CN111205865A - Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4Method for producing luminescent material - Google Patents

Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4Method for producing luminescent material Download PDF

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CN111205865A
CN111205865A CN202010097741.1A CN202010097741A CN111205865A CN 111205865 A CN111205865 A CN 111205865A CN 202010097741 A CN202010097741 A CN 202010097741A CN 111205865 A CN111205865 A CN 111205865A
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吕莉
韩梅杏
范红艳
杨楠
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Inner Mongolia University of Technology
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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Abstract

The invention discloses a template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a light material. Dissolving polyvinylpyrrolidone in absolute ethyl alcohol, sequentially adding emulsion-shaped polystyrene spheres, magnesium nitrate hexahydrate, citric acid and manganese nitrate solution, uniformly mixing, dropwise adding the mixture into tetrabutyl titanate ethanol solution, and magnetically stirring for 24 hours; transferring the mixed solution to a reaction kettle, reacting for 12 hours at 160 ℃, and naturally cooling the reaction kettle to room temperature; standing for 12-24 hr, centrifuging the obtained sample, removing clear liquid, and drying at 60 deg.C for 4 hr; calcining the dried sample in a tubular furnace at 250 ℃ for 1 hour, and then heating to 600 ℃ for 4 hours to obtain the hollow spherical Mn4+Doping with Mg2TiO4A luminescent material. The invention prepares hollow spherical Mn4+Doping with Mg2TiO4The luminescent material can improve the crystallinity and stability of the luminescent material and improve the luminescent performance.

