material quantum yield under air at room temperature is high, die-away time
Long.
The method of the invention, in the carbon quantum dot, the percentage composition of N element is 10%～25%；And/or, the carbon
In quantum dot, the percentage composition of O elements is 10%～25%.
The method of the invention, the carbon quantum dot are with Folic Acid as raw material, preferably by the method system for comprising the steps
Standby form：
S11, Folic Acid is dissolved in deionized water, be sufficiently stirred for, obtain mixed solution, the Folic Acid and deionized water
Mass ratio is 1:50～1000, preferably 1:50～150；
S12, step S11 gained mixed solution is reacted 1～5 hour at 150～300 DEG C, obtain initial soln；
S13, step S12 gained initial soln is centrifuged, takes the supernatant, and the clear liquid is dried, obtain final product.
Adopt with Folic Acid as raw material, the advantage for preparing carbon quantum dot is：Folate molecule is rich in amino and carboxyl, easy autohemagglutination
The carbon quantum dot formed rich in N and O is closed, generally also rich in nitrogen heterocyclic ring and is contained with the carbon quantum dot that Folic Acid is prepared as raw material in addition
Oxygen functional group, this are conducive to singletstate to the intersystem crossing of triplet, are conducive to the transmitting of phosphorescence.
Further, described in above-mentioned steps S13, the mode of centrifugation is：Under 3000～10000 revs/min of rotating speed, from
The heart 5～30 minutes；Preferably, under 8000～10000 revs/min of rotating speed, it is centrifuged 10～30 minutes；It is furthermore preferred that in rotating speed
Under 9500 revs/min, it is centrifuged 20 minutes.And/or, the mode dried described in step S13 is：Lyophilization 12～96 hours,
It is preferred that 60～80 hours, more preferably 72 hours.
The method of the invention, the quality of water described in step S1 are 1～1.2 times, preferably 1 times of urea quality.
The method of the invention, carbon quantum dot described in step S1 are 1 with the mass ratio of carbamide:300～50000, preferably
For 1:2400～12000 or 1:20000～40000.Above-mentioned carbon quantum dot and the preferred version of the mass ratio of carbamide, are promoting two
While person preferably plays interaction, more preferable economic benefit is also achieved.Further, the carbon quantum dot and carbamide
Mass ratio also preferably be following several schemes：1:6000～12000,1:1200～20000,1:300～24000, or 1:
1200～6000.
The method of the invention, reaction mixture described in step S2 are heated 2～8 hours preferably at 120～180 DEG C,
Heat more preferably at 150～170 DEG C 4～6 hours, further preferably heat 6 hours at 155 DEG C.
Present invention also offers the pure organic room temperature phosphorimetry material of high-performance prepared by said method.Prepared room temperature phosphorus
Luminescent material under air at room temperature quantum yield up to 36% (fluorescence and phosphorescence), average phosphorescent lifetime is up to 0.92s.
Present invention also offers the application of the pure organic room temperature phosphorimetry material of the high-performance, preferably in white light LEDs or anti-
The application of pseudo- aspect.
The above-mentioned technical proposal of the present invention has the advantages that：The method of the invention, raw material pure organic, nontoxic,
Inexpensively, it is easy to get, synthetic route is simple, easy to operate, reaction condition is gentle, is suitable for producing in enormous quantities；Prepared room temperature phosphorimetry material
Expect that quantum yield is up to 36% (fluorescence and phosphorescence) under air at room temperature, average phosphorescent lifetime, is prevented in white light LEDs up to 0.92s
The fields such as the encryption of pseudo-, information, cell imaging or biochemical analysises have great application value.
Description of the drawings
The electron microscope (1a) of carbon quantum dots of the Fig. 1 for being prepared with Folic Acid as raw material in the embodiment of the present invention 1, grain size distribution
(1b), infrared spectrum (1c), and XPS spectrum (1d)；
Fig. 2 is the emission spectrum of the fluorescent/phosphorescent of the pure organic room temperature phosphorimetry material of high-performance prepared by the embodiment of the present invention 3
(2a) with phosphorescent lifetime decay spectrum (2b)；
Fig. 3 is for carbon quantum dot in preparation method step S1 described in the embodiment of the present invention 1～8 with carbamide in different quality ratio
Under, the spectrogram of the pure organic room temperature phosphorimetry material of the high-performance of preparation, Fig. 3 a are fluorescence emission spectrum (1～8 point of sequence number therein
Each embodiment is not referred to), Fig. 3 b are phosphorescence emission spectra (sequence number therein 1～8 refers to each embodiment respectively)；
Fig. 4 be preparation method step S2 described in the embodiment of the present invention 9～12 and 3 in reaction mixture in the different heating time
Under, the spectrogram of the room temperature phosphorimetry material of preparation, Fig. 4 a are phosphorescence emission spectra, and Fig. 4 b are phosphorescent lifetime decay spectrum.
