CN110172345A - A kind of graphene nanocomposite material doping prepares rare earth phosphor and preparation method thereof - Google Patents
A kind of graphene nanocomposite material doping prepares rare earth phosphor and preparation method thereof Download PDFInfo
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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Abstract
The present invention provides a kind of graphene nanocomposite material doping and prepares rare earth phosphor and preparation method thereof.The general formula of the rare earth phosphor are as follows: Ca(1-2x)CO3: x(Eu3+, K+) it include calcium nitrate tetrahydrate, potassium carbonate, six nitric hydrate europiums, graphene oxide, carbon quantum dot, the molar ratio of the calcium nitrate tetrahydrate and potassium carbonate is (0.70~0.90): (0.05~0.20), the molar ratio of the calcium nitrate tetrahydrate and six nitric hydrate europiums is (0.70~0.90): the mass ratio of (0.05~0.20), the graphene oxide and carbon quantum dot is (1~2): (1~4).The beneficial effects of the present invention are: being prepared for novel rare earth phosphor by simple and easy methods such as grinding, roastings, realizes and tentatively improve rare earth phosphor luminous efficiency, and improve the stability of rare earth phosphor.
Description
Technical field
The invention belongs to fluorescent powder fields more particularly to a kind of graphene nanocomposite material doping to prepare rare earth phosphor
And preparation method thereof.
Background technique
The purposes of fluorescent powder is very extensive, has in the Working Life of people and has been widely used.Fluorescent powder have it is bright-coloured and
Very strong fluorescent color, while in terms of having the advantages that temperature tolerance, tinting strength, tinting power and vividness, be suitable for squeezing out, injection molding, blow molding and
The techniques such as blown film, production safety facility, toy, packaging material, do shopping material, shopping bag and some other eye-catching commodity.Fluorescence
Powder has higher tinting strength, tinting power, stronger fade resistance, superfine partial size and stronger solvent resistance energy, is suitable for curved surface and notch board
Ink is printed, screen printing ink, textile printing and dyeing ink, wax crayon colorant, paint, the molten paint of gas, mopping and spray painting are baked
Paint, plastisol etc. is aqueous and non-aqueous system.But existing red fluorescence powder is since effective transfer efficiency is low, property is unstable
Calmly, light decay is big, limits the application range of fluorescent powder.Fluorescence powder composite material is a kind of energy saving, low pollution green material,
" energy-saving and emission-reduction " that country advocates under the new situation, are studied and will necessarily be created preferably using fluorescent powder environmentally friendly material
Market efficiency.
Summary of the invention
Against the above technical problems, the invention discloses a kind of novel rare earth fluorescent powder, including calcium nitrate tetrahydrate, carbonic acid
The molar ratio of potassium, six nitric hydrate europiums, graphene oxide, carbon quantum dot, the calcium nitrate tetrahydrate and potassium carbonate be (0.70~
0.90): the molar ratio of (0.05~0.20), the calcium nitrate tetrahydrate and six nitric hydrate europiums is (0.70~0.90): (0.05
~0.20), the graphene oxide and the mass ratio of carbon quantum dot are (1~2): (1~4).
Calcium nitrate is a kind of widely used industrial products, is mainly used for the flocculant of rubber latex, petroleum prospect pit, sewage
Processing etc.；Agriculturally it is used as soilless cultivation, the quick-acting fertilizer of acid soil；Light industry is for manufacturing pyrotechnics and incandescent lampshade；State
Anti- industry is for manufacturing explosive；Electronic instrument industry is used for coated cathode；It is simultaneously also the raw material of the other Nitrates of manufacture.
Potassium carbonate is also a kind of widely used industrial products, is mainly used in inorganic industrial manufacture sodium potassium tartrate tetrahydrate, aluminium
Potassium fluorozirconate, potassium rhodanide, titanium dioxide；Medical industry is for manufacturing sulfamethoxyplridazine, progesterone, cortisone, Orthocoll, benzoic acid
The medicines such as estradiol；Glass is warded off industry and is prepared for enamel frit, to enhance its levelability, is added in glass and plays fluxing action, and improve
Glass transparent degree and refraction coefficient；Dye industry is for manufacturing negative red native woods, Disperse Red 3B, Vat Grey M etc.；Printing and dyeing industry is used for
The printing and dyeing of reducing dye and the dawn of ice dyeing；Rubber industry is for manufacturing 4010 anti-aging agents；Maoma cotton industry is used for cotton boiling-off
With the degreasing of wool.
