CN110172345B - Rare earth fluorescent powder prepared by doping graphene nano composite material and preparation method thereof - Google Patents
Rare earth fluorescent powder prepared by doping graphene nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides rare earth fluorescent powder prepared by doping a graphene nano composite material and a preparation method thereof. The general formula of the rare earth fluorescent powder is as follows: ca（1‑2x）CO3：x（Eu3+，K+) The composite material comprises calcium nitrate tetrahydrate, potassium carbonate, europium nitrate hexahydrate, graphene oxide and carbon quantum dots, wherein the molar ratio of the calcium nitrate tetrahydrate to the potassium carbonate is (0.70-0.90) to (0.05-0.20), the molar ratio of the calcium nitrate tetrahydrate to the europium nitrate hexahydrate is (0.70-0.90) to (0.05-0.20), and the mass ratio of the graphene oxide to the carbon quantum dots is (1-2) to (1-4). The invention has the beneficial effects that: the novel rare earth fluorescent powder is prepared by simple methods such as grinding, roasting and the like, so that the luminous efficiency of the rare earth fluorescent powder is preliminarily improved, and the stability of the rare earth fluorescent powder is improved.
Description
Technical Field
The invention belongs to the field of fluorescent powder, and particularly relates to rare earth fluorescent powder prepared by doping a graphene nano composite material and a preparation method thereof.
Background
The fluorescent powder has wide application and has wide application in the work and life of people. The fluorescent powder has bright and strong fluorescent color, and has the advantages of temperature resistance, tinting strength and brightness, and is suitable for processes such as extrusion, injection molding, blow molding, film blowing and the like, production of safety facilities, toys, packaging materials, shopping bags and other eye-catching commodities. The fluorescent powder has higher tinting strength, stronger fading resistance, extremely fine particle size and stronger solvent resistance, and is suitable for aqueous and non-aqueous systems such as curved surface and intaglio printing ink, screen printing ink, textile printing and dyeing ink, crayon colorant, paint coating, air-soluble paint, brushing paint, spray paint, baking paint, plastisol and the like. However, the existing red fluorescent powder has low effective conversion efficiency, unstable property and large light decay, so that the application range of the fluorescent powder is limited. The fluorescent powder composite material is an energy-saving and low-pollution green material, and under the new trend of 'energy conservation and emission reduction' advocated by the state, better market benefits can be inevitably created by researching and applying the fluorescent powder environment-friendly material.
Disclosure of Invention
Aiming at the technical problems, the invention discloses novel rare earth fluorescent powder which comprises calcium nitrate tetrahydrate, potassium carbonate, europium nitrate hexahydrate, graphene oxide and carbon quantum dots, wherein the molar ratio of the calcium nitrate tetrahydrate to the potassium carbonate is (0.70-0.90) - (0.05-0.20), the molar ratio of the calcium nitrate tetrahydrate to the europium nitrate hexahydrate is (0.70-0.90) - (0.05-0.20), and the mass ratio of the graphene oxide to the carbon quantum dots is (1-2) - (1-4).
Calcium nitrate is an industrial product with wide application, and is mainly used as a flocculant of rubber emulsion, a petroleum exploration well, sewage treatment and the like; the fertilizer is used as a quick-acting fertilizer for soilless culture and acid soil in agriculture; the light industry is used to manufacture fireworks and incandescent lampshades; the national defense industry is used for manufacturing explosives; the electronics industry is used to coat cathodes; and also is a raw material for preparing other nitrates.
The potassium carbonate is also an industrial product with wide application, and is mainly applied to the inorganic industry for manufacturing sodium potassium tartrate, potassium fluoaluminate, potassium thiocyanate and titanium dioxide; the medicine industry is used for preparing long-acting sulfanilamide, progesterone, cortisone, leucoderma, estradiol benzoate and other medicines; the glass enamel industry is used for preparing enamel powder to enhance the leveling property of the enamel powder, and the enamel powder is added into glass to play a role in fluxing and improve the transparency and the refractive index of the glass; the dye industry is used for manufacturing Yindan Tulin, disperse red 3B, reducing ash M and the like; the printing and dyeing industry is used for printing and dyeing of vat dyes and white discharge of ice dyeing; the rubber industry is used for manufacturing 4010 anti-aging agent; the wool and linen cotton industry is used for scouring cotton cloth and degreasing wool.
