CN111003944A - Rare earth ion Eu3+Doping with Bi3LaTi3O12Ferroelectric glass-ceramic up-conversion luminescent powder - Google Patents
Rare earth ion Eu3+Doping with Bi3LaTi3O12Ferroelectric glass-ceramic up-conversion luminescent powder Download PDFInfo
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0072—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition having a ferro-electric crystal phase
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- 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
Abstract
The invention provides rare earth ion Eu3+ doped Bi3LaTi3O12 ferroelectric glass-ceramic up-conversion luminescent powder, which comprises the following components: bismuth lanthanum titanate Bi3LaTi3O12 ferroelectric microcrystalline glass xEu3+, wherein x is 1-10 mol%. The invention uses tartaric acid as complexing agent and glycol as cross-linking agent to obtain uniform and stable sol, the used equipment is simple, the operation is easy, the heating speed and time can be controlled to adjust the viscosity of the sol, the preparation method has good process performance, is simple and the product quality is easy to control. May be used in a variety of photoluminescent device applications.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a combination of a photoluminescent material and a ferroelectric glass ceramic material, rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12And (3) converting the luminescent powder on the ferroelectric glass ceramics.
Background
At present, rare earth ion doped up-conversion nano materials are applied to numerous fields such as biomedicine, photocatalysis, three-dimensional display, photovoltaics and the like by using unique up-conversion spectral characteristics. However, the upconversion materials still face great challenges in many practical applications, mainly due to the low luminescence efficiency and small absorption cross section of the existing upconversion materials[15-18]. The high efficiency upconverters of interest have focused primarily on some trivalent rare earth ions, such as Er, with matched intermediate energy levels3+、Tm3+、Ho3+Ion plasma (in Yb)3+As a sensitizer) and the f-f electric dipole transition of these trivalent rare earth ions is an astronomical forbidden transition, with the common problem of smaller absorption cross section and narrower excitation band. Meanwhile, the rare earth ions capable of generating up-conversion luminescence often have richer and dense intermediate state energy levels, so that the coupling between excited state electrons and lattices, namely electron-phonon coupling, is enhanced, and the up-conversion luminescence efficiency is not ideal; the most efficient up-conversion luminescent material currently recognized is NaYF with hexagonal phase4:Yb3+,Er3+The luminescent quantum efficiency of the system is still lower than 10%.
With the rise of nano materials and nano technology, ferroelectric crystal grains are separated out from a glass matrix to form the ferroelectric glass ceramic material, on one hand, the local field of rare earth ions is changed by high-concentration doping of the rare earth ions and ferroelectric polarization, and on the other hand, the ferroelectric glass ceramic material combines the characteristics of large absorption cross section and high luminous efficiency of crystals, easy preparation of glass, excellent physical and chemical stability, mechanical property and the like. The invention utilizes rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Ferroelectric glass ceramics, and the preparation methodThe method has good and simple process performance and easy control of product quality.
Disclosure of Invention
The invention aims to provide rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12And (3) converting the luminescent powder on the ferroelectric glass ceramics.
The rare earth ion Eu provided by the invention3+Bismuth lanthanum titanate doped Bi3LaTi3O12The ferroelectric glass-ceramic up-conversion luminescent powder material comprises the following components:
bismuth lanthanum titanate Bi3LaTi3O12Ferroelectric glass ceramics x Eu3+
Wherein x is 1% -10% mol, and the numbers at the lower right corner of the elements represent the mol ratio of each corresponding element.