Description

Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4Method for producing luminescent material
Technical Field
The invention belongs to the technical field of luminescent material preparation, and particularly relates to a template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a light material.
Background
In recent years, red phosphors having excellent properties have been gradually applied to various fields such as medicine, military, production, scientific research, and daily life. Phase (C)Compared with blue and yellow-green luminescent materials, the development of the red fluorescent material in various fields is not completely mature, and certain performance defects exist, so that the development of a novel red fluorescent material is urgently needed. Among the numerous red luminescent materials, Mn4+Doped into a host material as a luminescent center, and can emit light in a red wavelength range under the excitation of near ultraviolet and blue light in a certain coordination environment. The manganese element in the transition metal elements is rich in the earth crust, and the Mn element4+Has good optical performance and has wider development prospect than the luminescent material doped with rare earth ions. Due to Mg2TiO4Stable crystal structure, good chemical stability, no toxicity, low cost, and suitability for use as Mn4+A doped host material. Usually in order to make Mn4+Can be doped into a matrix material, and the agglomeration of particles is serious and the appearance is not uniform in the preparation process due to high-temperature calcination treatment, so that the application of the catalyst is limited to a certain extent.
During the performance research of functional materials, the properties of the materials are closely related to the particle size and the morphology, so that a great deal of research work is carried out in the field. In the field of luminescence research, researchers also show great interest in the novel properties and potential applications exhibited by luminescent materials of different sizes and different morphologies. Preparation of Mn with controllable size and novel morphology4+The red material as the luminescence center is the focus of the current research. For Mn4+Doping with Mg2TiO4In the preparation process of the luminescent material, Mn is promoted in order to improve the crystallinity of the material4+The luminescent center Mn is easily formed into a hard agglomerated random structure by direct calcination, so that the luminescent center Mn is stable and the luminescent performance is improved4+The utilization efficiency of (2) is lowered and the light emitting performance is affected. The polystyrene sphere synthesis has the advantages of simplicity, easy size control and the like, and the polystyrene sphere is used as a template to prepare the core-shell nano-microsphere and is widely used. If Mn is being prepared4+Doping with Mg2TiO4When the material is prepared, polystyrene balls are used as templates and added into a reaction system to generate Mn4+Doping with Mg2TiO4The precursor can be coated on the surface of the polystyrene sphereThe microspheres with regular appearance and uniform size are easy to form. Application of template polystyrene spheres to Mn4+Doping with Mg2TiO4The preparation method can solve the problems of non-uniform size and serious sintering of the synthesized particles in the traditional preparation process. Adding template material polystyrene ball to prepare Mn at high temperature4+Doping with Mg2TiO4The luminescent material can be removed simultaneously in the process, and no impurity phase is introduced to the system. Removal of polystyrene spheres during high temperature calcination to remove Mn4+Doping with Mg2TiO4The light emitting material forms a hollow structure. The special hollow structure promotes the luminescent material to have the properties of large specific surface area, small density, large internal space, good surface permeability and the like. The polystyrene spheres are used as templates, and not only can hollow structures be formed and the structures are not easy to collapse after high-temperature calcination in the preparation process, but also the improvement of the luminescent property of the material and the improvement of the stability and crystallization property of the material are facilitated, so that a new idea can be provided for the development of luminescent materials. The polystyrene sphere is used as a carrier of the object substance to finally form a hollow structure, and the method has important application prospects in the fields of medicine, material science, dye industry and the like.
Disclosure of Invention
The invention aims to provide a template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a light material. The method takes magnesium nitrate hexahydrate and tetrabutyl titanate as raw materials to prepare Mn4+Doping with Mg2TiO4In the material process, polystyrene balls are added as templates, Mn4+Doping with Mg2TiO4The precursor is coated on the outer surface of the polystyrene sphere. Removing the polystyrene spheres in the inner layer in the subsequent calcining process to finally form the hollow spherical Mn4+Doping with Mg2TiO4A luminescent material.
The technical scheme of the invention is as follows:
step 1, preparing template-polystyrene sphere
Adding 225mL of distilled water into a 500mL three-neck flask and placing the three-neck flask into a constant-temperature water bath at 80 ℃; weighing 1.10g of sodium dodecyl sulfate and 0.625g of sodium bicarbonate, sequentially adding the sodium dodecyl sulfate and the sodium bicarbonate into the three-necked bottle to form a mixed solution, and magnetically stirring for 10 minutes; transferring 27.55mL of styrene solution, dropwise adding the styrene solution into the mixed solution, and magnetically stirring for 1 hour; weighing 0.125g of potassium persulfate, continuously adding the potassium persulfate into the mixed solution in the three-necked bottle, and continuously magnetically stirring for 18 hours to obtain emulsion-shaped polystyrene spheres;
