CN110551500A - DTAB-assisted red fluorescent powder with enhanced luminescence property and preparation method thereof - Google Patents
DTAB-assisted red fluorescent powder with enhanced luminescence property and preparation method thereof Download PDFInfo
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Abstract
the invention discloses a DTAB-assisted red fluorescent powder with enhanced luminescent property and a preparation method thereof, wherein the chemical general formula of the fluorescent powder is LiGd 0.85 (MoO 4) 2: 15% Eu 3+, required medicines are weighed according to the stoichiometric ratio of Gd, Mo and Eu elements in the general formula, an intermediate product is obtained by a hydrothermal method, and finally the intermediate product is calcined at 650 ℃ to obtain the red fluorescent powder with significantly enhanced luminescent property, an excitation spectrogram and an emission spectrogram show that the luminescent intensity is more than two times higher than that when the surfactant DTAB is not added, the fluorescent powder has a strong excitation peak at 465nm within the range of 350-plus-500 nm, which shows that the fluorescent powder can be effectively excited by blue light and the absorption of ultraviolet light is also obviously improved compared with that when the surfactant is not added, the fluorescent powder synthesized by the method successfully and effectively improves the red fluorescent powder with effectively excited by the blue light, and provides an important thought for subsequent research.
Description
Technical Field
the invention relates to the field of rare earth luminescent materials, in particular to DTAB-assisted red fluorescent powder with enhanced luminescent property and a preparation method thereof.
Background
4 2 3+The most common white light LED in the market at present has low color rendering index due to lack of red light composition, cannot realize warm white light emission, and the gadolinium lithium molybdate has a scheelite structure, belongs to dimolybdate and has high physical and chemical stability.
at present, no report is found on a method for improving the performance of the fluorescent powder by the surfactant-assisted hydrothermal synthesis, the method effectively improves the luminous performance of the fluorescent powder, provides an important idea for subsequent research, and no report related to the fluorescent powder is found so far.
disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the DTAB-assisted red fluorescent powder with enhanced luminous performance and the preparation method thereof, the luminous performance of the red fluorescent powder is enhanced by more than two times than that of the original red fluorescent powder by adding the surfactant DTAB, and a certain foundation is laid for the research and preparation of the performance of the rare earth doped luminous material taking LiGd (MoO 4) 2 as a matrix.
In order to achieve the purpose, the invention adopts the following technical scheme that the DTAB-assisted red fluorescent powder with enhanced luminescence property and the preparation method thereof comprise the following steps:
Step 1, weighing Gd (NO 3) 3 & 6H 2 O solid powder and Li 2 MoO 4 solid powder and weighing Eu (NO 3) 3 solution respectively according to the stoichiometric ratio of Eu element, Mo element and Gd element in LiGd (MoO 4) 2: 15% Eu 3+;
Step 2, dissolving Gd (NO 3) 3.6H 2 O solid powder obtained in the step 1 in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
Step 3, dripping the solution A obtained in the step 2 into the solution B, and uniformly mixing at room temperature;
Step 4, adjusting the pH value of the mixed milky white solution obtained in the step 3 to 3-11 to obtain a solution C;
step 5, adding DTAB solid powder into the solution C obtained in the step 4, and uniformly stirring to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 20 mmol/L-180 mmol/L;
step 6, reacting the precursor solution obtained in the step 5 at 240 ℃ for 24 hours, and cooling to room temperature to obtain a solution D;
step 7, separating the solution D obtained in the step 6, washing, centrifuging and drying to obtain an intermediate product;
And 8, calcining the intermediate product obtained in the step 7 at 635-700 ℃ for 3-5 h in an air atmosphere to obtain the DTAB-assisted red fluorescent powder with enhanced luminescence property.
In the step 3, when the solution A is dripped into the solution B, the dripping speed is 2-3 minutes per 5 mL.
In the step 3, magnetic stirring is adopted, and the stirring time is 60-100 min.
In step 4, the pH value of the mixed solution is adjusted by LiOH and diluted HNO 3 solution.
further, in step 5, DTAB was added at a concentration of 60 mmol/L.
and (5) sealing and reacting the precursor solution obtained in the step (5) in a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%.
washing the solution D obtained in the step 6 by water and ethanol alternately; the centrifugal speed is 10000r/min, and the centrifugal time is 3 min; drying at 70 deg.C for 24 h.
further, the calcination temperature in step 7 was 650 ℃.
the chemical formula of the fluorescent powder prepared by the method is LiGd (MoO 4) 2: 15% Eu 3+.