Europium nitrate is mainly applied to the industries of manufacturing fluorescent powder, electronic ceramic materials, europium compound intermediates, chemical reagents and the like.
Graphene oxide is a novel carbon material with excellent performance, and has a high specific surface area and rich functional groups on the surface. The graphene oxide composite materials including polymer composite materials and inorganic composite materials have a wide application field, so that the surface modification of graphene oxide becomes another important research point. The Shanghai application physical research of Chinese academy of sciences discovers that the application of graphene oxide in the PCR technology can obviously improve the specificity, sensitivity and amplification yield of PCR, can eliminate primer dimers formed in amplification, has a wide optimization interval, and can be widely applied to DNA templates with various concentrations and complexity. Compared with other carbon nano materials applied to the PCR technology, the graphene oxide has more excellent comprehensive effect on the optimization of PCR.
The carbon quantum dots are novel nano carbon materials which are composed of dispersed spheroidal carbon particles, have extremely small sizes (below 10 nm) and have fluorescence properties. The proper size, low cost and good biocompatibility of carbon quantum dots are crucial to the research in the fields of biomarkers and the like, and thus the emergence of the carbon quantum dots has attracted extensive attention of researchers. The carbon quantum dots have wide raw material sources and low preparation cost, have great advantages in the field of material preparation, and have good application prospects in wide fields of medical imaging equipment, tiny light-emitting diodes, chemical sensors, photocatalytic reactions and the like.
By adopting the technical scheme, the invention has the advantages that the luminescent efficiency and stability of the rare earth fluorescent powder are improved by adding the reduced graphene oxide-carbon quantum dot composite material, so that the luminescent performance is improved.
Preferably, the rare earth phosphor Ca（1-2x）CO3：x（Eu3+，K+) The preparation method of (0 < x < 0.50) comprises the following steps:
step A1: accurately weighing calcium nitrate tetrahydrate and potassium carbonate in a molar ratio of (0.70-0.90) to (0.05-0.20), and respectively and completely dissolving the calcium nitrate tetrahydrate and the potassium carbonate with a proper amount of deionized water;
step A2: accurately measuring (0.05-0.20) mol of europium nitrate hexahydrate solution, adding the solution into calcium nitrate tetrahydrate solution, and stirring and mixing uniformly;
step A3: the potassium carbonate solution was added dropwise to the calcium nitrate tetrahydrate solution to completely co-precipitate calcium ions and europium ions.
Step A4: the solution was filtered using a suction filtration apparatus and the precipitate was washed with deionized water.
Step A5: drying the precipitate in a constant-temperature drying oven at the drying temperature of 60-120 ℃ for 120-300 min to obtain a rare earth phosphor precursor;
step A6: accurately weighing a certain amount of potassium carbonate, adding a precursor, adding a small amount of deionized water, uniformly mixing and grinding, transferring into a crucible, and roasting in a high-temperature furnace at the roasting temperature of 150-550 ℃ for 180-480 min;
step A7: and grinding the roasted product to obtain the rare earth fluorescent powder sample.
Preferably, the preparation method of the reduced graphene oxide-carbon quantum dot composite material comprises the following steps:
step B1: accurately measuring the volume ratio of 1: (1-4) dripping the graphene oxide solution and the carbon quantum dot solution into the lining of the hydrothermal reaction kettle, and putting the lining into the hydrothermal reaction kettle;
step B2: placing the hydrothermal reaction kettle into a constant-temperature drying oven, and carrying out hydrothermal reaction at 120-300 ℃ for 3-24 h to obtain a graphene composite material;
preferably, the preparation method of the graphene phosphor material comprises the following steps:
step C1: accurately weighing the components in a mass ratio of 1: (0.0005-0.005) placing the rare earth fluorescent powder sample and the reduced graphene oxide-carbon quantum dot composite material into a mortar, adding deionized water to make the sample pasty, mixing and grinding to make the sample uniform;
step C2: putting the mixed and ground sample into a constant-temperature drying oven for drying at the drying temperature of 60-240 ℃ for 2-8 h;
step C3: and grinding and collecting the sample to obtain the graphene fluorescent powder.