step 2, solvothermal reaction stage
Weighing 1.00g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 45mL of absolute ethyl alcohol, adding 4-8mL of emulsion-shaped polystyrene spheres obtained in the step 1 after magnetic stirring for dissolution, sequentially adding 1.80g of magnesium nitrate hexahydrate, 5.12g of citric acid and 0.25mL of a 50% manganese nitrate solution under the condition of magnetic stirring, and continuously stirring for 10 minutes to form a solution 1; transferring 0.85mL of tetrabutyl titanate solution and 20mL of absolute ethyl alcohol solution, and magnetically stirring and uniformly mixing to form a solution 2; dropwise adding the solution 1 into the solution 2, and continuing to stir for 24 hours by magnetic force; transferring the mixed solution into a 100mL reaction kettle, reacting at 160 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and centrifuging a sample prepared by solvent heating after 12-24 hours; drying at 60 deg.C for 4 hr, and grinding to obtain solid powder;
step 3, high-temperature calcination reaction stage
Calcining solid powder obtained in the solvothermal reaction stage in a tubular furnace, firstly reacting for 1 hour at 250 ℃, then heating to 600 ℃ for reacting for 4 hours, and naturally cooling to obtain Mn4+Doping with Mg2TiO4A luminescent material.
The invention has the following advantages:
1. the invention utilizes emulsion polystyrene balls as templates to obtain Mn4+Doping with Mg2TiO4The luminescent material is in a hollow spherical shape, and has uniform particle size and good controllability.
Preparation of Mn4+Doped MgTiO4Firstly, adding Mn as a template into emulsion-like polystyrene spheres in a solvothermal reaction stage4+Doped MgTiO4The precursor is coated on the outer surface of the polystyrene sphere to form a compact inorganic nanoparticle coating layer. Because the polystyrene ball is used as a template, the size of the polystyrene ball is controllable and largeSmall and uniform, and thus Mn prepared using it as a template4+Doped MgTiO4The precursor particles are uniform in size, and organic-inorganic composite microspheres with regular structures can be formed. Avoid Mn4+Doped MgTiO4Irregular shape of the precursor, uneven size and the like. Mn formation in subsequent high temperature calcination reaction stage4+Doped MgTiO4The polystyrene sphere template can be removed while the luminescent material is used, so that hollow spherical Mn is formed4+Doping with Mg2TiO4A luminescent material. Although the sample is calcined in the preparation process, the phenomenon that the sample is seriously hard agglomerated is not caused. The polystyrene ball is used as a template, the specific surface area of the material is improved, the density is reduced, and more importantly, the Mn is improved4+The utilization rate of the luminescent center improves the luminescent property of the material.
2. The preparation method is simple and easy to implement.
Due to Mn4+Doping with Mg2TiO4The preparation process of the luminescent material comprises a solvothermal reaction stage and a high-temperature calcination reaction stage. Although the emulsion polystyrene spheres and the surfactant polyvinylpyrrolidone are added in the solvothermal reaction process, the sample does not need to be washed to remove impurity phases after the solvothermal reaction, so that the use of solvents such as distilled water and absolute ethyl alcohol is saved, and the preparation time is saved. Because the temperature of the subsequent high-temperature calcination reaction stage is 600 ℃, Mn is obtained in the calcination process4+Doping with Mg2TiO4The luminescent material can also remove the added polystyrene spheres and the surfactant polyvinylpyrrolidone, so that an impurity phase cannot be introduced in the system, and pure-phase Mn can be obtained4+Doping with Mg2TiO4The sample of (1). It is important to improve crystallinity and stability of the luminescent material by calcination, thereby increasing the luminous intensity.
Drawings
FIG. 1 is an X-ray diffraction pattern of samples 1, 2, and 3 prepared in examples 1, 4, and 5 of the present invention.
FIG. 2 is a transmission electron micrograph of samples 1, 2, 3 prepared in examples 1, 4, 5 of the present invention. (a, b) sample 1, (c, d) sample 2, and (e, f) sample 3
FIG. 3 shows the excitation spectra of the prepared samples 1, 2, 3 in examples 1, 4, 5 of the present invention.
FIG. 4 is an emission spectrum of prepared samples 1, 2, and 3 in examples 1, 4, and 5 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited thereto.
Example 1
Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a luminescent material, comprising the steps of:
step 1, preparing template-polystyrene sphere
Adding 225mL of distilled water into a 500mL three-neck flask and placing the three-neck flask into a constant-temperature water bath at 80 ℃; weighing 1.10g of sodium dodecyl sulfate and 0.625g of sodium bicarbonate, sequentially adding the sodium dodecyl sulfate and the sodium bicarbonate into the three-necked bottle to form a mixed solution, and magnetically stirring for 10 minutes; transferring 27.55mL of styrene solution, dropwise adding the styrene solution into the mixed solution, and magnetically stirring for 1 hour; weighing 0.125g of potassium persulfate, continuously adding the potassium persulfate into the mixed solution in the three-necked bottle, and continuously magnetically stirring for 18 hours to obtain emulsion-shaped polystyrene spheres;
step 2, solvothermal reaction stage