Compared with the prior art, the invention has the beneficial effects that Gd (NO 3) 3 & 6H 2 O and Li 2 MoO 4 are used as reaction raw materials, main elements of the Gd are the same as target products, other impurity ions or other phases are not introduced or generated in the reaction process, the product purity is improved, hydrothermal reaction is carried out at a higher temperature, phase crystallization is facilitated, Li 2 MoO 4 provides two elements required by target products, the preparation process can be simplified, meanwhile, Eu (NO 3) 3 does not introduce other impurity ions different from a substrate, DTAB is added into a reaction system, the emission spectra of the DTAB and the DTAB are similar, the luminous intensity is different, the luminous intensity is more than that of the original DTAB after the DTAB is added, the appearance of the fluorescent powder is changed after the DTAB is added, the luminous performance is obviously enhanced after the DTAB is added, the luminous performance of the fluorescent powder with stronger absorption capacity on blue light is better than that of the DTAB without DTAB, the luminous performance of the fluorescent powder is improved, and the invention provides a luminous performance of a subsequent luminous chip (4) for researching the luminous performance of the luminescent chip on blue light, and provides a luminous material for the MoAB, namely, a luminous chip for improving the luminescent performance of the luminescent chip for a blue light.
drawings
FIG. 1 is an XRD spectrum of LiGd (MoO 4) 2: 15% Eu 3+, a red phosphor obtained in example 9 after adding 60mmol/LDTAB without adding a surfactant.
FIG. 2 is an excitation spectrum of LiGd (MoO 4) 2: 15% Eu 3+, a red phosphor obtained in example 9 without adding a surfactant and after adding 60 mmol/LDTAB.
FIG. 3 is a graph showing the emission spectra of LiGd (MoO 4) 2: 15% Eu 3+, a red phosphor obtained in example 9 without adding a surfactant and after adding 60 mmol/LDTAB.
FIG. 4a is a scanning electron microscope image of the morphology of red phosphor LiGd (MoO 4) 2: 15% Eu 3+ without adding surfactant.
fig. 4b is a partial enlarged view of fig. 4 a.
FIG. 5a is a scanning electron microscope image of the morphology of red phosphor LiGd (MoO 4) 2: 15% Eu 3+ obtained after 60mmol/LDTAB is added.
Fig. 5b is a partial enlarged view of fig. 5 a.
Detailed Description
the invention is described in further detail below with reference to the figures and specific examples.
according to the technical scheme, the red fluorescent powder LiGd (MoO 4) 2: 15% Eu 3+ with DTAB auxiliary enhanced luminescence property is prepared at different calcination temperatures
example 1
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) Dropwise adding the solution A into the solution B, stirring for 60min on a magnetic device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 10min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) And (3) calcining the intermediate product obtained in the step (5) for 4 hours at the temperature of 650 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
Example 2
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) dropwise adding the solution A into the solution B, stirring for 60min on a magnetic device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 10min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and (3) calcining the intermediate product obtained in the step (5) for 4 hours at 635 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
Example 3
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) dropwise adding the solution A into the solution B, stirring for 60min on a magnetic device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 10min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) And (3) calcining the intermediate product obtained in the step (5) for 4 hours at 665 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
example 4
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) Dropwise adding the solution A into the solution B, stirring for 60min on a magnetic force device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3, adding DTAB solid powder into the solution C, and stirring for 10min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) Washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and (3) calcining the intermediate product obtained in the step (5) for 4 hours at 680 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
Example 5
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) dropwise adding the solution A into the solution B, stirring for 60min on a magnetic device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 10min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) Transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and (3) calcining the intermediate product obtained in the step (5) for 4 hours at 700 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
example 6:
preparation of LiGd (MoO 4) 2: 15% Eu 3+
(1) 2.975mmol of Gd (NO 3) 3.6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3 are weighed by using Gd (NO 3) 3.6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials.
(2) dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) dropwise adding the solution A into the solution B, stirring for 80min on a magnetic device at room temperature to obtain a mixed milky solution, and adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a precursor solution;
(4) Transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) Washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+.
