CN111718712A - Eu (Eu)3+/Tb3+Co-doped SiO2Ribbon fiber film luminescent material and preparation method thereof - Google Patents
Eu (Eu)3+/Tb3+Co-doped SiO2Ribbon fiber film luminescent material and preparation method thereof Download PDFInfo
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- CN111718712A CN111718712A CN201910210754.2A CN201910210754A CN111718712A CN 111718712 A CN111718712 A CN 111718712A CN 201910210754 A CN201910210754 A CN 201910210754A CN 111718712 A CN111718712 A CN 111718712A
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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Abstract
The invention discloses Eu3+/Tb3+Co-doped SiO2A banded fiber membrane luminescent material and a preparation method thereof belong to the technical field of inorganic luminescent materials. The method takes tetraethoxysilane and rare earth nitrate as raw materials, and concretely comprises glacial acetic acid, deionized water and Eu (NO)3)3、Tb(NO3)3And adding tetraethoxysilane and polyvinylpyrrolidone into the N, N-dimethylformamide mixed solution in sequence to obtain spinning solution, and synthesizing PVP/SiO by using an electrostatic spinning technology2:xEu3+,yTb3+Calcining the precursor fiber film at high temperature in air atmosphere to remove the organic template, and finally preparing Eu3+/Tb3+Co-doped SiO2The ribbon fiber film luminescent material. Eu prepared by the invention3+/Tb3+Co-doped SiO2The ribbon fiber film luminescent material has a fiber diameter of 0.7-1.2 μm, and has bright red, orange and green luminescence under the excitation of ultraviolet lightHas wide application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic luminescent materials, and particularly relates to Eu3+/Tb3+Co-doped SiO2A banded fiber film luminescent material and a preparation method thereof.
Background
The rare earth doped luminescent material has important application value in the fields of illumination, biological imaging and the like, and is a hot spot of research of people. The silicon dioxide has the advantages of stable chemical property, excellent mechanical property, higher transparency and the like due to the unique three-dimensional network structure, and is an excellent rare earth doped matrix material. However, the rare earth doped silica material prepared by the traditional sol-gel method is mainly a spherical or massive powder product, has a single appearance and is difficult to recover, which undoubtedly limits the further application of the rare earth doped silica material, so how to prepare a novel rare earth doped silica material with a regular appearance and easy recovery is a problem to be solved by researchers.
In addition, the rare earth doped silica luminescent material prepared at present is mainly rare earth ion single doped silica, and has single luminescent color and narrow application range. For example, Liu Long shadow is used to prepare Eu by sol-gel method3+Doped SiO2Sol (SiO)2And Eu3+Doped SiO2Preparation and Performance Studies of antireflection films [ D]Zhejiang university, 2014). Slow light blue et al prepared Ce by sol-gel method3+Doped nano SiO2Material (preparation of Ce by sol-gel method)3+Doped nano SiO2Material photoluminescence study [ J]Optics journal, 2005, 25(8): 1081-. In order to achieve the purpose of multi-color luminescence of rare earth doped luminescent materials, and to widen the color gamut, researchers have begun to adopt a method of co-doping two kinds of rare earth ions. For example, Ntwaeaborowa prepared Ce using a sol-gel method3+，Eu3+Co-doped SiO2Phosphor (phosphor of cerium-europeum co-doped SiO)2phosphor prepared by a sol-gel process[J].Surface&Interface Analysis, 2010, 38(4): 458-. However, there has been no discussion of Eu up to now3+，Tb3+Report of co-doped silica fibers. This is mainly because trivalent terbium is easily oxidized into tetravalent terbium by calcining the sample in a high-temperature air atmosphere, and therefore, when green light emission of trivalent terbium is utilized, calcining the sample in a reducing atmosphere is mostly employed. However, trivalent europium having red emission is easily reduced to divalent europium having blue emission in a reducing atmosphere, and thus trivalent europium and trivalent terbium are hardly coexisted, for example, Eu and Tb co-doped SiO prepared in a reducing atmosphere by Hudaoyun et al2In the gel, Eu is mainly in +2 valence state. Therefore, how to realize that the valence states of the trivalent europium and the trivalent terbium are not changed in the high-temperature calcination process and the trivalent europium and the trivalent terbium are simultaneously