CN106220179A - A kind of Ba2laF7: Er3+the preparation method of upper conversion transparent ceramic - Google Patents

A kind of Ba2laF7: Er3+the preparation method of upper conversion transparent ceramic Download PDF

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CN106220179A
CN106220179A CN201610536085.4A CN201610536085A CN106220179A CN 106220179 A CN106220179 A CN 106220179A CN 201610536085 A CN201610536085 A CN 201610536085A CN 106220179 A CN106220179 A CN 106220179A
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preparation
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upper conversion
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王殿元
段兴凯
王庆凯
王侃民
郭艳艳
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Jiujiang University
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Abstract

The invention discloses a kind of Ba2LaF7:Er3+The preparation method of upper conversion transparent ceramic.The method comprises the steps: with barium nitrate, lanthanum nitrate hexahydrate, five water Erbium trinitrate and ammonium fluoride as raw material, uses hydro-thermal method to prepare Ba2LaF7:Er3+Nanocrystalline, by gained Ba2LaF7:Er3+Nanocrystalline washing, dry, grinding, in sintering furnace, 900 DEG C of vacuum heating-press sinterings, finally give Ba2LaF7:Er3+Crystalline ceramics.It is simple that the preparation method of the present invention has technique, it is not necessary to agglutinant, it is easy to operates and the advantage such as production, the Ba prepared2LaF7:Er3+Crystalline ceramics has a good light transmission, and up-conversion luminescence efficiency is high, shows at biological fluorescent labelling, 3 D stereo, the field such as upconversion laser, anti-counterfeiting detection, lighting source is respectively provided with wide application prospect.