Specific embodiment
With reference to the accompanying drawings and examples embodiments of the present invention are described in further detail.Following examples are used for
The present invention is described, but can not be used for limiting the scope of the present invention.In this specific embodiment, involved raw material is commercially available
Obtain, and without the need for purification processes.
Embodiment 1
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 30 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 2
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 60 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 3
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 100 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 4
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 200 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 5
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 500 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 6
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 1000 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is continued
20 minutes are stirred until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 7
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 2000 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is continued
20 minutes are stirred until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 8
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 4000 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is continued
20 minutes are stirred until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 6 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 9
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 100 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 1 hour, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 10
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 100 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 2 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 11
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 100 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 4 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 12
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 10 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 260 DEG C
Heat 2 hours, obtains initial soln；
(3) by step (2) gained initial soln in 9500 revs/min of rotating speed, it is centrifuged 20 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 72 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 100 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is persistently stirred
20 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 155 DEG C
Heating 8 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 13
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 1g Folic Acid is dissolved in the deionized water of 950ml, is sufficiently stirred for 7 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in politef autoclave, at 150 DEG C, heating 5 is little
When, obtain initial soln；
(3) by step (2) gained initial soln in 3000 revs/min of rotating speed, it is centrifuged 30 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 90 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 12 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 7ml water, and is persistently stirred
18 minutes are mixed until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 125 DEG C
Heating 7.5 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Embodiment 14
A kind of preparation method of the pure organic room temperature phosphorimetry material of high-performance is present embodiments provided, which comprises the following steps：
(1) 2g Folic Acid is dissolved in the deionized water of 100ml, is sufficiently stirred for 15 minutes, obtains mixed solution；
(2) step (1) gained mixed solution is placed in the politef autoclave of 200ml, is added at 280 DEG C
Heat 1.5 hours, obtains initial soln；
(3) by step (2) gained initial soln in 8000 revs/min of rotating speed, it is centrifuged 25 minutes, the black for removing lower floor sinks
Form sediment, take upper strata brown color clear liquid, and by upper strata brown color clear liquid lyophilization 14 hours, that is, black is obtained rich in N, O element
Carbon quantum dot powder, then the carbon quantum dot powder is made into the carbon quantum dot aqueous solution of 5mg/ml；
(4) 10000 μ l of step (3) gained carbon quantum dot aqueous solution are taken with 6g carbamide mixed dissolution in 6ml water, and is continued
30 minutes are stirred until mixture is completely dissolved, reaction mixture is obtained；
(5) step (4) gained reaction mixture is placed in beaker, the beaker is placed in baking oven at 175 DEG C
Heating 2.5 hours, then natural cooling, grinding obtain the pure organic room temperature phosphorimetry material of the high-performance.
Referring to Fig. 1, the projection Electronic Speculum of Fig. 1 a carbon quantum dots shows that carbon quantum is almost spherical, disperses more uniform.Particle diameter
Scattergram (1b) shows the particle diameter distribution of carbon quantum dot in 1～6nm, and mean diameter is 3.41nm；Infrared spectrogram (1c) shows
The carbon quantum dot contains C=N, C=O ,-NH and OH-group group；XPS spectrum figure (1d) shows, the matter of C, N, O in the carbon quantum dot
Amount fraction is respectively 63.76%, 22.96% and 13.28%, shows that substantial amounts of N element and O units are contained in the carbon quantum dot surface
Element.
As shown in Figure 2 a, the pure organic room temperature phosphorimetry material of high-performance that prepared by embodiment 3, its phosphorescence compare fluorescence have wider
Emission peak, the phosphorescence quantum yields for measuring in the case where 280nm and 360nm are excited in addition be respectively 5% and 7%.Fig. 2 b are to implement
Example 3 excitation wavelength be 280nm, launch wavelength be 490nm under room temperature phosphorimetry average life figure, through calculating prepare phosphorescence
Material average life is up to 0.92s.