doped in the silicon dioxide with regular shapes to adjust the luminescence of the material is the problem solved by the patent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides Eu3+/Tb3+Co-doped SiO2The ribbon fiber film luminescent material and the preparation method thereof can effectively solve the defects that the product has single appearance and is mostly a powder sample. Meanwhile, because a large number of high-molecular polymer templates exist in the precursor spinning fiber and strong interaction exists between the templates and silicon dioxide, after the templates are removed by high-temperature calcination, a large number of defect centers are introduced into the fiber, which is favorable for preventing the oxidation of trivalent terbium, so that trivalent europium with red light emission and trivalent terbium with green light emission simultaneously exist in SiO2In the ribbon fiber film, the color gamut of the material is widened.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problem is as follows:
eu (Eu)3+/Tb3+Co-doped SiO2The ribbon fiber film luminescent material has a fiber diameter of 0.7-1.2 μm and a chemical formula of SiO2:xEu3+,yTb3+Wherein SiO is2Is a matrix, Eu3+And Tb3+Is a luminous center, x and y represent the mole number of rare earth ion doping, x is more than or equal to 0 and less than or equal to 0.04, y is more than or equal to 0 and less than or equal to 0.04, and x + y =0.04, the color of the emitted light of the fiber film under the excitation of ultraviolet light realizes the color from red and orange under the excitation of the ultraviolet light by adjusting the doping ratio of x and yThe controllable adjustment to green color is realized, and the color gamut range is wider.
Eu (Eu)3+/Tb3+Co-doped SiO2The preparation method of the banded fiber membrane luminescent material specifically comprises the following steps:
(1) adding glacial acetic acid, deionized water and Eu (NO)3)3、Tb(NO3)3Adding tetraethoxysilane into the mixed solution of N, N-dimethylformamide, and magnetically stirring for 15-30 min at room temperature to obtain a clear transparent mixed solution; wherein the molar ratio of Eu to Si is (0-4): 100, the molar ratio of Tb to Si is (0-4): 100, and the sum of the molar numbers of Eu and Tb doping is 0.04;
(2) adding polyvinylpyrrolidone (molecular weight of 1,300,000) into the mixed solution, and magnetically stirring for 40-50 min at room temperature to obtain viscous and transparent electrostatic spinning solution; wherein the concentration of the polyvinylpyrrolidone is (0.0625-0.1) g/mL;
(3) electrostatic spinning is carried out by using electrostatic spinning equipment under the condition of proper parameters, and PVP/SiO is obtained on receiving equipment after 30min of spinning2:xEu3+,yTb3+A precursor fiber film;
(4) mixing PVP/SiO2:xEu3+,yTb3+The precursor fiber film is taken off from the receiving equipment, folded and placed in a 50mL large crucible, placed in a muffle furnace, calcined at high temperature for 2-3 h in air atmosphere, the organic components such as the template and the like are removed, and finally Eu is prepared3+/Tb3+Doped SiO2The ribbon fiber film luminescent material.
The invention provides Eu3+/Tb3+Co-doped SiO2The banded fiber film luminescent material and the preparation method thereof have the following beneficial effects:
1. the invention adopts the electrostatic spinning technology, overcomes the defects of high energy consumption, high temperature and high pressure environment required by a high temperature solid phase method and a hydrothermal method adopted by the conventional fluorescent powder, and realizes the purposes of low energy consumption, easy operation, green and environment-friendly preparation of the high-quality rare earth luminescent material;
2. eu prepared by the invention3+/Tb3+Co-doped SiO2Ribbon fiberThe film luminescent material has obvious fiber film appearance, overcomes the defect that the powder material is difficult to recover, and has uniform product fiber size and excellent luminescent performance;
3. the prepared silicon dioxide spinning fiber has more defects inside, and can effectively avoid the oxidation reaction of trivalent terbium ions in high-temperature air atmosphere, thereby avoiding the fluorescence quenching effect of tetravalent terbium and improving the luminous intensity of the prepared fiber film;
4. by adjusting the molar doping concentration of the trivalent europium and the trivalent terbium, the controllable adjustment of the luminescent color from red, orange to green is realized, and the color gamut range of the luminescent material is widened.
