CN105254184A - Li3YCl6 glass ceramics doped with rare earth ions and preparation method of Li3YCl6 glass ceramics - Google Patents

Li3YCl6 glass ceramics doped with rare earth ions and preparation method of Li3YCl6 glass ceramics Download PDF

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Publication number
CN105254184A
CN105254184A CN201510852817.6A CN201510852817A CN105254184A CN 105254184 A CN105254184 A CN 105254184A CN 201510852817 A CN201510852817 A CN 201510852817A CN 105254184 A CN105254184 A CN 105254184A
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ycl
devitrified glass
acetic acid
rare earth
sio
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欧阳绍业
张约品
张为欢
张志雄
王倩
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Ningbo University
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Ningbo University
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Abstract

The invention discloses Li3YCl6 glass ceramics doped with rare earth ions. The Li3YCl6 glass ceramics is prepared from 87.8-94 mol% of SiO2, 5.5-10 mol% of Li3YCl6 and 0.5-3 mol% of LnCl3, wherein LnCl3 is at least one of YbCl3, ErCl3, TmCl3 and HoCl3. The Li3YCl6 glass ceramics has the advantages of being transparent, resistant to air slake, good in mechanical performance, high in blue and purple light transmittance, low in phonon energy, high in up-conversion efficiency, capable of greatly improving efficiency of an up-conversion laser device, simple in preparation method and low in production cost.