By adopting the technical scheme of the invention, the reduced graphene oxide-carbon quantum dot composite material has the function of modifying the surface of the fluorescent powder, so that the luminous conversion efficiency of the fluorescent powder is improved, and the property is more stable. The yield of the fluorescence quantum of the carbon quantum dot can reach 80%, and the carbon quantum dot has a strong and wide excitation spectrum in a near ultraviolet band, the wide and strong excitation spectrum absorbs near ultraviolet energy, and then Eu can be enhanced through energy transfer+3The light emission of (1). When graphene is used as an energy acceptor, the energy transfer efficiency is increased in the same distance, so that reduced graphene oxide can be used as the energy acceptor in an energy transfer system to improve the energy transfer efficiency, and the graphene carbon quantum dots have excellent fluorescence performance, and can be compounded with reduced graphene to further enhance the function of the graphene carbon quantum dots as an energy transfer donor.
The invention has the beneficial effects that: the novel rare earth fluorescent powder is prepared by simple methods such as grinding, roasting and the like, so that the luminous efficiency of the rare earth fluorescent powder is preliminarily improved, and the stability of the rare earth fluorescent powder is improved.
Drawings
FIG. 1 is a fluorescence spectrum of example 1.
FIG. 2 is a fluorescence spectrum of example 2.
FIG. 3 is a fluorescence spectrum of example 3.
Detailed Description
Preferred embodiments of the present invention will be described in further detail below with reference to the accompanying drawings:
example 1
Firstly, preparing rare earth phosphor powder Ca0.80CO3：0.10（Eu3+，K+）。
(1) 11.335g of Ca (NO) were weighed out3)2·4H2Dissolving O in deionized water;
(2) slowly dripping 6mL of europium nitrate solution with the molar concentration of 1mmol/mL, and uniformly mixing;
(3) weighing 7.878g of K2CO3Dissolving in deionized water;
(4) will K2CO3The solution was slowly added dropwise to Ca (NO)3)2And Eu (NO)3)3A white precipitate is generated in the mixed solution of (1);
(5) filtering, washing and drying to obtain a fluorescent powder precursor;
(6) weighing 0.4146g of K2CO3Adding the mixture into a fluorescent powder precursor, adding a small amount of deionized water, and grinding to uniformly mix the fluorescent powder precursor and the deionized water;
(7) transferring the uniformly mixed sample into a crucible, and roasting in a muffle furnace at the roasting temperature of 200 ℃ for 300 min;
(8) and grinding and collecting the roasted product to obtain the rare earth fluorescent powder sample.
And secondly, preparing the reduced graphene oxide-carbon quantum dot composite material.
(1) Accurately measuring 1ml of graphene oxide solution with the concentration of 2 mg/ml;
(2) accurately measuring 2ml of carbon quantum dot solution with the concentration of 1 mg/ml;
(3) adding the two solutions into the inner liner of the hydrothermal reaction kettle;
(4) heating the reaction kettle in a constant-temperature drying box at a set temperature of 180 ℃ for 18 h;
and thirdly, preparing the graphene fluorescent powder material.
(1) Accurately weighing 12.00g of rare earth fluorescent powder, putting the rare earth fluorescent powder into a mortar, adding the reduced graphene oxide-carbon quantum dot composite material subjected to hydrothermal reaction, adding a small amount of deionized water, mixing and grinding to uniformly mix the two materials;
(2) putting the sample into a constant-temperature drying oven for drying, setting the temperature at 100 ℃ and the time for 240 min;
(3) and grinding and collecting the sample to obtain the required graphene fluorescent powder sample.
(4) And detecting the luminous intensity and luminous effect of the prepared fluorescent powder.
As shown in FIG. 1, the prepared rare earth fluorescent powder sample is analyzed by a FluoroMax-4 scientific research grade fluorescence spectrometer, the emission peak is 616nm, and the fluorescence intensity can reach more than 46 ten thousand (the light incoming quantity is 0.5).