Drawings
FIG. 1 is a SiO solid prepared in example 2 of the present invention2:0.01Eu3+,0.03Tb3+Macroscopic electron micrographs (FIG. 1 a) and microscopic scanning electron micrographs (FIG. 1 b) of the fiber film luminescent material.
FIG. 2 is SiO prepared according to example 2 of the present invention2:0.01Eu3+,0.03Tb3+And the X-ray powder diffraction spectrum of the fiber film luminescent material.
FIG. 3 shows SiO prepared in examples 1, 2 and 5 of the present invention2:xEu3+,yTb3+Fluorescence spectrum of the fiber film luminescent material.
FIG. 4 shows SiO prepared in examples 1, 2 and 5 of the present invention2:xEu3+,yTb3+CIE chromaticity diagram of the fiber film luminescent material.
Detailed Description
The technical solution of the present invention is described in detail by the following specific examples, all of which are operated according to the operation procedures described in the present invention. The electrostatic spinning equipment used by the invention is produced by Beijing Yongkang Leye science and technology development Limited company, and the model is SS series 2535D.
Example 1
(1) Selecting Eu with the purity of 99.99 percent2O3And Tb4O7Dissolving the powder in aqueous solution of nitric acid, heating and stirring with magnetic stirrer to remove excessive nitric acidAnd moisture to obtain molten Eu (NO)3)3And Tb (NO)3)3Cooling and grinding to obtain Eu (NO)3)3And Tb (NO)3)3Powder;
(2) 0.123gTb (NO)3)3The powder was added to a mixed solution of 2mL glacial acetic acid, 1mL deionized water and 8mL N, N-Dimethylformamide (DMF), stirred for 10min and the powder dissolved to give a homogeneous clear solution. Then 2mL of tetraethyl orthosilicate (TEOS) was added and magnetically stirred at room temperature (22 ℃) for 30min (400 rpm) to obtain a clear and transparent mixed solution. At this time, the molar ratio of Tb to Si was 4: 100, volume ratio of ethyl orthosilicate, glacial acetic acid, deionized water and DMF is 2: 2: 1: 8;
(3) adding 1g polyvinylpyrrolidone powder (PVP, molecular weight 1,300,000) with concentration of 0.0769g/mL into the above clear solution, and magnetically stirring at room temperature (22 deg.C) for 40min to obtain viscous clear electrostatic spinning solution;
(4) measuring 2mL of electrostatic spinning solution by using a 5mL syringe, placing on electrostatic spinning equipment, wrapping an aluminum foil on a roller receiving device to serve as a cathode (the rotating speed is 300 revolutions per minute), connecting a 20G stainless steel needle (the inner diameter is 0.61 mm) to the syringe to serve as an anode, switching on a 20kV high-voltage power supply between the anode and the cathode, carrying out electrostatic spinning at the injection flow rate of 1.5mL/h, spinning for 30min, and obtaining PVP/SiO on the receiving device2:0.04Tb3+A precursor fiber film;
(5) taking off the precursor fiber film from the aluminum foil, folding and placing the precursor fiber film into a 50mL large crucible, placing the crucible in a muffle furnace, calcining for 2h at 700 ℃ in the air atmosphere, wherein the heating rate is 2 ℃/min, and finally preparing SiO2:0.04Tb3+The fiber film luminescent material.
For SiO prepared in this example2:0.04Tb3+The fiber film luminescent material is subjected to fluorescence spectrum test, and the result is shown in fig. 3 and 4, under the excitation of ultraviolet light of 377nm, the main emission peak of the prepared fiber film sample is located 541nm, and the chromaticity coordinates (x, y) = (0.2586, 0.4433) are located in the green color gamut.
