Preparation method of Er<3+> and Yb<3+> co-doped YOF red up-conversion fluorescent material

Abstract

The invention provides a preparation method of an Er<3+> and Yb<3+> co-doped YOF red up-conversion fluorescent material. The preparation method is low in heat treatment temperature, relatively wide in temperature adjusting range and simple in process. The preparation method specifically comprises the following steps: mixing yttrium nitrate, ytterbium nitrate and erbium nitrate according to a general formula mixing ratio; taking isopropanol, ethanol and water as a solvent, adding trifluoroacetic acid into the solvent, and stirring uniformly to obtain a transparent sol A; drying the transparent sol A to obtain a colloidal substance for heat treatment; heating from room temperature to 350-600DEG C, keeping the temperature for a certain period of time, cooling to the room temperature along with a furnace, and grinding to obtain Er<3+> and Yb<3+> co-doped YOF powder; or coating the transparent sol A on a glass or silicon chip substrate by virtue of a rotary coating method, drying in the air for 15-30 minutes at room temperature, then drying in a drying box at 100DEG C, then putting into a high-temperature furnace to perform annealing treatment, heating to 350-600DEG C according to a heating rate of 1-10DEG C / min, and performing heat preservation and cooling to obtain an Er<3+> and Yb<3+> co-doped YOF fluorescent thin film.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth doped luminescent materials, in particular to an Er 3+ , Yb 3+ The preparation method of co-doped YOF red up-conversion fluorescent material. Background technique [0002] In the development of up-conversion photoluminescent fluorescent materials, the host material is the key factor affecting the up-conversion luminous efficiency. At present, the hosts of up-conversion fluorescent materials with high luminous efficiency mainly include fluoride, oxide, and oxyfluoride. Due to the lower phonon energy of fluoride, the occurrence of non-radiative relaxation is greatly reduced, and the light lifetime of the metastable energy level of rare earth ions is improved, so the luminous efficiency of rare earth is effectively improved, but the mechanical properties of fluoride The strength and chemical stability are poor, special equipment and conditions are required for preparation, and the...

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Problems solved by technology

Due to the lower phonon energy of fluoride, the occurrence of non-radiative relaxation is greatly reduced, and the light lifetime of the metastable energy level of rare earth ions is improved, so the luminous efficiency of rare earth is effectively improved, but the mechanical properties of fluoride The strength and chemical stability are poor, special equipment and conditions are required for preparation, and there are many problems in practical application; the oxide matrix has good mechanical strength and chemical stability, but the phonon energy is large, so the luminescence performance is poor; and oxyfluoride has both fluorine The high up-conversion luminous efficiency of the compound matrix and the mechanical strength and stability of the oxide matrix, and easy processing, is a kind of up-conversion fluorescent material matrix with good comprehensive performance.

[0003] Among rare earth ion-doped up-conversion photoluminescence fluorescent materials, green up-conversion fluorescent materials are relatively high luminous efficiency and widely studied fluorescent materials. Among them, Yb 3+ As a sensitizer, Er 3+ As an activator, through Yb 3+ →Er 3+ The energy transfer between can achieve effective infrared-visible upconversion photoluminescence efficiency, Er 3+ ,Yb 3+ Most of the co-doped upconversion fluorescent materials belong to the green emission mechanism, while the Er 3+ ,Yb 3+ Co-doped red up-conversion fluorescent materials have been less studied, and the efficiency is low and the color purity is not high

[0004] In the Chinese patent with publication number CN103450902A, the inventor aged the mixture of Y, Yb and Er hydrochloride solution and ammonium bicarbonate to obtain a white powder, and then heated the white powder at 1200°C Calcined for 3 hours to obtain a white solid, then added lithium fluoride and ammonium bifluoride for mixing and grinding to obtain a precursor, and finally calcined the precursor at 800°C for 3 hours, cooled to obtain a red up-conversion material Y 3.9 Yb 1 Er 0.1 o 4 f 7 , this method prepares Er 3+ ,Yb 3+ A small amount of YF 3 , which will affect the color purity of red light, and the preparation process is cumbersome, requiring high-temperature calcination, which consumes a lot of energy

[0005] Chinese patent CN101195747A discloses a hydrothermal method for preparing red up-conversion phosphor NaY 1-x-y-z (Yb x Ho y Ce z )F 4 Although the synthesis temperature is only 180~220°C, the production cycle is long, the production cost is high, and the red light emission is enhanced through the quenching effect of Ce, which will cause the overall luminous intensity to decrease.

By this method, Er can be obtained 3+ ,Yb 3+ Co-doped YOF red light up-conversion fluorescent materials, but this method has relatively high requirements for equipment, and the control of experimental technical conditions is also relatively harsh, the preparation process is cumbersome, and it is not suitable for large-scale production

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