Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof

A technology of transparent ceramics and calcium fluoride, applied in the field of laser transparent ceramics preparation

Inactive Publication Date: 2012-09-19
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, factors such as grain boundaries, pores, compositional gradients, and incomplete lattices in ceramics increase the light scattering loss and reduce the light transmittance of the material, so reports on transparent ceramics doped with CaF2 Rarely, in 2006, Bensalah, A et al. reported the synthesis of CaF2 nanopowder with an average particle size of 20nm by the inverse microemulsion method, which laid the foundation for the next step of ceramic sintering (see literature Bensalah, A.; Mortier,M.; Patriarche, G.; Gredin, P.; Vivien, D., Synthesis and optical characterizations of undoped and rare-earth-doped CaF2 nanoparticles. J. Solid State Chem. 2006, 179, 2636-2644.), 2009 Aubry, P et al. successfully prepared Yb:CaF2 transparent ceramics and characterized their optical properties (see literature Aubry, P .; Bensalah, A.; Gredin, P.; Patriarche, G.; Vivien, D.; Mortier, M., Synthesis and optical characterizations of Yb-doped CaF2 ceramics. Opt. Mater. 2009, 31, 750-753.)

Method used

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  • Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof
  • Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof
  • Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0039] Weigh Ca(NO 3 ) 2 4H 2 O, Er(NO 3 ) 3 ·5H 2 O and KF 2H 2 O, respectively dissolved in deionized water, prepared as Ca with a molar concentration of 0.5 mol / L 2+ and Er 3+ cationic solution, the molar concentration is 0.5mol / L of F - Anionic solution, Ca in cationic solution 2+ and Er 3+ The molar content ratio is n(Ca 2+ ): n (Er 3+ )=95:5, and then the two solutions were quickly mixed and reacted. Er 3+ :CaF 2 The nanoparticle suspension was washed with deionized water, centrifuged three times, and then dried in vacuum at 75°C to obtain Er with a grain size of 15-50nm. 3+ :CaF 2 Nano powder. single doped Er 3+ :CaF 2 The nano-powder is loaded into a graphite mold and sintered in a vacuum hot-press furnace with a heating rate of 15°C / min, a sintering temperature of 800°C, a pressure of 30MPa, and a holding time of 60 minutes.

[0040] After the obtained samples were roughly ground with different types of sandpaper, they were polished on both sides on...

Embodiment 2

[0042] Er 3+ The blending amount is 5mol% of Er 3+ :CaF 2 The preparation of nanopowder is identical with embodiment 1 method, the Er of gained 3+ :CaF 2 Nano powder and NaF powder (Na + The ion content is 0.5mol%) is fully mixed in alcohol, and then dried to form a sintered powder. The sintered powder is sintered in a vacuum hot-press furnace, and the process parameters are the same as in Example 1.

[0043] After double-sided polishing of the obtained sample, the finished product of erbium-sodium co-doped calcium fluoride transparent ceramics was obtained, with a density of 99.9% and a transmittance of 83.998% at a wavelength of 1363nm. The luminous intensity of 1530nm under the excitation of 978nmLD changes with time, such as image 3 As shown in the curve in (b), the fitted fluorescence lifetime is 5.91ms.

Embodiment 3

[0045] Er 3+ The blending amount is 5mol% of Er 3+ :CaF 2 The preparation of nanopowder is identical with embodiment 1 method, the Er of gained 3+ :CaF 2 Nano powder and NaF powder (Na + The ion content is 1.0mol%) is fully mixed in alcohol, and then dried to form a sintered powder. The sintered powder is sintered in a vacuum hot-press furnace, and the process parameters are the same as in Example 1.

[0046] Gained samples are obtained after double-sided polishing to obtain erbium-sodium co-doped calcium fluoride transparent ceramic finished products such as figure 1 As shown, the density is 99.94%, and the transmittance of the sample is tested by the UV3600 ultraviolet-visible-near-infrared spectrophotometer of Japan Shimadzu Company, and the results are as follows figure 2 shown. The transmittance at the wavelength of 1363nm is 85.096%. The luminous intensity of 1530nm under the excitation of 978nmLD changes with time, such as image 3 As shown in the middle (c) ...

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Abstract

The invention provides an Er3+ and Na+cadoping CaF2 transparent ceramic and a preparation method thereof. The preparation method includes: synthesis of precursor powder and sintering and post-processing of the transparent ceramic. The precursor powder is prepared by adopting a direct precipitation method in water solution, grain size of the precursor powder is 15-50nm, synthetic Er3+: CaF2 nano powder and NaF powder are mixed with alcohol fully, and Er3+, Na+: CaF2 transparent ceramic is prepared by vacuum hot-pressing sintering. Maximum transmissivity of visible light and near-infrared wave band is 85.096%, the transparent ceramic has strong absorption peak at the positions of 377nm, 519nm and 654nm and has wind absorption belt at the positions of 975nm and 1530nm, and can be used as a working gain medium for infrared and up-conversion laser. The erbium sodium codoping calcium fluoride transparent ceramic and the preparation method of the erbium sodium codoping calcium fluoride transparent ceramic are simple to operate, ceramic sintering temperature is low, ceramic sintering time is short, and the Er3+, Na+: CaF2 transparent ceramic is long in fluorescent life time.

Description

technical field [0001] The present invention relates to a kind of Er 3+ and Na + Co-doped CaF 2 Transparent ceramics and preparation method thereof, the Er 3+ , Na + :CaF 2 The fluorescence lifetime of transparent ceramics is higher than that of single-doped Er 3+ :CaF 2 A transparent ceramic belongs to the technical field of laser transparent ceramic preparation. Background technique [0002] Er 3+ Doped laser materials have luminescent channels in the 1.5 μm and 2.9 μm wavelength bands that are in the safe range of human eyes. Lasers in this band can be widely used in optical communication, medical treatment, laser detection and ranging and other fields. In addition, Er 3+ Some laser bands of ions have cross-relaxation phenomenon under high-concentration doping, which is especially suitable for laser pumping, that is, cooperative up-conversion pumping, and is an up-conversion material with broad application prospects. [0003] The matrix material has a crucial in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/553C04B35/622
Inventor 梅炳初李小女宋京红李威威
Owner WUHAN UNIV OF TECH
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