Fig. 3 is the spectrogram of the pure organic room temperature phosphorimetry material of high-performance prepared by the embodiment of the present invention 1～8, wherein：
The excitation wavelength of Fig. 3 a be 280nm, from Fig. 3 a it can be seen that room temperature phosphorimetry material fluorescence radiation cover 300～
600nm scopes, peak position is in 435nm；
The excitation wavelength of Fig. 3 b is 280nm, from Fig. 3 b it can be seen that the phosphorescence of room temperature phosphorimetry material luminous cover 400～
620nm scopes, peak position is in 490nm；
Fig. 4 is the spectrogram of the pure organic room temperature phosphorimetry material of high-performance prepared by the embodiment of the present invention 9～12 and 3, wherein：
The excitation wavelength of Fig. 4 a is 280nm；Fig. 4 b be excitation wavelength be 280nm, launch wavelength be 490nm under phosphorescent lifetime decay
Figure.
The performance parameter of the phosphor material that table 1 is prepared for different embodiments 1-8.
Table 1：Quantum yield and phosphorescent lifetime of the carbon quantum dot under different embodiments
Embodiments of the invention in order to example and description for the sake of and be given, and be not exhaustively or by this
Bright it is limited to disclosed form.Many modifications and variations are obvious for the ordinary skill in the art.Choosing
It is the principle and practical application in order to the present invention is more preferably described to select and describe embodiment, and makes one of ordinary skill in the art
It will be appreciated that the present invention is so as to designing the various embodiments with various modifications for being suitable to special-purpose.
Claims (10)
1. the preparation method of the pure organic room temperature phosphorimetry material of a kind of high-performance, it is characterised in that comprise the following steps：
S1, the carbon quantum dot that will be enriched in N element and O elements and carbamide are by 1:100～100000 quality is than mixed dissolution in water
In, agitated uniformly obtain reaction mixture；
S2, step S1 gained reaction mixture is heated 1～10 hour at 100～200 DEG C, then sequentially pass through cooling and grind
Mill, obtains final product.
2. method according to claim 1, it is characterised in that in the carbon quantum dot percentage composition of N element be 10%～
25%；And/or, the percentage composition 10%～25% of O elements in the carbon quantum dot.
3. method according to claim 1 or claim 2, it is characterised in that the carbon quantum dot is prepared from Folic Acid as raw material.
4. method according to claim 3, it is characterised in that the carbon quantum dot with Folic Acid as raw material, by including following step
Rapid method is prepared from：
S11, Folic Acid is dissolved in deionized water, be sufficiently stirred for, obtain mixed solution, the quality of the Folic Acid and deionized water
Than for 1:50～1000, preferably 1:50～150；
S12, step S11 gained mixed solution is reacted 1～5 hour at 150～300 DEG C, obtain initial soln；
S13, step S12 gained initial soln is centrifuged, takes the supernatant, and the clear liquid is dried, obtain final product.
5. method according to claim 4, it is characterised in that
Described in step S13, the mode of centrifugation is：Under 3000～10000 revs/min of rotating speed, it is centrifuged 5～30 minutes；It is preferred that
, under 8000～10000 revs/min of rotating speed, it is centrifuged 10～30 minutes；
And/or, the mode dried described in step S13 is：Lyophilization 12～96 hours, preferably 60～80 hours.
6. according to Claims 1 to 5 any one methods described, it is characterised in that the quality of water described in step S1 is carbamide matter
1～1.2 times of amount；
And/or, carbon quantum dot described in step S1 is 1 with the mass ratio of carbamide:300～50000, preferably 1:2400～
12000 or 1:20000～40000.
7. according to claim 1～6 any one methods described, it is characterised in that reaction mixture described in step S2 120～
Heat 2～8 hours at 180 DEG C, heat 4～6 hours preferably at 150～170 DEG C.
8. a kind of pure organic room temperature phosphorimetry material of the high-performance that prepared by any one of claim 1～7 methods described.
9. the application of the pure organic room temperature phosphorimetry material of high-performance described in claim 8.
10. application according to claim 9, it is characterised in that the pure organic room temperature phosphorimetry material of the high-performance is in white light
The application of LED or false proof aspects.
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