The preparation method provided by the invention specifically comprises the following steps:
the rare earth ion Eu according to claim 13+Bismuth lanthanum titanate doped Bi3LaTi3O12The preparation method of the (BLT) ferroelectric glass ceramics up-conversion luminescent powder material comprises the following steps:
a) rare earth ion Eu3+Bismuth lanthanum titanate Bi3LaTi3O12Sol preparation of up-conversion luminescent material of (BLT) ferroelectric glass ceramics
The bismuth nitrate, lanthanum nitrate, butyl titanate, europium nitrate, tartaric acid, zinc acetate, bismuth nitrate, ethyl orthosilicate, tri-n-butyl borate, glycol, ammonia water and the like used in the test are all analytically pure. Bismuth lanthanum titanate Bi3LaTi3O12Ferroelectric glass ceramics xEu3+Wherein x is 1-10 mol%, wherein the molar ratio of bismuth nitrate, lanthanum nitrate and butyl titanate is Bi: La: Ti is 3:1:3, and the Bi component is excessive by 0-10 mol%. The glass component is mainly zinc-aluminum-silicon-boron (Zn-Al-Si-B-O) (Zn: Al: Si: B is 1: 0.05-0.1: 1-2: 0.5-1), and the glass component accounts for 10-40 mol% of the total mole number. Mixing a certain amount of bismuth nitrate, europium nitrate and lanthanum nitrate according to a stoichiometric ratio, and adding 1: 1-2 molar amount of tartaric acid aqueous solution, heating and stirring with magnetic stirrerStirring, and keeping the temperature at 45-55 ℃ until the mixed solid is completely dissolved to obtain a tartaric acid solution containing bismuth, europium and lanthanum; adding a certain amount of butyl titanate into tartaric acid solution with the equal molar weight and the pH value of 6-8, heating and stirring, keeping the temperature at 50-70 ℃ to form stable yellowish transparent solution, and mixing the solution with the tartaric acid solution containing bismuth, europium and lanthanum to obtain sol containing Ba, Eu, La and Ti; then, dissolving a certain amount of zinc acetate, aluminum nitrate, ethyl orthosilicate and tri-n-butyl borate in ethylene glycol to obtain a glass phase sol containing zinc (Zn), aluminum (Al), silicon (Si) and boron (B); mixing the two sols together, adjusting the viscosity and pH value of the sols by using ethylene glycol and ammonia water, reacting for more than 3 hours, fully stirring, and filtering to obtain 0.1-0.5mol/L light yellow sols;
b) rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Putting the ferroelectric glass-ceramic sol into a high-temperature oven, and drying for 24 hours at 100-150 ℃ to obtain gel; then putting the gel into a high-temperature muffle furnace, raising the room temperature to 750-1000 ℃ at a heating rate of 5-10 ℃/min, treating in air at the temperature of 750-1000 ℃ for 1-10 hours, then naturally cooling to the room temperature, crushing and grinding into powder to obtain rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Ferroelectric glass ceramics up-conversion luminescent powder material.
The invention has the following main characteristics:
(1) tartaric acid is used as a complexing agent, ethylene glycol is used as a cross-linking agent, uniform and stable sol is obtained, the used equipment is simple, the operation is easy, the heating speed and time can be controlled to prepare the viscosity of the sol, and the traditional sol-gel method mostly adopts organic metal compounds as precursors, so the cost is high, the operation is complex, the transformation process of the sol-gel cannot be effectively controlled, and the viscosity of the sol is not easy to prepare;
(2) the preparation method has the advantages of good and simple process performance and easy control of product quality. May be used in a variety of photoluminescent device applications.
Detailed Description
Example 1
According to bismuth lanthanum titanate Bi3LaTi3O12Ferroelectric glass ceramics xEu3+X is 2 mol%, and europium nitrate (Eu (NO) is weighed in terms of molar ratio3)3·6H20.0002mol of O), 0.10mol of tartaric acid, and bismuth nitrate (Bi (NO)3)3·5H2O)0.029mol, lanthanum nitrate (La (NO)3)3·6H2O)0.0088mol, butyl titanate (Ti (C)4H9O)4)0.0264mol of three components, glass component takes (Zn-Al-Si-B-O) as main component (Zn: al: si: b1: 0.05: 1: 1) the glass component is 12 mol% of the total mole number, zinc acetate 0.0012, aluminum nitrate 0.00006, ethyl orthosilicate 0.0012mol and tri-n-butyl borate 0.0012mol are weighed according to the molar ratio. Mixing weighed bismuth nitrate, europium nitrate and lanthanum nitrate according to a molar ratio of 1: 1, adding 40ml of tartaric acid aqueous solution, heating and stirring by using a magnetic stirrer, and keeping the temperature at 48 ℃ until the mixed solid is completely dissolved to obtain the citric acid solution containing bismuth, europium and lanthanum. Weighed amounts of butyl titanate were added to a corresponding molar ratio of PH 6.5 of 1: 1, heating and stirring the mixture in 20ml of tartaric acid solution, keeping the temperature at 55 ℃ to form a stable yellowish transparent solution, and mixing the solution with the tartaric acid solution containing bismuth, europium and lanthanum to obtain sol containing Ba, Eu, La and Ti; then, zinc acetate, aluminum nitrate, ethyl orthosilicate and tri-n-butyl borate which are weighed are dissolved in 30ml of ethylene glycol to obtain sol containing Zn, Al, Si and B. The two sols are mixed together by a complex phase structure method to obtain the ferroelectric material sol of the bismuth lanthanum titanate composite glass. And adjusting the pH value to 5.5 by using ammonia water, obtaining a solution with the concentration of 0.1mol/L by using the viscosity of the ethylene glycol sol and the total volume of the sol, fully stirring, and filtering to obtain a light yellow precursor sol.
Rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Putting the ferroelectric glass-ceramic sol into a high-temperature oven to be dried for 24 hours at 110 ℃ to obtain gel; then putting the gel into a high-temperature muffle furnace, heating the gel to 850 ℃ at room temperature at a heating rate of 7 ℃/min, treating the gel in air at 850 ℃ for 4 hours, naturally cooling the gel to room temperature, crushing and grinding the gelGrinding into powder to obtain rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Ferroelectric glass ceramics up-conversion luminescent powder material.
Example 2
According to bismuth lanthanum titanate Bi3LaTi3O12Ferroelectric glass ceramics xEu3+X is 5 mol%, and europium nitrate (Eu (NO) is weighed in terms of molar ratio3)3·6H2O)0.0005mol, tartaric acid (0.10mol), bismuth nitrate (Bi (NO)3)3·5H2O)0.027mol, lanthanum nitrate (La (NO)3)3·6H2O)0.0082mol, butyl titanate (Ti (C)4H9O)4)0.0246mol of three components, the glass component is mainly (Zn-Al-Si-B-O) as (Zn: al: si: b is 1: 0.1: 1: 1) the glass component is 18mol percent of the total mole number, 0.0018mol of zinc acetate, 0.00018 mol of aluminum nitrate, 0.0018mol of ethyl orthosilicate and 0.0018mol of tri-n-butyl borate are weighed according to the molar ratio. Zinc acetate, aluminum nitrate, ethyl orthosilicate 0.0105mol and tri-n-butyl borate 0.0105mol are weighed according to the mol ratio. Mixing weighed bismuth nitrate, europium nitrate and lanthanum nitrate according to a molar ratio of 1: 1, adding 40ml of tartaric acid aqueous solution, heating and stirring by using a magnetic stirrer, and keeping the temperature at 50 ℃ until the mixed solid is completely dissolved to obtain the citric acid solution containing bismuth, europium and lanthanum. Weighed amounts of butyl titanate were added to a pH of 7 in a corresponding molar ratio of 1: 1, heating and stirring the mixture in 20ml of tartaric acid solution, keeping the temperature at 60 ℃ to form a stable yellowish transparent solution, and mixing the solution with the tartaric acid solution containing bismuth, europium and lanthanum to obtain sol containing Ba, Eu, La and Ti; then, zinc acetate, aluminum nitrate, ethyl orthosilicate and tri-n-butyl borate which are weighed are dissolved in 30ml of ethylene glycol to obtain sol containing Zn, Al, Si and B. The two sols are mixed together by a complex phase structure method to obtain the ferroelectric material sol of the bismuth lanthanum titanate composite glass. And adjusting the pH value to 5.5 by using ammonia water, obtaining a solution with the concentration of 0.1mol/L by using the viscosity of the ethylene glycol sol and the total volume of the sol, fully stirring, and filtering to obtain a light yellow precursor sol.
Rare earth ion Eu3+Doped titaniumBismuth lanthanum acid Bi3LaTi3O12Putting the ferroelectric glass-ceramic sol into a high-temperature oven to be dried for 24 hours at 110 ℃ to obtain gel; then putting the gel into a high-temperature muffle furnace, heating the gel to 800 ℃ at the room temperature at the heating rate of 6 ℃/min, treating the gel in the air at the temperature of 800 ℃ for 8 hours, naturally cooling the gel to the room temperature, crushing the gel and grinding the gel into powder to obtain rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Ferroelectric glass ceramics up-conversion luminescent powder material.