Description

A kind of rare earth ion doped Li 3yCl 6devitrified glass and preparation method thereof
Technical field
The present invention relates to a kind of rare earth ion doped devitrified glass, especially relate to a kind of rare earth ion doped Li being used as up-conversion luminescent material 3yCl 6devitrified glass and preparation method thereof.
Background technology
When the up-conversion luminescence of rare earth ion refers to the sample when the excitation light irradiation doping with rare-earth ions adopting wavelength longer, launch the phenomenon that wavelength is less than the light of excitation wavelength.Utilize the upper conversion characteristic of rare earth ion, can obtain cheap, that can at room temperature work and export purplish blue green-light fiber laser continuously.Up-conversion lasing can be applicable to the every field such as color monitor, data storing, information technology, laser printing and medical treatment.The efficiency improving up-conversion luminescence need reduce the phonon energy of substrate material, this is mainly because lower phonon energy can reduce the generation of non-radiative relaxation probability, improve the fluorescence lifetime of metastable level in the middle of rare earth ion, effectively can improve the efficiency of up-conversion luminescence.Li 3yCl 6crystal has the phonon energy lower than fluorochemical, is more suitable for as rear-earth-doped up-conversion luminescence matrix, rare earth ion doped Li 3yCl 6crystal has the upper efficiency of conversion higher than rare earth ion doped crystal of fluoride, but Li 3yCl 6the easy moisture absorption of crystal, need special processing and storage, be difficult to preparation, chemical stability and its practical application of the disadvantages affect such as physical strength is poor.
Transparent glass-ceramics is a kind of photoelectron material having crystal and glass advantage concurrently.Chloride current transparent glass-ceramics is mainly used as flashing and up-conversion luminescent material, and if publication number is CN103382089, name is called " containing Cs 3laCl 6nanocrystalline transparent sulfur-halogen glass pottery and preparation thereof " application for a patent for invention disclose doping Nd 3+or Er 3+ion, with Cs 3laCl 6for crystallite phase, glassy phase are the devitrified glass of sulfide, but the physical and chemical performance of sulfide is poorer than oxide compound, and not saturating in visible ray shortwave strong point, have impact on up-conversion luminescence and exports; If publication number is CN103951243, name is called " rare earth ion doped Cs 2liYCl 6devitrified glass and preparation method thereof " application for a patent for invention also disclose a kind of crystallite mutually for Cs 2liYCl 6, glassy phase is GeO 2be main devitrified glass, the rare earth ion of doping is Ce 3+, Eu 3+, Tb 3+, Pr 3+and Nd 3+in one, adopt melt supercooled method and subsequent heat treatment preparation, there is good scintillation properties, be mainly used as scintillation material.But also there is no rare earth ion Yb at present 3+, Er 3+, Tm 3+and Ho 3+the Li of doping 3yCl 6devitrified glass is used for the open report of up-conversion luminescent material.
Summary of the invention
The rare earth ion doped Li that technical problem to be solved by this invention is to provide that a kind of phonon energy is low, little, the upper conversion quantum yield of radiationless transition probability is high, Deliquescence-resistant, good mechanical property, up-conversion luminescence are very strong 3yCl 6devitrified glass and preparation method thereof.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of rare earth ion doped Li 3yCl 6devitrified glass, its molar percentage is composed as follows: SiO 287.8 ~ 94mol%, Li 3yCl 65.5 ~ 10mol%, LnCl 30.5 ~ 3mol%, wherein LnCl 3for YbCl 3, ErCl 3, TmCl 3and HoCl 3in at least one.
This devitrified glass molar percentage consists of: SiO 287.8mol%, Li 3yCl 610mol%, TmCl 30.2mol%, YbCl 32mol%.
This devitrified glass molar percentage consists of: SiO 289mol%, Li 3yCl 68mol%, ErCl 30.5mol%, YbCl 32.5mol%.
This devitrified glass molar percentage consists of: SiO 288mol%, Li 3yCl 69mol%, ErCl 30.1mol%, TmCl 30.1mol%, YbCl 32.8mol%.
Described rare earth ion doped Li 3yCl 6the preparation method of devitrified glass, comprises the following steps:
(1) by mole% composition SiO 287.8 ~ 94mol%, Li 3yCl 65.5 ~ 10mol%, LnCl 30.5 ~ 3mol%, wherein LnCl 3for YbCl 3, ErCl 3, TmCl 3and HoCl 3in at least one; Take at least one in acetic acid yttrium, Lithium Acetate and acetic acid ytterbium, acetic acid erbium, acetic acid thulium and acetic acid holmium, wherein the deal of acetic acid yttrium, Lithium Acetate is respectively by mole% Li in composition 3yCl 6molar content take, the deal of acetic acid ytterbium, acetic acid erbium, acetic acid thulium and at least one in acetic acid holmium is respectively by LnCl in above-mentioned identical molar percentage composition 3molar content take, and above-mentioned acetate is dissolved in deionized water forms Acetate Solution, in Acetate Solution, add trichoroacetic acid(TCA) obtain transparent mixing solutions, wherein in trichoroacetic acid(TCA) and Acetate Solution, the mol ratio of metal ion summation is 3: 1;
(2) SiO in forming by the molar percentage identical with step (1) 2molar content take tetraethoxy and be dissolved in ethanol, obtain teos solution, then stir 1 hour after being mixed with teos solution by mixing solutions obtained for step (1), then regulate its pH value to 5 with dust technology, obtain precursor liquid;
(3) the precursor liquid room temperature ageing that step (2) obtains is placed on baking oven in 2 weeks, is warming up to 142 DEG C of dryings 9 days, obtains transparent xerogel;
(4) xerogel that step (3) obtains is placed in nitrogen fine annealing stove, thermal treatment 10 hours at the temperature of 560 ~ 590 DEG C, and then be cooled to 50 DEG C with the speed of 10 DEG C/h, close fine annealing stove power supply, automatically be cooled to room temperature, obtain transparent rare earth ion doped Li 3yCl 6devitrified glass.