Europium nitrate is mainly used in the works such as manufacture fluorescent powder, electron ceramic material, europium compound intermediate, chemical reagent
Industry.
Graphene oxide is a kind of new carbon haveing excellent performance, specific surface area with higher and surface official abundant
It can group.Graphene oxide composite material, which includes polymerization species composite material, and inorganic species composite material is even more has widely
Application field, therefore the surface of graphene oxide is modified as another research emphasis.Chinese Academy of Sciences's Shanghai Applied Physics is ground
Study carefully and find for graphene oxide to be applied in round pcr, is remarkably improved specificity, sensitivity and the amplification yield of PCR, and
The primer dimer formed in amplification can be eliminated, and optimization section is wide, is widely portable to the DNA of various concentration and complexity
Template.Compared with the carbon nanomaterial that other have been applied in round pcr, graphene oxide has the optimization of PCR more excellent
Different resultant effect.
Carbon quantum dot is made of the near-spherical carbon particle dispersed, and size is minimum (in 10nm or less), has photoluminescent property
Novel nano carbon material.Suitably sized, the cheap cost of carbon quantum dot and good bio-compatibility are for biomarker
The research in equal fields is vital, therefore its appearance causes researcher and widely pays close attention to.The raw material of carbon quantum dot comes
Source is extensive, and preparation cost is also relatively low, there is very big advantage in field of material preparation, in medical imaging devices, small shines
There is preferable application prospect in the very wide field of diode, chemical sensor, light-catalyzed reaction etc..
The invention adopts the above technical scheme, the advantage is that, compound by the way that redox graphene-carbon quantum dot is added
Material improves the luminous efficiency and stability of rare earth phosphor, to improve luminescent properties.
Preferably, the rare earth phosphor Ca(1-2x)CO3: x(Eu3+, K+) (0 < x < 0.50) preparation method include with
Under several steps:
Step A1: it accurately weighs molar ratio (0.70~0.90): the calcium nitrate tetrahydrate and potassium carbonate of (0.05~0.20), respectively
It is completely dissolved with suitable deionized water；
Step A2: the accurate six nitric hydrate europium solution for measuring (0.05~0.20) mol are added in calcium nitrate tetrahydrate solution, stir
It mixes uniformly mixed；
Step A3: solution of potassium carbonate is added dropwise in calcium nitrate tetrahydrate solution, and calcium ion and europium ion is made to sink jointly completely
It forms sediment.
Step A4: above-mentioned solution is filtered using Suction filtration device, and sediment is washed with deionized.
Step A5: sediment being put into thermostatic drying chamber and is dried, and 60~120 DEG C of drying temperature, drying time 120~
300min obtains rare earth phosphor presoma；
Step A6: accurately weighing a certain amount of potassium carbonate and presoma be added, a small amount of deionized water is added, and mixed grinding is uniform, turns
It moves in crucible, is put into high temperature furnace and roasts, 150~550 DEG C of maturing temperature, 180~480min of calcining time；
Step A7: baked product is ground, and rare earth phosphor sample can be obtained.
Preferably, the redox graphene-carbon quantum dot composite material preparation method including the following steps:
Step B1: volume ratio 1:(1~4 will accurately be measured) graphene oxide solution and carbon quantum dot solution, instill hydro-thermal it is anti-
It answers in kettle liner, and liner is put into hydrothermal reaction kettle；
Step B2: hydrothermal reaction kettle is put into thermostatic drying chamber, it is made to carry out hydro-thermal reaction at 120~300 DEG C, when reaction
Between 3~for 24 hours, obtain graphene composite material；
Preferably, the preparation method of the graphene phosphor material powder including the following steps:
Step C1: accurately weigh mass ratio be 1:(0.0005~0.005) rare earth phosphor sample and redox graphene-
Carbon quantum dot composite material is placed in mortar and is added deionized water, makes sample in starchiness, and mixed grinding makes it uniformly；
Step C2: the sample after mixed grinding being put into thermostatic drying chamber and is dried, and 60~240 DEG C of drying temperature, drying
2~8h of time；
Step C3: sample is ground, and collects, graphene fluorescent powder can be obtained.