Example 3
According to bismuth lanthanum titanate Bi3LaTi3O12Ferroelectric glass ceramics xEu3+X is 8 mol%, and europium nitrate (Eu (NO) is weighed in terms of molar ratio3)3·6H20.0008mol of O), 0.15mol of tartaric acid, and bismuth nitrate (Bi (NO)3)3·5H2O)0.025mol, lanthanum nitrate (La (NO)3)3·6H20.0075mol of O), butyl titanate (Ti (C)4H9O)4)0.0225mol of three components, a glass component, and a glass composition, wherein the glass component is composed of (Zn-Al-Si-B-O) system as a main component (Zn: al: si: b1: 0.05: 1.5: 1) the glass component is 25mol percent of the total mole number, 0.0025mol of zinc acetate, 0.000125 mol of aluminum nitrate, 0.00375mol of ethyl orthosilicate and 0.0025mol of tributyl borate are weighed according to the molar ratio. Mixing weighed bismuth nitrate, europium nitrate and lanthanum nitrate according to a molar ratio of 1: 1.5 adding 40ml tartaric acid aqueous solution, using magnetic stirrer to heat and stir, keeping temperature at 50 deg.C until the mixed solid is completely dissolved, obtaining bismuth, europium and lanthanum containing citric acid solution. Weighed amounts of butyl titanate were added to a pH of 7 in a corresponding molar ratio of 1: 1.5, heating and stirring the mixture in 20ml of tartaric acid solution, keeping the temperature at 60 ℃ to form a stable yellowish transparent solution, and mixing the solution with the tartaric acid solution containing bismuth, europium and lanthanum to obtain sol containing Ba, Eu, La and Ti; then, zinc acetate, aluminum nitrate, ethyl orthosilicate and tri-n-butyl borate which are weighed are dissolved in 30ml of ethylene glycol to obtain sol containing Zn, Al, Si and B. The two sols are mixed together by a complex phase structure method to obtain the ferroelectric material sol of the bismuth lanthanum titanate composite glass. Adjusting pH to 6.0 with ammonia water, and dissolving with glycol solThe solution with the concentration of 0.08mol/L is obtained by the viscosity and the total volume of the sol, and the faint yellow precursor sol is obtained by filtering after fully stirring.
Rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Putting the ferroelectric glass-ceramic sol into a high-temperature oven to be dried for 24 hours at 110 ℃ to obtain gel; then putting the gel into a high-temperature muffle furnace, heating the gel to 900 ℃ at the room temperature at the heating rate of 8 ℃/min, treating the gel in the air at 900 ℃ for 5 hours, naturally cooling the gel to the room temperature, crushing the gel and grinding the gel into powder to obtain rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Ferroelectric glass ceramics up-conversion luminescent powder material.
Example 4
According to bismuth lanthanum titanate Bi3LaTi3O12Ferroelectric glass ceramics xEu3+X is 10 mol%, and europium nitrate (Eu (NO) is weighed in terms of molar ratio3)3·6H20.001mol of O), 0.20mol of tartaric acid, and bismuth nitrate (Bi (NO)3)3·5H2O)0.0215mol, lanthanum nitrate (La (NO)3)3·6H2O)0.0065mol, butyl titanate (Ti (C)4H9O)4)0.0195mol of three components, wherein the glass component is mainly composed of (Zn-Al-Si-B-O) system (Zn: al: si: b is 1: 0.5: 1: 0.8) glass component was 35 mol% based on the total number of moles, 0.0035 mol of zinc acetate, 0.00018 mol of aluminum nitrate, 0.0018mol of ethyl orthosilicate, and 0.0018mol of tri-n-butyl borate were weighed in terms of molar ratio. Zinc acetate, aluminum nitrate, ethyl orthosilicate 0.0105mol and tri-n-butyl borate 0.0105mol are weighed according to the mol ratio. Mixing weighed bismuth nitrate, europium nitrate and lanthanum nitrate according to a molar ratio of 1: 2 adding 40ml of tartaric acid aqueous solution, heating and stirring by using a magnetic stirrer, and keeping the temperature at 55 ℃ until the mixed solid is completely dissolved to obtain the citric acid solution containing bismuth, europium and lanthanum. Weighed amounts of butyl titanate were added to a corresponding molar ratio of PH 7.5 of 1: 2, heating and stirring the mixture in 20ml of tartaric acid solution, keeping the temperature at 65 ℃ to form a stable yellowish transparent solution, and mixing the solution with the tartaric acid solution containing bismuth, europium and lanthanum to obtain sol containing Ba, Eu, La and Ti; then, the user can use the device to perform the operation,dissolving weighed zinc acetate, aluminum nitrate, ethyl orthosilicate and tri-n-butyl borate in 30ml of ethylene glycol to obtain sol containing Zn, Al, Si and B. The two sols are mixed together by a complex phase structure method to obtain the ferroelectric material sol of the bismuth lanthanum titanate composite glass. And adjusting the pH value to 6 by using ammonia water, obtaining a solution with the concentration of 0.1mol/L by using the viscosity of the ethylene glycol sol and the total volume of the sol, fully stirring, and filtering to obtain a light yellow precursor sol.
Rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Putting the ferroelectric glass-ceramic sol into a high-temperature oven to be dried for 24 hours at 120 ℃ to obtain gel; then putting the gel into a high-temperature muffle furnace, heating the gel to 950 ℃ at the room temperature at the heating rate of 10 ℃/min, treating the gel in air at 950 ℃ for 4 hours, naturally cooling the gel to the room temperature, crushing the gel and grinding the powder to obtain rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Ferroelectric glass ceramics up-conversion luminescent powder material.
Claims (2)
1. Rare earth ion Eu3+ doped Bi3LaTi3O12 ferroelectric microcrystalline glass up-conversion luminescent powder comprises the following components:
bismuth lanthanum titanate Bi3LaTi3O12 ferroelectric microcrystalline glass xEu3+, wherein x is 1-10 mol%.
2. The method for preparing rare earth ion Eu3+ doped Bi3LaTi3O12 ferroelectric microcrystalline glass up-conversion luminescent powder according to claim 1, comprising the following steps:
a) rare earth ion Eu3+Bismuth lanthanum titanate Bi3LaTi3O12Preparation of sol of ferroelectric glass-ceramic up-conversion luminescent material
The bismuth nitrate, lanthanum nitrate, butyl titanate, europium nitrate, tartaric acid, zinc acetate, bismuth nitrate, ethyl orthosilicate, tri-n-butyl borate, glycol, ammonia water and the like used in the test are all analytically pure. Bismuth lanthanum titanate Bi3LaTi3O12Ferroelectric glass ceramics xEu3+Wherein x is 1-10 mol%, and the molar ratio of bismuth nitrate, lanthanum nitrate and butyl titanate is Bi, La, Ti3:1:3, and adding 0-10 mol% of Bi component in excess. The glass component is mainly zinc-aluminum-silicon-boron (Zn-Al-Si-B-O) (Zn: Al: Si: B is 1: 0.05-0.1: 1-2: 0.5-1), and the glass component accounts for 10-40 mol% of the total mole number. Mixing a certain amount of bismuth nitrate, europium nitrate and lanthanum nitrate according to a stoichiometric ratio, adding an equimolar amount of tartaric acid aqueous solution, heating and stirring by using a magnetic stirrer, and keeping the temperature at 45-55 ℃ until the mixed solid is completely dissolved to obtain a tartaric acid solution containing bismuth, europium and lanthanum; adding a certain amount of butyl titanate into tartaric acid solution with the equal molar weight and the pH value of 6-8, heating and stirring, keeping the temperature at 50-70 ℃ to form stable yellowish transparent solution, and mixing the solution with the tartaric acid solution containing bismuth, europium and lanthanum to obtain sol containing Ba, Eu, La and Ti; then, dissolving a certain amount of zinc acetate, aluminum nitrate, ethyl orthosilicate and tri-n-butyl borate in ethylene glycol to obtain a glass phase sol containing zinc (Zn), aluminum (Al), silicon (Si) and boron (B); mixing the two sols together, adjusting the viscosity and pH value of the sols by using ethylene glycol and ammonia water, reacting for more than 3 hours, fully stirring, and filtering to obtain 0.1-0.5mol/L light yellow sols;
b) rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Putting the ferroelectric glass-ceramic sol into a high-temperature oven, and drying for 24 hours at 100-150 ℃ to obtain gel; then putting the gel into a high-temperature muffle furnace, raising the room temperature to 750-1000 ℃ at a heating rate of 5-10 ℃/min, treating in air at the temperature of 750-1000 ℃ for 1-10 hours, then naturally cooling to the room temperature, crushing and grinding into powder to obtain rare earth ion Eu3+Bismuth lanthanum titanate doped Bi3LaTi3O12Ferroelectric glass ceramics up-conversion luminescent powder material.
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| CN112745841A (en) * | 2020-12-25 | 2021-05-04 | 广西大学 | Alkali metal reinforced bismuth titanate-based up-conversion fluorescent material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112194367A (en) * | 2020-10-09 | 2021-01-08 | 新昌中国计量大学企业创新研究院有限公司 | Ferroelectric glass-ceramic up-conversion luminescent material and preparation method thereof |
| CN112745841A (en) * | 2020-12-25 | 2021-05-04 | 广西大学 | Alkali metal reinforced bismuth titanate-based up-conversion fluorescent material and preparation method thereof |
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