Compared with prior art, the invention has the advantages that: this devitrified glass has Li 3yCl 6the feature that in the excellence of crystalline host material, the physical strength of conversion performance and silica glass, stability and being easy to is processed; The experiment proved that: by the rare earth ion doped Li obtained by preparation method of the present invention 3yCl 6devitrified glass is transparent, Deliquescence-resistant, good mechanical property, royal purple light transmission rate are higher, has the performances such as low, the upper efficiency of conversion of phonon energy is high, upconversion laser efficiency can be made greatly to improve; In addition, the preparation method of this devitrified glass is simple and have good repeatability, and production cost is lower.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of the devitrified glass that embodiment 1 obtains;
Fig. 2 is the Tm that embodiment 1 obtains 3+, Yb 3+the Li of doping 3yCl 6the 970nm laser apparatus of devitrified glass excites up-conversion luminescence spectrum;
Fig. 3 is the Tm that comparative example 1 obtains 3+, Yb 3+the Li of doping 3yF 6the 970nm laser apparatus of devitrified glass excites up-conversion luminescence spectrum.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1
Tm 3+, Yb 3+li doped 3yCl 6the molar percentage of devitrified glass consists of: SiO 287.8mol%, Li 3yCl 610mol%, TmCl 30.2mol%, YbCl 32mol%, the technique preparing devitrified glass of above composition is as follows:
(1) take acetic acid yttrium, Lithium Acetate, acetic acid ytterbium, acetic acid thulium, wherein the deal of acetic acid yttrium, Lithium Acetate is respectively by mole% Li in composition 3yCl 6molar content take, the deal of acetic acid ytterbium, acetic acid thulium is respectively by YbCl in above-mentioned identical molar percentage composition 3, TmCl 3molar content take, be dissolved in deionized water by above-mentioned acetate and form Acetate Solution, add trichoroacetic acid(TCA) and obtain transparent mixing solutions in Acetate Solution, wherein in trichoroacetic acid(TCA) and Acetate Solution, the mol ratio of metal ion summation is 3: 1;
(2) SiO in forming by the molar percentage identical with step (1) 2molar content take tetraethoxy and be dissolved in ethanol, obtain teos solution, then stir 1 hour after being mixed with teos solution by mixing solutions obtained for step (1), then regulate its pH value to 5 with dust technology, obtain precursor liquid;
(3) the precursor liquid room temperature ageing that step (2) obtains is placed on baking oven in 2 weeks, is warming up to 142 DEG C of dryings 9 days, obtains transparent xerogel;
(4) xerogel that step (3) obtains is placed in nitrogen fine annealing stove, 560 ~ 590 DEG C of thermal treatments 10 hours, and then be cooled to 50 DEG C with the speed of 10 DEG C/h, close fine annealing stove power supply, automatically be cooled to room temperature, obtain transparent rare earth ion Tm 3+, Yb 3+the Li of doping 3yCl 6devitrified glass.
To obtained Li 3yCl 6devitrified glass carries out X-ray diffraction test, obtains the XRD figure of this devitrified glass as shown in Figure 1, and its result is as follows: the XRD diffraction peak of the sample obtained through Overheating Treatment and Li 3yCl 6the main diffraction peak of the standard x RD figure of crystalline phase all conforms to, and the material therefore obtained is Li 3yCl 6the devitrified glass of crystallization phase.Measure by TRIAX550 fluorescence spectrophotometer, under 970nm laser apparatus shooting conditions, the up-conversion luminescence spectrum of this devitrified glass recorded as shown in Figure 2, the integration luminous intensity of blue light (476nm), ruddiness (679nm) respectively about 4.43 × 10 5, 7.34 × 10 5, blue, red up-conversion luminescence is very strong.
Embodiment 2
Er 3+, Yb 3+li doped 3yCl 6the molar percentage of devitrified glass consists of: SiO 289mol%, Li 3yCl 68mol%, ErCl 30.5mol%, YbCl 32.5mol%, after the preparation identical with embodiment 1 and heat treatment process, obtains transparent rare earth ion Er 3+, Yb 3+the Li of doping 3yCl 6devitrified glass.This devitrified glass TRIAX550 fluorescence spectrophotometer is measured, under 970nm laser apparatus shooting conditions, observes strong green and red up-conversion luminescence.
Embodiment 3
Er 3+, Tm 3+, Yb 3+li doped 3yCl 6the molar percentage of devitrified glass consists of: SiO 288mol%, Li 3yCl 69mol%, ErCl 30.1mol%, TmCl 30.1mol%, YbCl 32.8mol%, after the preparation identical with embodiment 1 and heat treatment process, obtains transparent rare earth ion Er 3+, Tm 3+, Yb 3+the Li of doping 3yCl 6devitrified glass.This devitrified glass TRIAX550 fluorescence spectrophotometer is measured, under 970nm laser apparatus shooting conditions, observes strong blueness, green and red up-conversion luminescence.
Embodiment 4
Ho 3+li doped 3yCl 6the molar percentage of devitrified glass consists of: SiO 294mol%, Li 3yCl 65.5mol%, HoCl 30.5mol%, after the preparation identical with embodiment 1 and heat treatment process, obtains transparent rare earth ion Ho 3+the Li of doping 3yCl 6devitrified glass.This devitrified glass TRIAX550 fluorescence spectrophotometer is measured, and under 970nm laser apparatus shooting conditions, observes strong green and red up-conversion luminescence.
Comparative example 1
Tm 3+, Yb 3+li doped 3yF 6the molar percentage of devitrified glass consists of: SiO 287.8mol%, Li 3yF 610mol%, TmF 30.2mol%, YbF 32mol%, after the preparation identical with embodiment 1 and heat treatment process, obtains transparent rare earth ion Tm 3+, Yb 3+the Li of doping 3yF 6devitrified glass.Measure by TRIAX550 fluorescence spectrophotometer, under 970nm laser apparatus shooting conditions, the up-conversion luminescence spectrum of this devitrified glass recorded as shown in Figure 3, the integration luminous intensity of blue light (476nm), ruddiness (679nm) respectively about 3.96 × 10 4, 6.56 × 10 4, compare with embodiment 1, blue, red Up-conversion Intensity is low, and the Tm that embodiment 1 obtains is described 3+, Yb 3+the Li of doping 3yCl 6the Tm that the up-conversion luminescence performance test ratio 1 of devitrified glass obtains 3+, Yb 3+the Li of doping 3yF 6devitrified glass is better.