Using technical solution of the present invention, redox graphene-carbon quantum dot composite material plays modified fluorescent powder table
The effect in face promotes the luminance conversion efficiency of fluorescent powder, and property is more stable.Not only fluorescence quantum yield may be up to carbon quantum dot
80%, and have a strong and roomy excitation spectrum near ultraviolet band, the strong excitation spectrum of this width absorbs the energy of near ultraviolet
Amount may then pass through energy transfer and remove enhancing Eu+3Shine.When graphene is as energy acceptor, in same distance, energy
Transfer efficiency increases, it is possible to be used for energy transfer system using redox graphene as energy acceptor to improve energy and turn
Efficiency is moved, and since graphene carbon quantum dot has excellent fluorescence property, it is compound with reduced graphene, it can be further
Enhance its function as energy transfer donor.
The beneficial effects of the present invention are: it is prepared for novel rare earth phosphor by simple and easy methods such as grinding, roastings, it is real
Rare earth phosphor luminous efficiency is now tentatively improved, and improves the stability of rare earth phosphor.
Detailed description of the invention
Fig. 1 is the fluorescence spectra of embodiment 1.
Fig. 2 is the fluorescence spectra of embodiment 2.
Fig. 3 is the fluorescence spectra of embodiment 3.
Specific embodiment
With reference to the accompanying drawing, preferably embodiment of the invention is described in further detail:
Embodiment 1
One, rare earth phosphor powder Ca is prepared0.80CO3: 0.10(Eu3+, K+).
(1) Ca (NO of 11.335g is weighed3)2·4H2O is dissolved in deionized water；
(2) the europium nitrate solution 6mL that molar concentration is 1mmol/ml is slowly added dropwise, is uniformly mixed；
(3) K of 7.878g is weighed2CO3It is dissolved in deionized water；
(4) by K2CO3Solution is slowly dropped to Ca (NO3)2With Eu (NO3)3Mixed solution in, generate white precipitate；
(5) it is filtered, washed, dries, obtain fluorescent powder presoma；
(6) K of 0.4146g is weighed2CO3It is added in fluorescent powder presoma, a small amount of deionized water is added, grind, mix the two
Uniformly；
(7) uniformly mixed sample is transferred in crucible, is put into Muffle furnace and is roasted, 200 DEG C of maturing temperature, when roasting
Between 300min；
(8) baked product is ground, collects, obtains rare earth phosphor sample.
Two, redox graphene-carbon quantum dot composite material is prepared.
(1) the graphene oxide solution 1ml that concentration is 2mg/ml is accurately measured；
(2) the carbon quantum dot solution 2ml that concentration is 1mg/ml is accurately measured；
(3) two kinds of solution are added in hydrothermal reaction kettle liner；
(4) reaction kettle is placed in thermostatic drying chamber and is heated, 180 DEG C of set temperature, setting time 18h；
Three, graphene phosphor material powder is prepared.
(1) it accurately weighs 12.00g rare earth phosphor to be put into mortar, the reduction-oxidation graphite Jing Guo hydro-thermal reaction is added
Alkene-carbon quantum dot composite material, can be added a small amount of deionized water, and mixed grinding is uniformly mixed two kinds of materials；
(2) sample is put into thermostatic drying chamber and is dried, 100 DEG C of set temperature, setting time 240min；
(3) sample is ground, collects, obtains required graphene fluorescent powder sample.
(4) luminous intensity and illumination effect of the prepared fluorescent powder of detection.
As shown in Figure 1, prepared rare earth phosphor sample is analyzed by FluoroMax-4 scientific research grade Fluorescence Spectrometer,
It radiates peak and is in 616nm, and fluorescence intensity is up to 460,000 or more (light-inletting quantities 0.5).
Embodiment 2
One, rare earth phosphor powder Ca is prepared0.84CO3: 0.08(Eu3+, K+).