the following examples prepare LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescent properties by adding varying amounts of DTAB
Example 7:
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) Dropwise adding the solution A into the solution B, stirring for 80min on a magnetic force device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 15min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 20 mmol/L;
(4) transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) Washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) And calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
Example 8:
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) dropwise adding the solution A into the solution B, stirring for 80min on a magnetic force device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 15min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 40 mmol/L;
(4) Transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) Washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
example 9:
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) dropwise adding the solution A into the solution B, stirring for 80min on a magnetic force device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 15min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) Washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
example 10:
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) Dropwise adding the solution A into the solution B, stirring for 80min on a magnetic force device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 15min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 100 mmol/L;
(4) Transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) And calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
example 11:
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) dropwise adding the solution A into the solution B, stirring for 80min on a magnetic force device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 15min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 140 mmol/L;
(4) Transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
Example 12:
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) Dropwise adding the solution A into the solution B, stirring for 80min on a magnetic force device at room temperature to obtain a mixed milky solution, adjusting the pH of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 15min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 180 mmol/L;
(4) Transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) Washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
FIG. 1 is an XRD spectrum of the red fluorescent powder LiGd (MoO 4) 2: Eu 3+ obtained after the surfactant is not added and 60mmol/LDTAB is added in the above embodiment, compared with a standard card, the XRD spectrum is obviously seen from the diagram, the half-height width of the diffraction peak without the surfactant is narrow, the peak shape is sharp, the prepared sample is a pure-phase substance and has better crystallinity, and after the surfactant is added, each peak is consistent with the standard card, the crystallinity is better, and the pure-phase LiGd (MoO 4) 2: 15% Eu 3+ red fluorescent powder is generated.
FIG. 2 is an excitation spectrum of a red phosphor LiGd (MoO 4) 2: 15% Eu 3+ obtained without adding DTAB and after adding 60mmol/L DTAB, and it is evident from the figure that when the monitoring wavelength is 615nm, all characteristic excitation peaks of Eu 3+ can be monitored at 350-500nm after adding a surfactant, and the intensity of each peak is higher than that of the original surfactant, and the excitation peak at 465nm is strongest, and has strong absorption to blue light, and the absorption to ultraviolet light is also obviously improved compared with that without adding a surfactant.
FIG. 3 is a graph showing the emission spectra of red phosphor LiGd (MoO 4) 2: 15% Eu 3+ obtained without adding DTAB and with 60mmol/L DTAB, when the excitation wavelength is 465nm, the characteristic emission peak of Eu 3+ at 617nm can be observed, and it can be seen from the graph that the emission spectra are similar when DTAB is added and without surfactant, but the emission intensities are different, and the emission intensity is more than twice of the original emission intensity after surfactant is added, therefore, the emission performance is obviously enhanced after surfactant is added, which shows that the phosphor powder with strong blue light absorption capability obtained after surfactant is added has better emission performance than that without surfactant.
FIG. 4 is a scanning electron micrograph of a surfactant-free red phosphor LiGd (MoO 4) 2: 15% Eu 3+, which is a platelet-like structure similar to a oatmeal, and is randomly assembled from irregular platelets, as seen in FIG. 4a, and FIG. 4b is a partial enlargement of FIG. 4a, and which has a surface with some platelets attached, but with few cracks, as seen in FIG. 4 b.
FIG. 5 is a scanning electron microscope image of a red phosphor LiGd (MoO 4) 2: 15% Eu 3+ obtained after 60mmol/LDTAB is added, as can be seen from FIG. 5a, the surface is a smooth sheet-shaped structure after DTAB is added and is formed by randomly combining irregular sheets, FIG. 5b is a partial enlarged view of FIG. 5a, but from FIG. 5b, the surface has more cracks compared with that without the surfactant, the surfactant mainly influences the luminescence performance by changing the morphology, and the luminescence performance of the phosphor is influenced by the morphology, the composition and the synthesis method, therefore, the addition of DTAB influences the morphology of the LiGd (MoO 4) 2: 15% Eu 3+ phosphor, and thus the luminescence performance of the phosphor can be changed
LiGd (MoO 4) 2: 15% Eu 3+ was prepared at different pH values by
example 13:
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) Dropwise adding the solution A into the solution B, stirring for 90min on a magnetic force device at room temperature to obtain a mixed milky solution, and adjusting the pH value of the mixed milky solution to 3 by using a LiOH solution and diluted HNO 3 to obtain a solution C;
(4) Adding DTAB solid powder into the solution C obtained in the step 3, and stirring for 20min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L; transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, and cooling to room temperature to obtain a solution D;
(5) Washing the solution D obtained in the step 4 with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property, and calcining for 4 hours.
example 14:
preparation of LiGd (MoO 4) 2: 15% Eu 3+
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) Dropwise adding the solution A into the solution B, stirring for 90min on a magnetic force device at room temperature to obtain a mixed milky solution, and adjusting the pH value of the mixed milky solution to 5 by using LiOH solution and diluted HNO 3 to obtain a solution C;
(4) adding DTAB solid powder into the solution C obtained in the step 3, and stirring for 20min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L; transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, and cooling to room temperature to obtain a solution D;
(5) Washing the solution D obtained in the step 4 with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property, and calcining for 4 hours.