Description

A kind of Ba2LaF7:Er3+The preparation method of upper conversion transparent ceramic
Technical field
The present invention relates to a kind of Ba2LaF7:Er3+The preparation method of upper conversion transparent ceramic, particularly belongs to ceramic material system Standby technical field.
Background technology
Rear-earth-doped up-conversion luminescent material is a kind of at the infrared ray excited lower luminescent material that can send visible ray, three The fields such as dimension stereo display, biological fluorescent labelling, upconversion laser, anti-counterfeiting detection have broad application prospects.Since 1964 Year having found since up-conversion luminescence phenomenon, this has been carried out and has studied widely by people, but mostly in monocrystalline or glass system.By Harsh in crystal growth condition, the chemical stability of glass and bad mechanical strength, and pottery has doping content height, uniform doping Property good, sintering temperature is low, and the cycle is short, low cost, and quality controllability is strong, and size is big, the advantages such as freedom shape is big, and glass phase Ratio, it is good that it has again monochromaticity, thermal conductivity height and the radiant power advantages of higher that can bear, the therefore upper conversion to ceramic systems The research of luminescent material causes to be paid close attention to widely.
Rear-earth-doped binary fluoride be in the last few years people research most up-conversion luminescent materials it One, owing to its phonon energy is low, the advantages such as up-conversion luminescence efficiency is high, good stability, have been obtained for well applying.In recent years Coming, the most of research are exactly NaYF4、LiYF4、NaGdF4Deng material, owing to this kind of material belongs to binary solid solution material, alkali Earth metal fluoride and rare earth fluoride can form solid solution in the larger context, and have many individual system to have face-centered cubic Structure, such as Ba2LaF7、BaGdF5Deng, and after the rare earth doped light emitting ionic of the two system, it is also possible to obtain high efficiency upper turn Change light.Due to Ba2LaF7:Er3+Having cubic structure, the Refractive Index of Material of cubic structure does not have directional dependence, it is easy to Sintering obtains crystalline ceramics.Therefore, Ba is prepared2LaF7:Er3+Upper conversion transparent ceramic will expand the application neck of this material Territory, improves its performance.Therefore, a kind of Ba of invention2LaF7:Er3+The preparation method of upper conversion transparent ceramic is to have very much actual meaning Justice.
Summary of the invention
It is an object of the invention to provide a kind of Ba2LaF7:Er3+The preparation method of upper conversion transparent ceramic, especially by Techniques below scheme realizes.
The invention discloses a kind of Ba2LaF7:Er3+The preparation method of upper conversion transparent ceramic, comprises the steps:
(1) barium nitrate 2.091g, lanthanum nitrate hexahydrate 1.715g and five water Erbium trinitrate 0.0177g are dissolved in 70ml water, add 5ml polyethylene glycol 200, magnetic agitation 15min, obtain solution A；Ammonium fluoride 3.108g is dissolved in 35ml water, stirs molten Liquid B；Solution B is slowly dropped in solution A, magnetic agitation, room temperature reaction 1-2h, is aged 24-36h, obtains mixed solution；Nitric acid Barium is 1:10-12 with the mol ratio of ammonium fluoride, and polyethylene glycol 200 is 1:10-12 with the volume ratio of water in solution A.
(2) the mixed liquor immigration of step (1) gained is contained in teflon-lined autoclave, heated sealed To 180-200 DEG C, be incubated 24-36h, naturally cool to room temperature after completion of the reaction, product by centrifugation, wash, be dried, Ba2LaF7:Er3+Nanocrystalline material；
(3) by the Ba of step (2) gained2LaF7:Er3+Nanocrystalline material grinds 30-60min in agate mortar, ~ 10-3Pa In vacuum atmosphere, hot pressed sintering 4-8h under the conditions of 900 DEG C and 80-100Mpa, obtain Ba2LaF7:Er3+The transparent pottery of upper conversion Porcelain.
It is an advantage of the invention that
Ba disclosed by the invention2LaF7:Er3+The preparation method of upper conversion transparent ceramic, uses hydro-thermal method to prepare Ba2LaF7:Er3+ Nanocrystalline powder, polyethylene glycol 200 is dispersant, and nanocrystalline particle diameter is at 20-40nm, and pattern is spherical, favorable dispersibility, Ba2LaF7:Er3+Having cubic structure, the Refractive Index of Material of cubic structure does not have directional dependence, it is easy to sintering obtains transparent Pottery.The method provided in the present invention have employed 900 DEG C of vacuum heating-press sinterings, both avoid Ba2LaF7:Er3+Oxidized, again Ceramic dense degree can be improved, thus obtain Ba2LaF7:Er3+Crystalline ceramics.It is simple that the preparation method of the present invention has technique, nothing Need agglutinant, it is easy to operate and the advantage such as production, the Ba prepared2LaF7:Er3+Crystalline ceramics has good light transmission, Up-conversion luminescence efficiency is high, shows at biological fluorescent labelling, 3 D stereo, upconversion laser, anti-counterfeiting detection, lighting source etc. Field is respectively provided with wide application prospect.
Accompanying drawing explanation
Fig. 1 is Ba of the present invention2LaF7:Er3+The photo in kind of upper conversion transparent ceramic.
Detailed description of the invention
Embodiment 1
A kind of Ba2LaF7:Er3+The preparation method of upper conversion transparent ceramic, comprises the following steps:
(1) barium nitrate 2.091g, lanthanum nitrate hexahydrate 1.715g and five water Erbium trinitrate 0.0177g are dissolved in 70ml water, add 5ml polyethylene glycol 200, magnetic agitation 15min, obtain solution A；Ammonium fluoride 3.108g is dissolved in 35ml water, stirs molten Liquid B, is slowly dropped into solution B in solution A, magnetic agitation, room temperature reaction 1h, is aged 24h, obtains mixed solution；
(2) the mixed liquor immigration of step (1) gained is contained in teflon-lined autoclave, heated sealed to 180 DEG C, be incubated 24h, naturally cool to room temperature after completion of the reaction, product by centrifugation, wash, be dried, obtain Ba2LaF7:Er3+Receive The brilliant material of rice；
(3) by the Ba of step (2) gained2LaF7:Er3+Nanocrystalline material grinds 30min in agate mortar, ~ 10-3Pa is true In 900 DEG C of 80Mpa hot pressed sintering 4h in air atmosphere, finally give Ba2LaF7:Er3+Crystalline ceramics.