(1) Ca (NO of 11.902g is weighed3)2·4H2O is dissolved in deionized water；
(2) the europium nitrate solution 4.8mL that molar concentration is 1mmol/ml is slowly added dropwise, is uniformly mixed；
(3) K of 7.962g is weighed2CO3It is dissolved in deionized water；
(4) by K2CO3Solution is slowly dropped to Ca (NO3)2With Eu (NO3)3Mixed solution in, generate white precipitate；
(5) it is filtered, washed, dries, obtain fluorescent powder presoma；
(6) K of 0.3317g is weighed2CO3It is added in fluorescent powder presoma, a small amount of deionized water is added, grind, mix the two
Uniformly；
(7) uniformly mixed sample is transferred in crucible, is put into Muffle furnace and is roasted, 200 DEG C of maturing temperature, when roasting
Between 300min；
(8) baked product is ground, collects, obtains rare earth phosphor sample.
Two, redox graphene-carbon quantum dot composite material is prepared.
(1) the graphene oxide solution 1ml that concentration is 2mg/ml is accurately measured；
(2) the carbon quantum dot solution 2ml that concentration is 1mg/ml is accurately measured；
(3) two kinds of solution are added in hydrothermal reaction kettle liner；
(4) reaction kettle is placed in thermostatic drying chamber and is heated, 180 DEG C of set temperature, setting time 18h；
Three, graphene phosphor material powder is prepared.
(1) it accurately weighs 12.00g rare earth phosphor to be put into mortar, the reduction-oxidation graphite Jing Guo hydro-thermal reaction is added
Alkene-carbon quantum dot composite material, can be added a small amount of deionized water, and mixed grinding is uniformly mixed two kinds of materials；
(2) sample is put into thermostatic drying chamber and is dried, 100 DEG C of set temperature, setting time 240min；
(3) sample is ground, collects, obtains required graphene fluorescent powder sample.
(4) luminous intensity and illumination effect of the prepared fluorescent powder of detection.
As shown in Figure 2, prepared rare earth phosphor sample is analyzed by FluoroMax-4 scientific research grade Fluorescence Spectrometer,
It radiates peak and is in 614nm, and fluorescence intensity is up to 400,000 or more (light-inletting quantities 0.5).
Embodiment 3
One, rare earth phosphor powder Ca0.88CO3:0.06(Eu3+, K+ are prepared).
(1) Ca (NO3) 24H2O for weighing 12.469g is dissolved in deionized water；
(2) the europium nitrate solution 3.6mL that molar concentration is 1mmol/ml is slowly added dropwise, is uniformly mixed；
(3) K2CO3 for weighing 8.043g is dissolved in deionized water；
(4) K2CO3 solution is slowly dropped in the mixed solution of Ca (NO3) 2 and Eu (NO3) 3, generates white precipitate；
(5) it is filtered, washed, dries, obtain fluorescent powder presoma；
(6) K2CO3 for weighing 0.2487g is added in fluorescent powder presoma, and a small amount of deionized water is added, and grinds, and mixes the two
Uniformly；
(7) uniformly mixed sample is transferred in crucible, is put into Muffle furnace and is roasted, 200 DEG C of maturing temperature, when roasting
Between 300min；
(8) baked product is ground, collects, obtains rare earth phosphor sample.
Two, redox graphene-carbon quantum dot composite material is prepared.
(1) the graphene oxide solution 1ml that concentration is 2mg/ml is accurately measured；
(2) the carbon quantum dot solution 2ml that concentration is 1mg/ml is accurately measured；
(3) two kinds of solution are added in hydrothermal reaction kettle liner；
(4) reaction kettle is placed in thermostatic drying chamber and is heated, 180 DEG C of set temperature, setting time 18h；
Three, graphene phosphor material powder is prepared.
(1) it accurately weighs 12.00g rare earth phosphor to be put into mortar, the reduction-oxidation graphite Jing Guo hydro-thermal reaction is added
Alkene-carbon quantum dot composite material, can be added a small amount of deionized water, and mixed grinding is uniformly mixed two kinds of materials；
(2) sample is put into thermostatic drying chamber and is dried, 100 DEG C of set temperature, setting time 240min；
(3) sample is ground, collects, obtains required graphene fluorescent powder sample.
(4) luminous intensity and illumination effect of the prepared fluorescent powder of detection.
As shown in figure 3, prepared rare earth phosphor sample is analyzed by FluoroMax-4 scientific research grade Fluorescence Spectrometer,
It radiates peak and is in 616nm, and fluorescence intensity is up to 360,000 or more (light-inletting quantities 0.5).