Example 15:
preparation of LiGd (MoO 4) 2: 15% Eu 3+
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) dropwise adding the solution A into the solution B, stirring for 90min on a magnetic device at room temperature to obtain a mixed milky solution, and adjusting the pH value of the mixed milky solution to 7 by using a LiOH solution and diluted HNO 3 to obtain a solution C;
(4) adding DTAB solid powder into the solution C obtained in the step 3, and stirring for 20min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L; transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, and cooling to room temperature to obtain a solution D;
(5) washing the solution D obtained in the step 4 with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property, and calcining for 4 hours.
Example 16:
preparation of LiGd (MoO 4) 2: 15% Eu 3+
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) Dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) dropwise adding the solution A into the solution B, stirring for 90min on a magnetic force device at room temperature to obtain a mixed milky solution, and adjusting the pH value of the mixed milky solution to 9 by using a LiOH solution and diluted HNO 3 to obtain a solution C;
(4) Adding DTAB solid powder into the solution C obtained in the step 3, and stirring for 20min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L; transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, and cooling to room temperature to obtain a solution D;
(5) washing the solution D obtained in the step 4 with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property, and calcining for 4 hours.
example 17:
preparation of LiGd (MoO 4) 2: 15% Eu 3+
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) dissolving Gd (NO 3) 3.6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
(3) dropwise adding the solution A into the solution B, stirring for 90min on a magnetic force device at room temperature to obtain a mixed milky solution, and adjusting the pH value of the mixed milky solution to 11 by using a LiOH solution and diluted HNO 3 to obtain a solution C;
(4) adding DTAB solid powder into the solution C obtained in the step 3, and stirring for 20min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L; transferring the obtained precursor solution into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, and cooling to room temperature to obtain a solution D;
(5) Washing the solution D obtained in the step 4 with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) And calcining the intermediate product obtained in the step 5 at 650 ℃ in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property, and calcining for 4 hours.
The following examples are prepared by employing different calcination times to prepare LiGd (MoO 4) 2: 15% Eu 3+
Example 18:
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3;
(2) dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) dropwise adding the solution A into the solution B, stirring for 100min on a magnetic device at room temperature to obtain a mixed milky solution, adjusting the pH value of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 30min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) transferring the precursor solution obtained in the step (3) into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 4 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
example 19:
(1) Taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3, and then weighing 60mmol/L of DTAB solid powder;
(2) dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) dropwise adding the solution A into the solution B, stirring for 100min on a magnetic device at room temperature to obtain a mixed milky solution, adjusting the pH value of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 30min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) transferring the precursor solution obtained in the step (3) into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 5 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
example 20:
(1) taking Gd (NO 3) 3 & 6H 2 O, Li 2 MoO 4 and Eu (NO 3) 3 as reaction raw materials, weighing 2.975mmol of Gd (NO 3) 3 & 6H 2 O, 7mmol of Li 2 MoO 4 and 0.525mmol of Eu (NO 3) 3, and then weighing 60mmol/L of DTAB solid powder;
(2) Dissolving Gd (NO 3) 3 & 6H 2 O solid powder in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B.
(3) dropwise adding the solution A into the solution B, stirring for 100min on a magnetic device at room temperature to obtain a mixed milky solution, adjusting the pH value of the mixed milky solution to 7 by using LiOH solution and diluted HNO 3 to obtain a solution C, adding DTAB solid powder into the solution C, and stirring for 30min to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 60 mmol/L;
(4) Transferring the precursor solution obtained in the step (3) into a stainless steel reaction kettle with a p-polyphenyl lining, wherein the volume filling degree of the reaction kettle is 65%, carrying out sealed reaction at 240 ℃ for 24 hours, cooling to room temperature to obtain a solution D, and taking out the solution D;
(5) washing the solution D with water and ethanol alternately for 3 times, centrifuging, and then drying in a drying oven at 70 ℃ for 24 hours to obtain an intermediate product;
(6) and calcining the intermediate product obtained in the step 5 at 650 ℃ for 6 hours in an air atmosphere to obtain a pure-phase substance LiGd (MoO 4) 2: 15% Eu 3+ with enhanced luminescence property.
the above-mentioned embodiments are merely preferred embodiments of the present invention, which is not the only embodiments, and all modifications, equivalents, improvements and the like that do not depart from the spirit and principles of the present invention are intended to be covered by the appended claims.