Weighing 1.00g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 45mL of absolute ethyl alcohol, adding 4.0mL of emulsion-shaped polystyrene spheres obtained in the step 1 after magnetic stirring for dissolution, sequentially adding 1.80g of magnesium nitrate hexahydrate, 5.12g of citric acid and 0.25mL of a 50% manganese nitrate solution under the condition of magnetic stirring, and continuously stirring for 10 minutes to form a solution 1; transferring 0.85mL of tetrabutyl titanate solution and 20mL of absolute ethyl alcohol solution, and magnetically stirring and uniformly mixing to form a solution 2; dropwise adding the solution 1 into the solution 2, and continuing to stir for 24 hours by magnetic force; transferring the mixed solution into a 100mL reaction kettle, reacting at 160 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and centrifugally separating a sample prepared by solvent heating after 24 hours; drying at 60 deg.C for 4 hr, and grinding to obtain solid powder;
step 3, high-temperature calcination reaction stage
Solid powder obtained in the solvothermal reaction stageCalcining in a tubular furnace, reacting at 250 deg.C for 1 hr, heating to 600 deg.C, reacting for 4 hr, and naturally cooling to obtain Mn4+Doping with Mg2TiO4A luminescent material. The prepared sample was labeled sample 1.
Example 2
Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a luminescent material, comprising the steps of:
step 1, preparing template-polystyrene sphere
Adding 225mL of distilled water into a 500mL three-neck flask and placing the three-neck flask into a constant-temperature water bath at 80 ℃; weighing 1.10g of sodium dodecyl sulfate and 0.625g of sodium bicarbonate, sequentially adding the sodium dodecyl sulfate and the sodium bicarbonate into the three-necked bottle to form a mixed solution, and magnetically stirring for 10 minutes; transferring 27.55mL of styrene solution, dropwise adding the styrene solution into the mixed solution, and magnetically stirring for 1 hour; weighing 0.125g of potassium persulfate, continuously adding the potassium persulfate into the mixed solution in the three-necked bottle, and continuously magnetically stirring for 18 hours to obtain emulsion-shaped polystyrene spheres;
step 2, solvothermal reaction stage
Weighing 1.00g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 45mL of absolute ethyl alcohol, adding 6.0mL of emulsion-shaped polystyrene spheres obtained in the step 1 after magnetic stirring for dissolution, sequentially adding 1.80g of magnesium nitrate hexahydrate, 5.12g of citric acid and 0.25mL of a 50% manganese nitrate solution under the condition of magnetic stirring, and continuously stirring for 10 minutes to form a solution 1; transferring 0.85mL of tetrabutyl titanate solution and 20mL of absolute ethyl alcohol solution, and magnetically stirring and uniformly mixing to form a solution 2; dropwise adding the solution 1 into the solution 2, and continuing to stir for 24 hours by magnetic force; transferring the mixed solution into a 100mL reaction kettle, reacting at 160 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and centrifugally separating a sample prepared by solvent heating after 24 hours; drying at 60 deg.C for 4 hr, and grinding to obtain solid powder;
step 3, high-temperature calcination reaction stage
Calcining solid powder obtained in the solvothermal reaction stage in a tubular furnace, firstly reacting at 250 ℃ for 1 hour, then heating to 600 ℃ for reacting for 4 hours, and naturally cooling to obtain Mn4+Doping with Mg2TiO4A luminescent material.
Example 3
Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a luminescent material, comprising the steps of:
step 1, preparing template-polystyrene sphere
Adding 225mL of distilled water into a 500mL three-neck flask and placing the three-neck flask into a constant-temperature water bath at 80 ℃; weighing 1.10g of sodium dodecyl sulfate and 0.625g of sodium bicarbonate, sequentially adding the sodium dodecyl sulfate and the sodium bicarbonate into the three-necked bottle to form a mixed solution, and magnetically stirring for 10 minutes; transferring 27.55mL of styrene solution, dropwise adding the styrene solution into the mixed solution, and magnetically stirring for 1 hour; 0.125g of potassium persulfate is weighed and continuously added into the mixed solution of the three-necked flask, and the magnetic stirring is continuously carried out for 18 hours, so as to obtain the emulsion-shaped polystyrene spheres.
Step 2, solvothermal reaction stage
Weighing 1.00g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 45mL of absolute ethyl alcohol, adding 8.0mL of emulsion-shaped polystyrene spheres obtained in the step 1 after magnetic stirring for dissolution, sequentially adding 1.80g of magnesium nitrate hexahydrate, 5.12g of citric acid and 0.25mL of a 50% manganese nitrate solution under the condition of magnetic stirring, and continuously stirring for 10 minutes to form a solution 1; transferring 0.85mL of tetrabutyl titanate solution and 20mL of absolute ethyl alcohol solution, and magnetically stirring and uniformly mixing to form a solution 2; dropwise adding the solution 1 into the solution 2, and continuing to stir for 24 hours by magnetic force; transferring the mixed solution into a 100mL reaction kettle, reacting at 160 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and centrifugally separating a sample prepared by solvent heating after 24 hours; drying at 60 deg.C for 4 hr, and grinding to obtain solid powder;
step 3, high-temperature calcination reaction stage
Calcining solid powder obtained in the solvothermal reaction stage in a tubular furnace, firstly reacting at 250 ℃ for 1 hour, then heating to 600 ℃ for reacting for 4 hours, and naturally cooling to obtain Mn4+Doping with Mg2TiO4A luminescent material.