Example 2
Firstly, preparing rare earth phosphor powder Ca0.84CO3：0.08（Eu3+，K+）。
(1) 11.902g of Ca (NO) were weighed out3)2·4H2Dissolving O in deionized water;
(2) 4.8mL of europium nitrate solution with the molar concentration of 1mmol/mL is slowly dripped and mixed uniformly;
(3) weighing 7.962g of K2CO3Dissolving in deionized water;
(4) will K2CO3The solution was slowly added dropwise to Ca (NO)3)2And Eu (NO)3)3A white precipitate is generated in the mixed solution of (1);
(5) filtering, washing and drying to obtain a fluorescent powder precursor;
(6) 0.3317g of K was weighed2CO3Adding the mixture into a fluorescent powder precursor, adding a small amount of deionized water, and grinding to uniformly mix the fluorescent powder precursor and the deionized water;
(7) transferring the uniformly mixed sample into a crucible, and roasting in a muffle furnace at the roasting temperature of 200 ℃ for 300 min;
(8) and grinding and collecting the roasted product to obtain the rare earth fluorescent powder sample.
And secondly, preparing the reduced graphene oxide-carbon quantum dot composite material.
(1) Accurately measuring 1ml of graphene oxide solution with the concentration of 2 mg/ml;
(2) accurately measuring 2ml of carbon quantum dot solution with the concentration of 1 mg/ml;
(3) adding the two solutions into the inner liner of the hydrothermal reaction kettle;
(4) heating the reaction kettle in a constant-temperature drying box at a set temperature of 180 ℃ for 18 h;
and thirdly, preparing the graphene fluorescent powder material.
(1) Accurately weighing 12.00g of rare earth fluorescent powder, putting the rare earth fluorescent powder into a mortar, adding the reduced graphene oxide-carbon quantum dot composite material subjected to hydrothermal reaction, adding a small amount of deionized water, mixing and grinding to uniformly mix the two materials;
(2) putting the sample into a constant-temperature drying oven for drying, setting the temperature at 100 ℃ and the time for 240 min;
(3) and grinding and collecting the sample to obtain the required graphene fluorescent powder sample.
(4) And detecting the luminous intensity and luminous effect of the prepared fluorescent powder.
As shown in FIG. 2, the prepared rare earth fluorescent powder sample is analyzed by a FluoroMax-4 scientific research grade fluorescence spectrometer, the emission peak is 614nm, and the fluorescence intensity can reach more than 40 ten thousand (the light incoming amount is 0.5).
Example 3
Firstly, preparing rare earth fluorescent powder Ca0.88CO3: 0.06 (Eu 3+, K +).
(1) Weighing 12.469g of Ca (NO3) 2.4H 2O and dissolving in deionized water;
(2) slowly dripping 3.6mL of europium nitrate solution with the molar concentration of 1mmol/mL, and uniformly mixing;
(3) weighing 8.043g of K2CO3 and dissolving in deionized water;
(4) slowly and dropwise adding the K2CO3 solution into a mixed solution of Ca (NO3)2 and Eu (NO3)3 to generate white precipitates;
(5) filtering, washing and drying to obtain a fluorescent powder precursor;
(6) 0.2487g of K2CO3 is weighed and added into a fluorescent powder precursor, a small amount of deionized water is added, and grinding is carried out to ensure that the two are uniformly mixed;
(7) transferring the uniformly mixed sample into a crucible, and roasting in a muffle furnace at the roasting temperature of 200 ℃ for 300 min;
(8) and grinding and collecting the roasted product to obtain the rare earth fluorescent powder sample.
And secondly, preparing the reduced graphene oxide-carbon quantum dot composite material.
(1) Accurately measuring 1ml of graphene oxide solution with the concentration of 2 mg/ml;
(2) accurately measuring 2ml of carbon quantum dot solution with the concentration of 1 mg/ml;
(3) adding the two solutions into the inner liner of the hydrothermal reaction kettle;
(4) heating the reaction kettle in a constant-temperature drying box at a set temperature of 180 ℃ for 18 h;
and thirdly, preparing the graphene fluorescent powder material.
(1) Accurately weighing 12.00g of rare earth fluorescent powder, putting the rare earth fluorescent powder into a mortar, adding the reduced graphene oxide-carbon quantum dot composite material subjected to hydrothermal reaction, adding a small amount of deionized water, mixing and grinding to uniformly mix the two materials;
(2) putting the sample into a constant-temperature drying oven for drying, setting the temperature at 100 ℃ and the time for 240 min;
(3) and grinding and collecting the sample to obtain the required graphene fluorescent powder sample.