Claims (9)
1. a preparation method of a DTAB-assisted red fluorescent powder with enhanced luminescence property is characterized by comprising the following steps:
step 1, weighing Gd (NO 3) 3 & 6H 2 O solid powder and Li 2 MoO 4 solid powder and weighing Eu (NO 3) 3 solution respectively according to the stoichiometric ratio of Eu element, Mo element and Gd element in LiGd (MoO 4) 2: 15% Eu 3+;
step 2, dissolving Gd (NO 3) 3.6H 2 O solid powder obtained in the step 1 in deionized water, adding Eu (NO 3) 3 solution to obtain solution A, and dissolving Li 2 MoO 4 solid powder in deionized water to obtain solution B;
step 3, dripping the solution A obtained in the step 2 into the solution B, and uniformly mixing at room temperature;
step 4, adjusting the pH value of the mixed milky white solution obtained in the step 3 to 3-11 to obtain a solution C;
step 5, adding DTAB solid powder into the solution C obtained in the step 4, and uniformly stirring to obtain a precursor solution, wherein the concentration of DTAB in the precursor solution is 20 mmol/L-180 mmol/L;
Step 6, reacting the precursor solution obtained in the step 5 at 240 ℃ for 24 hours, and cooling to room temperature to obtain a solution D;
Step 7, separating the solution D obtained in the step 6, washing, centrifuging and drying to obtain an intermediate product;
And 8, calcining the intermediate product obtained in the step 7 at 635-700 ℃ for 3-5 h in an air atmosphere to obtain the DTAB-assisted red fluorescent powder with enhanced luminescence property.
2. The method for preparing a red fluorescent powder with the DTAB-assisted enhanced luminescence property according to claim 1, wherein in the step 3, the dropping speed of the solution A into the solution B is 2-3 minutes per 5 mL.
3. The method for preparing the DTAB-assisted enhanced luminescence property red fluorescent powder according to claim 1, wherein in the step 3, magnetic stirring is adopted, and the stirring time is 60-100 min.
4. The method for preparing the DTAB-assisted enhanced luminescence red phosphor according to claim 1, wherein in step 4, LiOH and a diluted HNO 3 solution are used to adjust the pH value of the mixed solution.
5. The method for preparing the DTAB-assisted enhanced luminescence property red phosphor according to claim 1, wherein in the step 5, the DTAB addition concentration is 60 mmol/L.
6. the method for preparing the DTAB-assisted enhanced luminescence red phosphor according to claim 1, wherein the precursor solution obtained in the step 5 is subjected to a sealing reaction in a p-polyphenyl lined stainless steel reaction kettle, and the volume filling degree of the reaction kettle is 65%.
7. the method for preparing the DTAB-assisted enhanced luminescence property red phosphor according to claim 1, wherein the solution D obtained in the step 6 is washed by water and ethanol alternately; the centrifugal speed is 10000r/min, and the centrifugal time is 3 min; drying at 70 deg.C for 24 h.
8. The method for preparing a red phosphor with enhanced light emitting property assisted by DTAB according to claim 1, wherein the calcination temperature in step 7 is 650 ℃.
9. A phosphor prepared by the method of any one of claims 1 to 8, wherein the phosphor has a chemical formula of LiGd (MoO 4) 2: 15% Eu 3+.
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| CN102344807A (en) * | 2011-07-29 | 2012-02-08 | 黑龙江大学 | Solvothermal synthesis method for NaLn(MoO4)2 micron crystal |
| CN102942925A (en) * | 2012-06-22 | 2013-02-27 | 四川师范大学 | NaEu(MoO4)2-x(WO4)x-type fluorescent microcrystals and chemical solution preparation method thereof |
| CN108998023A (en) * | 2018-07-13 | 2018-12-14 | 陕西科技大学 | A kind of phosphor host and preparation method thereof |
| CN109266347A (en) * | 2018-11-23 | 2019-01-25 | 陕西科技大学 | It is a kind of can be by red fluorescence powder and preparation method thereof that blue chip effectively excites |
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| CN102344807A (en) * | 2011-07-29 | 2012-02-08 | 黑龙江大学 | Solvothermal synthesis method for NaLn(MoO4)2 micron crystal |
| CN102942925A (en) * | 2012-06-22 | 2013-02-27 | 四川师范大学 | NaEu(MoO4)2-x(WO4)x-type fluorescent microcrystals and chemical solution preparation method thereof |
| CN108998023A (en) * | 2018-07-13 | 2018-12-14 | 陕西科技大学 | A kind of phosphor host and preparation method thereof |
| CN109266347A (en) * | 2018-11-23 | 2019-01-25 | 陕西科技大学 | It is a kind of can be by red fluorescence powder and preparation method thereof that blue chip effectively excites |
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