Claims (1)

1. a Ba2LaF7:Er3+The preparation method of upper conversion transparent ceramic, it is characterised in that: described preparation method include with Lower step:
(1) barium nitrate 2.091g, lanthanum nitrate hexahydrate 1.715g and five water Erbium trinitrate 0.0177g are dissolved in 70ml water, add 5ml polyethylene glycol 200, magnetic agitation 15min, obtain solution A；Ammonium fluoride 3.108g is dissolved in 35ml water, stirs molten Liquid B；Solution B is slowly dropped in solution A, magnetic agitation, room temperature reaction 1-2h, is aged 24-36h, obtains mixed solution；Nitric acid Barium is 1:10-12 with the mol ratio of ammonium fluoride, and polyethylene glycol 200 is 1:10-12 with the volume ratio of water in solution A；
(2) moving into the mixed liquor of step (1) gained containing in teflon-lined autoclave, heated sealed is extremely 180-200 DEG C, be incubated 24-36h, naturally cool to room temperature after completion of the reaction, product by centrifugation, wash, be dried, Ba2LaF7:Er3+Nanocrystalline material；
(3) by the Ba of step (2) gained2LaF7:Er3+Nanocrystalline material grinds 30-60min in agate mortar, ~ 10-3Pa In vacuum atmosphere, hot pressed sintering 4-8h under the conditions of 900 DEG C and 80-100Mpa, obtain Ba2LaF7:Er3+The transparent pottery of upper conversion Porcelain.
CN201610536085.4A 2016-07-10 2016-07-10 A kind of Ba2laF7: Er3+the preparation method of upper conversion transparent ceramic Pending CN106220179A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108046754A (en) * 2018-02-06 2018-05-18 上海高诚创意科技集团有限公司 It is a kind of that there are the ceramics of concealed anti-false
CN111020740A (en) * 2020-01-07 2020-04-17 巢湖市方太渔具有限责任公司 Preparation method of calcium lignosulphonate modified fishing net
CN112374525A (en) * 2020-11-12 2021-02-19 西南大学 Solid electrolyte material, solid electrolyte layer and preparation method thereof
CN112456536A (en) * 2020-11-12 2021-03-09 西南大学 Solid electrolyte material, fluorine ion battery and preparation method thereof
CN116425547A (en) * 2023-03-16 2023-07-14 广东省科学院资源利用与稀土开发研究所 Chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material and preparation method thereof

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CN102674843A (en) * 2012-04-28 2012-09-19 武汉理工大学 Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof
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CN102390932A (en) * 2011-07-28 2012-03-28 沈阳大学 Transparent oxyfluoride tellurite glass ceramic of fluoride-containing nanocrystalline
CN102674843A (en) * 2012-04-28 2012-09-19 武汉理工大学 Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof
CN102826850A (en) * 2012-08-20 2012-12-19 长春理工大学 Barium fluoride up-conversion transparent ceramic and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108046754A (en) * 2018-02-06 2018-05-18 上海高诚创意科技集团有限公司 It is a kind of that there are the ceramics of concealed anti-false
CN111020740A (en) * 2020-01-07 2020-04-17 巢湖市方太渔具有限责任公司 Preparation method of calcium lignosulphonate modified fishing net
CN112374525A (en) * 2020-11-12 2021-02-19 西南大学 Solid electrolyte material, solid electrolyte layer and preparation method thereof
CN112456536A (en) * 2020-11-12 2021-03-09 西南大学 Solid electrolyte material, fluorine ion battery and preparation method thereof
CN116425547A (en) * 2023-03-16 2023-07-14 广东省科学院资源利用与稀土开发研究所 Chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material and preparation method thereof
CN116425547B (en) * 2023-03-16 2024-01-30 广东省科学院资源利用与稀土开发研究所 Chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material and preparation method thereof

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