Example 2
Except as explained below, 0.123gTb (NO) was added in the same manner as in example 13)3The powder was adjusted to 0.030gEu (NO)3)3And 0.093gTb (NO)3)3Powder, the molar ratio of Eu to Si being 1: 100, molar ratio of Tb to Si of 3: 100, final preparation of SiO2:0.01Eu3+,0.03Tb3+The fiber film luminescent material.
For SiO prepared in this example2:0.01Eu3+,0.03Tb3+The fiber film luminescent material is subjected to macroscopic photographing and microscopic scanning electron microscope testing, the result is shown in figure 1, the prepared material presents the fiber film appearance macroscopically, is an obvious belt-shaped structure microscopically, has the diameter of 0.7-1.2 mu m, and has a smooth surface.
For SiO prepared in this example2:0.01Eu3+,0.03Tb3+The fiber film luminescent material is subjected to an X-ray powder diffraction test, and the result is shown in fig. 2, the prepared fiber film luminescent material only has a wide diffraction peak around 2 θ =23 °, and the diffraction peak is consistent with the diffraction peak of amorphous silica, which indicates that no other impurity phase is introduced to generate due to the doping of rare earth ions.
For SiO prepared in this example2:0.01Eu3+,0.03Tb3+The fiber film luminescent material is subjected to fluorescence spectrum test, and as shown in fig. 3 and 4, under the excitation of ultraviolet light with a single wavelength of 377nm, the prepared fiber film sample has two main emission peaks respectively at 541nm and 614nm, and chromaticity coordinates (x, y) = (0.5725, 0.3835) thereof are in an orange color gamut.
Example 3
Except as explained below, 0.123gTb (NO) was added in the same manner as in example 13)3The powder was adjusted to 0.060gEu (NO)3)3And 0.062gTb (NO)3)3Powder, the molar ratio of Eu to Si being 2: 100, molar ratio of Tb to Si is 2: 100, final preparation of SiO2:0.02Eu3+,0.02Tb3+The fiber film luminescent material.
Example 4
Except as explained below, 0.123gT was added in the same manner as in example 1b(NO3)3The powder was adjusted to 0.090gEu (NO)3)3And 0.031gTb (NO)3)3Powder, the molar ratio of Eu to Si in this case being 3: 100, molar ratio of Tb to Si of 1: 100, final preparation of SiO2:0.03Eu3+,0.01Tb3+The fiber film luminescent material.
Example 5
Except as explained below, 0.123gTb (NO) was added in the same manner as in example 13)3The powder was adjusted to 0.121gEu (NO)3)3Powder, the molar ratio of Eu to Si in this case being 4: 100, final preparation of SiO2:0.04Eu3+The fiber film luminescent material.
For SiO prepared in this example2:0.04Eu3+The fiber film luminescent material is subjected to fluorescence spectrum test, and the result is shown in fig. 3 and 4, under the excitation of ultraviolet light at 391nm, the prepared fiber film sample has a main emission peak at 614nm, and chromaticity coordinates (x, y) = (0.5581, 0.3250) thereof are in a red color gamut.
Example 6
The procedure of example 1 was repeated except that 8mL of N, N-dimethylformamide and 2mL of tetraethyl orthosilicate were changed to 6mL of N, N-dimethylformamide and 1mL of tetraethyl orthosilicate, i.e., the volume ratio of tetraethyl orthosilicate, glacial acetic acid, deionized water and DMF was 1: 2: 1: 6, the concentration of polyvinylpyrrolidone is 0.1 g/mL.
Example 7
The procedure of example 1 was repeated except that 8mL of N, N-dimethylformamide and 2mL of tetraethyl orthosilicate were changed to 10mL of N, N-dimethylformamide and 3mL of tetraethyl orthosilicate, i.e., the volume ratio of tetraethyl orthosilicate, glacial acetic acid, deionized water and DMF was 3: 2: 1: 10, the concentration of the polyvinylpyrrolidone is 0.0625 g/mL.
Example 8
Except for the following, the rotation speed of the receiver was changed to 500 rpm in the same manner as in example 1.