Claims (5)

1. a rare earth ion doped Li 3yCl 6devitrified glass, its molar percentage consists of: SiO 287.8 ~ 94mol%, Li 3yCl 65.5 ~ 10mol%, LnCl 30.5 ~ 3mol%, wherein LnCl 3for YbCl 3, ErCl 3, TmCl 3and HoCl 3in at least one.
2. Li rare earth ion doped as claimed in claim 1 3yCl 6devitrified glass, is characterized in that this devitrified glass molar percentage consists of: SiO 287.8mol%, Li 3yCl 610mol%, TmCl 30.2mol%, YbCl 32mol%.
3. Li rare earth ion doped as claimed in claim 1 3yCl 6devitrified glass, is characterized in that this devitrified glass molar percentage consists of: SiO 289mol%, Li 3yCl 68mol%, ErCl 30.5mol%, YbCl 32.5mol%.
4. Li rare earth ion doped as claimed in claim 1 3yCl 6devitrified glass, is characterized in that this devitrified glass molar percentage consists of: SiO 288mol%, Li 3yCl 69mol%, ErCl 30.1mol%, TmCl 30.1mol%, YbCl 32.8mol%.
5. Li rare earth ion doped as claimed in claim 1 3yCl 6the preparation method of devitrified glass, is characterized in that comprising the following steps:
(1) by mole% composition SiO 287.8 ~ 94mol%, Li 3yCl 65.5 ~ 10mol%, LnCl 30.5 ~ 3mol%, wherein LnCl 3for YbCl 3, ErCl 3, TmCl 3and HoCl 3in at least one; Take at least one in acetic acid yttrium, Lithium Acetate and acetic acid ytterbium, acetic acid erbium, acetic acid thulium and acetic acid holmium, wherein the deal of acetic acid yttrium, Lithium Acetate is respectively by mole% Li in composition 3yCl 6molar content take, the deal of acetic acid ytterbium, acetic acid erbium, acetic acid thulium and at least one in acetic acid holmium is respectively by LnCl in above-mentioned identical molar percentage composition 3molar content take, and above-mentioned acetate is dissolved in deionized water forms Acetate Solution, in Acetate Solution, add trichoroacetic acid(TCA) obtain transparent mixing solutions, wherein in trichoroacetic acid(TCA) and Acetate Solution, the mol ratio of metal ion summation is 3: 1;
(2) SiO in forming by the molar percentage identical with step (1) 2molar content take tetraethoxy and be dissolved in ethanol, obtain teos solution, then stir 1 hour after being mixed with teos solution by mixing solutions obtained for step (1), then regulate its pH value to 5 with dust technology, obtain precursor liquid;
(3) the precursor liquid room temperature ageing that step (2) obtains is placed on baking oven in 2 weeks, is warming up to 142 DEG C of dryings 9 days, obtains transparent xerogel;
(4) xerogel that step (3) obtains is placed in nitrogen fine annealing stove, thermal treatment 10 hours at the temperature of 560 ~ 590 DEG C, and then be cooled to 50 DEG C with the speed of 10 DEG C/h, close fine annealing stove power supply, automatically be cooled to room temperature, obtain transparent rare earth ion doped Li 3yCl 6devitrified glass.
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