(4) And detecting the luminous intensity and luminous effect of the prepared fluorescent powder.
As shown in FIG. 3, the prepared rare earth fluorescent powder sample is analyzed by a FluoroMax-4 scientific research grade fluorescence spectrometer, the emission peak is at 616nm, and the fluorescence intensity can reach more than 36 thousands (the light incoming amount is 0.5).
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (4)
1. The method for preparing the graphene fluorescent powder material is characterized in that the graphene fluorescent powder material comprises rare earth fluorescent powder and a reduced graphene oxide-carbon quantum dot composite material, and the general formula of the rare earth fluorescent powder is as follows: ca（1-2x）CO3：x（Eu3 +，K+) (x is more than 0 and less than 0.50), the molar ratio of the calcium nitrate tetrahydrate to the potassium carbonate is (0.70-0.90) to (0.05-0.20), the molar ratio of the calcium nitrate tetrahydrate to the europium nitrate hexahydrate is (0.70-0.90) to (0.05-0.20), and the mass ratio of the graphene oxide to the carbon quantum dots is (1-2) to (1-4); the method comprises the following steps:
step A1: accurately weighing calcium nitrate tetrahydrate and potassium carbonate in a molar ratio of (0.70-0.90) to (0.05-0.20), and respectively and completely dissolving the calcium nitrate tetrahydrate and the potassium carbonate with a proper amount of deionized water;
step A2: accurately measuring (0.05-0.20) mol of europium nitrate hexahydrate solution, adding the solution into calcium nitrate tetrahydrate solution, and stirring and mixing uniformly;
step A3: dropwise adding a potassium carbonate solution into a calcium nitrate tetrahydrate solution to ensure that calcium ions and europium ions are completely precipitated together;
step A4: filtering the solution by using a suction filtration device, and washing precipitates by using deionized water;
step A5: drying the precipitate in a constant-temperature drying oven at the drying temperature of 60-120 ℃ for 120-300 min to obtain a rare earth phosphor precursor;
step A6: accurately weighing a certain amount of potassium carbonate, adding a precursor, adding a small amount of deionized water, uniformly mixing and grinding, transferring into a crucible, and roasting in a high-temperature furnace at the roasting temperature of 150-550 ℃ for 180-480 min;
step A7: and grinding the roasted product to obtain the rare earth fluorescent powder sample.
2. The method of claim 1, wherein: the preparation method of the reduced graphene oxide-carbon quantum dot composite material comprises the following steps:
step B1: accurately measuring the volume ratio of 1: (1-4) dripping the graphene oxide solution and the carbon quantum dot solution into the lining of the hydrothermal reaction kettle, and putting the lining into the hydrothermal reaction kettle;
step B2: and (3) putting the hydrothermal reaction kettle into a constant-temperature drying oven, and carrying out hydrothermal reaction at the temperature of 120-300 ℃ for 3-24 h to obtain the reduced graphene oxide-carbon quantum dot composite material.
3. The method of claim 1, wherein: the preparation method of the graphene fluorescent powder comprises the following steps:
step C1: accurately weighing the components in a mass ratio of 1: (0.0005-0.005) placing the rare earth fluorescent powder and the reduced graphene oxide-carbon quantum dot composite material into a mortar, adding a small amount of deionized water to make a sample into a paste, and mixing and grinding to make the sample uniform;
step C2: putting the mixed and ground sample into a constant-temperature drying oven for drying at the drying temperature of 60-240 ℃ for 2-8 h;
step C3: and grinding and collecting the sample to obtain the required graphene fluorescent powder.
4. The method of claim 1, wherein in step a2, europium nitrate hexahydrate of concentration 1mmol/ml is used.
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| Hybrid luminescent materials of graphene oxide and rare-earth complexes with stronger luminescence intensity and better thermal stability;Zhang Xiaoxiong;《Dyes and Pigments》;20170110;第140卷;图6、图8，第156页左栏第2段 * |
| Low temperature microwave solid-state synthesis of CaCO3: Eu3+, K+ phosphors;Cheng Qijun;《Advanced Powder Technology》;20150228;第26卷(第3期);图5 * |
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