Example 4
Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a luminescent material, comprising the steps of:
step 1, preparing template-polystyrene sphere
Adding 225mL of distilled water into a 500mL three-neck flask and placing the three-neck flask into a constant-temperature water bath at 80 ℃; weighing 1.10g of sodium dodecyl sulfate and 0.625g of sodium bicarbonate, sequentially adding the sodium dodecyl sulfate and the sodium bicarbonate into the three-necked bottle to form a mixed solution, and magnetically stirring for 10 minutes; transferring 27.55mL of styrene solution, dropwise adding the styrene solution into the mixed solution, and magnetically stirring for 1 hour; weighing 0.125g of potassium persulfate, continuously adding the potassium persulfate into the mixed solution in the three-necked bottle, and continuously magnetically stirring for 18 hours to obtain emulsion-shaped polystyrene spheres;
step 2, solvothermal reaction stage
Weighing 1.00g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 45mL of absolute ethyl alcohol, adding 4.0mL of emulsion-shaped polystyrene spheres obtained in the step 1 after magnetic stirring for dissolution, sequentially adding 1.80g of magnesium nitrate hexahydrate, 5.12g of citric acid and 0.25mL of a 50% manganese nitrate solution under the condition of magnetic stirring, and continuously stirring for 10 minutes to form a solution 1; transferring 0.85mL of tetrabutyl titanate solution and 20mL of absolute ethyl alcohol solution, and magnetically stirring and uniformly mixing to form a solution 2; dropwise adding the solution 1 into the solution 2, and continuing to stir for 24 hours by magnetic force; transferring the mixed solution into a 100mL reaction kettle, reacting at 160 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and centrifugally separating a sample prepared by solvent heating after 12 hours; drying at 60 deg.C for 4 hr, and grinding to obtain solid powder;
step 3, high-temperature calcination reaction stage
Calcining solid powder obtained in the solvothermal reaction stage in a tubular furnace, firstly reacting at 250 ℃ for 1 hour, then heating to 600 ℃ for reacting for 4 hours, and naturally cooling to obtain Mn4+Doping with Mg2TiO4A luminescent material. The prepared sample was labeled sample 2.
Example 5
Preparation of Mn without template4+Doping with Mg2TiO4A method of emitting a luminescent material, comprising the steps of:
step 1 Solvothermal reaction stage
Weighing 1.00g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 45mL of absolute ethyl alcohol, stirring the mixture magnetically to dissolve the polyvinylpyrrolidone, sequentially adding 1.80g of magnesium nitrate hexahydrate, 5.12g of citric acid and 0.25mL of a 50% manganese nitrate solution by mass, and continuously stirring the mixture for 10 minutes to form a solution 1; transferring 0.85mL of tetrabutyl titanate solution and 20mL of absolute ethyl alcohol solution, and magnetically stirring and uniformly mixing to form a solution 2; dropwise adding the solution 1 into the solution 2, and continuing to stir for 24 hours by magnetic force; transferring the mixed solution into a 100mL reaction kettle, reacting at 160 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and centrifugally separating a sample prepared by solvent heating after 24 hours; drying at 60 deg.C for 4 hr, and grinding to obtain solid powder;
step 2 high temperature calcination reaction stage
Calcining solid powder obtained in the solvothermal reaction stage in a tubular furnace, firstly reacting at 250 ℃ for 1 hour, then heating to 600 ℃ for reacting for 4 hours, and naturally cooling to obtain Mn4+Doping with Mg2TiO4A luminescent material. The prepared sample was labeled sample 3.
Example 5 (sample 3) in comparison to example 1 (sample 1) and example 4 (sample 2), no emulsion-like polystyrene spheres were added as templates during the preparation of the samples. From the X-ray diffraction pattern analysis of FIG. 1, it can be seen that the X-ray diffraction peaks and Mg of the samples 1, 2 and 32TiO4No impurity phase was found to exist in the case of the standard card (JCPDS No. 01-073-1723). All three samples are indicated to be phase pure Mg2TiO4Sample Mn4+Does not change its crystal structure. It can be seen from the transmission electron micrograph of fig. 2 that both sample 1 and sample 2 have prepared hollow spherical samples with uniform particle size. Sample 3, however, exhibited non-uniform particle size, poor dispersion properties, and agglomeration. As can be seen from the analysis of the luminescence properties of the samples, samples 1, 2 and 3 all had Mn4+The characteristic d-d characteristic transition peak appears in the excitation spectrum of FIG. 3, indicating Mn4+Doping into Mg2TiO4Sample, but Mn of sample 34+The excitation peak intensity was weaker than that of sample 1 and sample 2. As can be seen from the emission spectrum of FIG. 4, the emission peak positions of the three samples are 660 nm, which are located in the red light emission region. Indicating that the sample was capable of emitting red light. But samples 1 and 2 were found to be stronger than sample 3 when comparing the emission peak intensities of the three samples. In view of the above-mentioned analysis, it can be seen that,hollow spherical Mn prepared by template method4+Doped Mg2TiO4The luminescent material has the advantages of controllable appearance, uniform size and good dispersibility, and more importantly, the luminescent property is improved, so the material has application prospect in the field of luminescence.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and it will be apparent to those skilled in the art that various modifications can be made in the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (1)

1. Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4A method of emitting a luminescent material, characterized by:
step 1, preparing template-polystyrene sphere
Adding 225mL of distilled water into a 500mL three-neck flask and placing the three-neck flask into a constant-temperature water bath at 80 ℃; weighing 1.10g of sodium dodecyl sulfate and 0.625g of sodium bicarbonate, sequentially adding the sodium dodecyl sulfate and the sodium bicarbonate into the three-necked bottle to form a mixed solution, and magnetically stirring for 10 minutes; transferring 27.55mL of styrene solution, dropwise adding the styrene solution into the mixed solution, and magnetically stirring for 1 hour; weighing 0.125g of potassium persulfate, adding into the mixed solution in the three-necked flask, and continuing to magnetically stir for 18 hours to obtain emulsion-shaped polystyrene spheres;
step 2, solvothermal reaction stage
Weighing 1.00g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 45mL of absolute ethyl alcohol, adding 4-8mL of emulsion-shaped polystyrene spheres obtained in the step 1 after magnetic stirring for dissolution, sequentially adding 1.80g of magnesium nitrate hexahydrate, 5.12g of citric acid and 0.25mL of a 50% manganese nitrate solution under the condition of magnetic stirring, and continuously stirring for 10 minutes to form a solution 1; transferring 0.85mL of tetrabutyl titanate solution and 20mL of absolute ethyl alcohol solution, and magnetically stirring and uniformly mixing to form a solution 2; dropwise adding the solution 1 into the solution 2, and continuing to stir for 24 hours by magnetic force; transferring the mixed solution into a 100mL reaction kettle, reacting at 160 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and centrifuging a sample prepared by solvent heating after 12-24 hours; drying at 60 deg.C for 4 hr, and grinding to obtain solid powder;
step 3, high-temperature calcination reaction stage
Calcining solid powder obtained in the solvothermal reaction stage in a tubular furnace, firstly reacting for 1 hour at 250 ℃, then heating to 600 ℃ for reacting for 4 hours, and naturally cooling to obtain Mn4+Doping with Mg2TiO4A luminescent material.
CN202010097741.1A 2020-02-17 2020-02-17 Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4Method for producing luminescent material Withdrawn CN111205865A (en)

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Citations (2)

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Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN1974404A (en) * 2006-12-14 2007-06-06 天津理工大学 Prepn process of nanometer titania ring
CN102198385A (en) * 2011-05-23 2011-09-28 同济大学 Preparation method of magnetic fluorescence dual-function silicon oxide hollow microspheres

Non-Patent Citations (2)

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Title
LI LV ET AL.,: ""Inducing luminescent properties of Mn4+ in magnesium titanate systems: An experimental and theoretical approach"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
YU GAO ET AL.,: ""Facile synthesis of hollow microspherical YPO4: Eu3+/Tb3+ using polystyrene spheres as sacrificial template and its photoluminescent properties"", 《MICRO & NANO LETTERS》 *

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