A terbium ytterbium rare earth ion double-doped lutetium gadolinium lithium fluoride up-conversion luminescent crystal and preparation method thereof

A technology of mixed lutetium-gadolinium fluoride and lutetium-gadolinium fluoride, which is applied in the field of up-conversion luminescent single crystals, can solve problems such as equipment loss, poor crystal quality, and large crystal stress, and achieve electricity cost savings and uniform ion distribution , The effect of small crystal stress

Inactive Publication Date: 2016-06-08
NINGBO UNIV
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Problems solved by technology

But when Yb 3+ / Tb 3+ Simultaneous doping of ions into LiLuF 4 In the crystal, the substituted Lu 3+ Ionic Radius and Dopant Ion Yb 3+ comparison match, but another dopant ion Tb 3+ with Lu 3+ difference mismatch, resulting in Tb 3+ The distribution of ions in the crystal is not uniform, resulting in large crystal stress, and the quality of the obtained crystal is poor
In addition LiLuF 4 Fluoride crystals will volatilize and produce highly corrosive fluoride gas during the high-temperature growth process, which will cause loss to equipment, and may cause serious harm to the human body, especially due to the volatilization of the gas, resulting in the loss of the original formula components. missing, affecting the quality of the crystal

Method used

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  • A terbium ytterbium rare earth ion double-doped lutetium gadolinium lithium fluoride up-conversion luminescent crystal and preparation method thereof
  • A terbium ytterbium rare earth ion double-doped lutetium gadolinium lithium fluoride up-conversion luminescent crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] LiF, LuF with a purity greater than 99.99% 3 , GdF 3 , YbF 3 , TbF 3 Mix according to the molar percentage ratio of 51.5:36.183:10.0:2.0:0.317, place in a mill, grind and mix for 5 hours to obtain a mixture of uniform powder, place the mixture in a boat-shaped platinum crucible, and then install it in a tube In the platinum pipe of the type resistance furnace, and then use N 2 Remove the air in the platinum pipeline, and then gradually raise the temperature of the furnace body to 740°C, and conduct reaction treatment for 2 hours under HF gas, and the reaction treatment is completed. Tube resistance furnace, with N 2 The residual HF gas in the gas cleaning pipeline is gradually cooled to room temperature to obtain polycrystalline powder. The polycrystalline powder is placed in a mill and ground into powder, then placed in a Pt crucible and compacted, and the Pt crucible is sealed. The Pt crucible is placed in a silicon-molybdenum rod furnace, and the crystal is grow...

Embodiment 2

[0026] Basically the same as embodiment 1, the difference is only LiF, LuF 3 , GdF 3 , YbF 3 , TbF 3 Mix according to the molar percentage ratio of 51.5: 33.183: 10.0: 5.0: 0.317, and react for 3 hours. The temperature gradient of the solid-liquid interface is 50°C / cm, and the crucible descending speed is 0.5mm / h. The furnace temperature was lowered to room temperature at 50° C. in one hour, and the samples were taken to measure α=0.071, β=0.0496, and γ=0.0032. The chemical formula of the single crystal is LiLu 0.8762 Gd 0.071 Yb 0.0496 Tb 00032 f 4 , and each sample obtained was polished into a thin slice with a thickness of 2 mm. Keeping the same optical test conditions as in Example 1, the obtained fluorescence intensity is comparable to that of the sample in Example 1. Under 960nm light excitation, under 960nm red light excitation, the upconversion fluorescence of embodiment 1 sees figure 2 , the intensity of blue light in the 550nm band is 12.40 units.

Embodiment 3

[0028] Basically the same as embodiment 1, the difference is only LiF, LuF 3 , GdF 3 , YbF 3 , TbF 3 Mix according to the molar percentage ratio of 51.5:30.183:10.0:8.0:0.317, and react for 4 hours. The temperature gradient of the solid-liquid interface is 80°C / cm, and the crucible descending speed is 1mm / h. The temperature of the furnace was lowered to room temperature at 70°C, and α=0.071, β=0.0793, and γ=0.0032 were measured by sampling. The chemical formula of the single crystal is LiLu 0.8465 Gd 0.071 Yb 0.0793 Tb 0.0032 f 4 , and each sample obtained was polished into a thin slice with a thickness of 2 mm. Keeping the same optical test conditions as in Example 1, the obtained fluorescence intensity is comparable to that of the sample in Example 1. Under 960nm light excitation, under 960nm red light excitation, the upconversion fluorescence of embodiment 1 sees figure 2 , the intensity of blue light in the 550nm band is 28.90 units.

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Abstract

The invention discloses a terbium / ytterbium rare earth ion codoped lithium gadolinium lutetium fluoride upconversion luminescent crystal and a preparation method thereof. Gd is introduced into a LiLuF4 crystal substrate, and Yb<3+> and Tb<3+> rare-earth luminescent ions are simultaneously doped to generate a monocrystal of which the chemical formula is LiLu(1-alpha-beta-gamma)GdalphaYbbetaTbgammaF4. The fluoride monocrystal has the advantages of low growth temperature, uniform distribution of Yb<3+> and Tb<3+>, high solubility, and favorable thermal, mechanical and chemical stability. The rare earth ions doped in the monocrystal have high luminescence efficiency; and by adopting a water-free oxygen-free sealed crucible descending process and carrying out high-temperature fluoridation treatment on the raw material, the preparation method can be used for preparing the high-quality crystal which is almost free of hydroxide ions and oxides. Under the excitation of 960nm-wavelength light and under the synergic energy transfer actions of Yb<3+> and Tb<3+>, strong 500nm fluorescence emission can be obtained; and the luminescent crystal is hopeful to be used as night light in the field of infrared detection, biological markers, long-afterglow luminescence warning markers, fireproof channel indicators or indoor wall painting.

Description

technical field [0001] The invention relates to a single crystal for up-conversion luminescence, in particular to a terbium-ytterbium rare-earth ion double-doped yttrium-gadolinium-lithium fluoride single crystal and a preparation method. Background technique [0002] Different from the traditional typical luminescence process, up-conversion luminescence, namely: Anti-Stokes luminescence (Anti-Stokes), is that long-wavelength light excites certain materials to emit short-wavelength light. The up-conversion process requires many intermediate states to accumulate the energy of low-frequency excited photons. There are mainly three luminescence mechanisms: excited state absorption, energy conversion process, and photon avalanche. These processes are all realized by the continuous absorption of one or more photons by the energy levels of active ions doped in crystal particles, and those active ions with f electrons and d electrons are used because of their large number of metast...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B11/00C30B29/12
Inventor 夏海平符立董艳明李珊珊唐磊汪沛渊彭江涛张约品
Owner NINGBO UNIV
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