Example 9
Except for the following description, the flow rate of the injection was changed to 1.5mL/h and the rotational speed was changed to 3.0mL/h in the same manner as in example 1.
Example 10
The calcination was carried out in the same manner as in example 1 except that the calcination was carried out at 700 ℃ for 2 hours and at 500 ℃ for 3 hours.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. Eu (Eu)3+/Tb3+Co-doped SiO2The ribbon fiber film luminescent material has a fiber diameter of 0.7-1.2 μm and a chemical formula of SiO2:xEu3+,yTb3+Wherein, SiO2Is a matrix, Eu3+And Tb3+The fiber film is a luminescent center, x and y represent the mole number of rare earth ion doping, x is more than or equal to 0 and less than or equal to 0.04, y is more than or equal to 0 and less than or equal to 0.04, and x + y =0.04, and by adjusting the doping proportion of x and y, the color of the emitted light of the fiber film under the excitation of ultraviolet light realizes the controllable adjustment from red, orange to green, and the color gamut range is wider.
2. Eu according to claim 13+/Tb3+Co-doped SiO2The preparation method of the banded fiber membrane luminescent material is characterized by comprising the following steps:
(1) adding glacial acetic acid, deionized water and Eu (NO)3)3、Tb(NO3)3Adding tetraethoxysilane into the mixed solution of the N, N-dimethylformamide, and magnetically stirring for 15-30 min at room temperature to obtain a clear and transparent mixed solution; wherein the molar ratio of Eu to Si is (0-4): 100, the molar ratio of Tb to Si is (0-4): 100, and the sum of the molar numbers of Eu and Tb doping is 0.04;
(2) adding polyvinylpyrrolidone (molecular weight of 1,300, 000) into the mixed solution, and magnetically stirring at room temperature for 40-50 min to obtain a viscous and transparent electrostatic spinning solution; wherein the concentration of the polyvinylpyrrolidone is (0.0625-0.1) g/mL;
(3) electrostatic spinning is carried out by using electrostatic spinning equipment under the condition of proper parameters, and PVP/SiO is obtained on receiving equipment after 30min of spinning2:xEu3+,yTb3+A precursor fiber film;
(4) mixing PVP/SiO2:xEu3+,yTb3+The precursor fiber film is taken off from the receiving equipment, folded and placed into a 50mL large crucible, placed in a muffle furnace, and calcined at high temperature for 2-3 h in air atmosphere, and finally Eu is prepared3+/Tb3+Co-doped SiO2The ribbon fiber film luminescent material.
3. The method according to claim 2, wherein in the step (1), the volume ratio of the tetraethoxysilane to the glacial acetic acid to the deionized water to the DMF is (1-3): 2: 1: (6-10).
4. The method according to claim 2, wherein in step (1), Eu (NO)3)3And Tb (NO)3)3Is Eu2O3And Tb4O7Dissolving the powder in aqueous solution of nitric acid, evaporating to dryness, and grinding to obtain Eu (NO)3)3And Tb (NO)3)3A crystalline powder.
5. The method of claim 2, wherein the solution is stirred in steps (1) and (2) at room temperature at a stirring rate of 400 rpm.
6. The method according to claim 2, wherein the receiving device in step (3) is a roller receiver, the rotation speed is 300-500 rpm, the voltage is 15-25 kV, and the flow rate of the injection is (1.5-3) mL/h.
7. The method of claim 2, wherein the PVP/SiO solid used in step (4)2:xEu3+,yTb3+Calcining the precursor fiber film in an air atmosphere at the calcining temperature of 500-700 DEG CThe temperature rise rate is 2-5 ℃/min.
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| CN115043409A (en) * | 2021-12-29 | 2022-09-13 | 渤海大学 | Tb 3+ Doped SiO 2 Nanowire and nanocrystal material and preparation method |
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| CN105088418A (en) * | 2015-09-17 | 2015-11-25 | 吉林大学 | Preparation method of one-dimensional SiO<2>: Eu<3+> fiber luminescent material with dimension controllable |
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Application publication date: 20200929 |