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (5)
1. a kind of rare earth phosphor, which is characterized in that the general formula of the rare earth phosphor are as follows: Ca(1-2x)CO3: x(Eu3+, K+) (0 <
X < 0.50) it include calcium nitrate tetrahydrate, potassium carbonate, six nitric hydrate europiums, graphene oxide, carbon quantum dot, the four hydrations nitre
The molar ratio of sour calcium and potassium carbonate is (0.70~0.90): (0.05~0.20), the calcium nitrate tetrahydrate and six nitric hydrates
The molar ratio of europium is (0.70~0.90): the mass ratio of (0.05~0.20), the graphene oxide and carbon quantum dot be (1~
2): (1~4).
2. a kind of method for preparing rare earth phosphor as described in claim 1, it is characterised in that: including the following steps:
Step A1: it accurately weighs molar ratio (0.70~0.90): the calcium nitrate tetrahydrate and potassium carbonate of (0.05~0.20), respectively
It is completely dissolved with suitable deionized water；
Step A2: the accurate six nitric hydrate europium solution for measuring (0.05~0.20) mol are added in calcium nitrate tetrahydrate solution, stir
It mixes uniformly mixed；
Step A3: solution of potassium carbonate is added dropwise in calcium nitrate tetrahydrate solution, and calcium ion and europium ion is made to sink jointly completely
It forms sediment；
Step A4: above-mentioned solution is filtered using Suction filtration device, and sediment is washed with deionized；
Step A5: sediment being put into thermostatic drying chamber and is dried, and 60~120 DEG C of drying temperature, drying time 120~
300min obtains rare earth phosphor presoma；
Step A6: accurately weighing a certain amount of potassium carbonate and presoma be added, a small amount of deionized water is added, and mixed grinding is uniform, turns
It moves in crucible, is put into high temperature furnace and roasts, 150~550 °C of maturing temperature, 180~480min of calcining time；
Step A7: baked product is ground, and rare earth phosphor sample can be obtained.
3. method according to claim 2, it is characterised in that: the preparation method of the graphene nanocomposite material include with
Under several steps:
Step B1: volume ratio 1:(1~4 will accurately be measured) graphene oxide solution and carbon quantum dot solution, instill hydro-thermal it is anti-
It answers in kettle liner, and liner is put into hydrothermal reaction kettle；
Step B2: hydrothermal reaction kettle is put into thermostatic drying chamber, it is made to carry out hydro-thermal reaction at 120~300 DEG C, when reaction
Between 3~for 24 hours, obtain graphene composite material.
4. the method stated such as claim 3, it is characterised in that: the preparation method of the graphene fluorescent powder includes following step
It is rapid:
Step C1: accurately weigh mass ratio be 1:(0.0005~0.005) rare earth phosphor and redox graphene-carbon amounts
Son point composite material, is placed in mortar and is added a small amount of deionized water, make sample in starchiness, mixed grinding makes it uniformly；
Step C2: the sample after mixed grinding being put into thermostatic drying chamber and is dried, and 60~240 DEG C of drying temperature, drying
2~8h of time；
Step C3: sample is ground, and collects, required graphene fluorescent powder can be obtained.
5. method according to claim 2, which is characterized in that in the step A2, use concentration for six water of 1mmol/ml
Close europium nitrate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116285988A (en) * | 2023-03-28 | 2023-06-23 | 中国科学院长春应用化学研究所 | Rare earth-framework nucleic acid nanocomposite and preparation method and application thereof |
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| CN101643643A (en) * | 2009-02-05 | 2010-02-10 | 西南科技大学 | Preparation method for low-temperature synthetic calcium carbonate-based red lanthanide luminescent material |
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2019
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101643643A (en) * | 2009-02-05 | 2010-02-10 | 西南科技大学 | Preparation method for low-temperature synthetic calcium carbonate-based red lanthanide luminescent material |
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| CHENG QIJUN: "Low temperature microwave solid-state synthesis of CaCO3: Eu3+, K+ phosphors", 《ADVANCED POWDER TECHNOLOGY》 * |
| ZHANG XIAOXIONG: "Hybrid luminescent materials of graphene oxide and rare-earth complexes with stronger luminescence intensity and better thermal stability", 《DYES AND PIGMENTS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116285988A (en) * | 2023-03-28 | 2023-06-23 | 中国科学院长春应用化学研究所 | Rare earth-framework nucleic acid nanocomposite and preparation method and application thereof |
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