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Growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals

A growth method, single crystal technology, applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., to achieve the effect of saving electricity costs, facilitating large-scale industrial production, and good quality

Inactive Publication Date: 2015-01-07
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, there is no α-NaYF at home and abroad so far 4 with β-NaYF 4 Efficient growth method for large-sized single crystals reported

Method used

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  • Growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals
  • Growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals
  • Growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals

Examples

Experimental program
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Effect test

Embodiment 1

[0021] According to NaF:KF:YF 3 The molar ratio is 1.25:1.00:2.48, and the NaF raw material with a purity greater than 99.99%, the KF raw material with a purity of 99.99%, and the YF raw material with a purity of 99.99% are weighed respectively. 3 The raw materials are mixed and placed in a mill, and ground and mixed for 5.5 hours to obtain a uniform powder mixture; the mixture is fluffy placed in a boat-shaped platinum crucible, and then the boat-shaped platinum crucible is installed in the tube-type resistance furnace Platinum piping, then high-purity N 2 Gas removes the air in the platinum pipe, and conducts leak detection on the platinum pipe; then gradually raises the temperature of the furnace body of the tubular resistance furnace to 790°C, passes HF gas, and reacts for 2 hours to remove possible H 2 O and oxyfluoride, during the reaction process, use NaOH solution to absorb HF gas in the tail gas. After the reaction, stop passing HF gas, close the tube resistance furn...

Embodiment 2

[0026] Basically the same as Example 1, the difference is only raw material NaF: KF: YF 3 The molar ratio is 1:1:2.24, weighed and mixed, placed in a mill, milled and mixed for 5 hours, the reaction time with HF gas in the platinum pipeline is 5 hours, the furnace temperature is 950°C, and the inoculation temperature is 820°C , the temperature gradient at the solid-liquid interface is 50° C. / cm, the crystal growth rate is 0.2 mm / h, and the furnace temperature drop rate is 80° C. / h. The XRD pattern and transmission spectrum of the crystal are basically the same as in Example 1.

Embodiment 3

[0028] Basically the same as Example 1, the difference is only raw material NaF: KF: YF 3 The molar ratio is 2.40:1:3.40, weighed and mixed, placed in a mill, milled and mixed for 6 hours, the reaction time with HF gas in the platinum pipeline is 1 hour, the furnace temperature is 980°C, and the inoculation temperature is 860°C. The temperature gradient at the solid-liquid interface is 90°C / cm, the crystal growth rate is 2.0mm / h, and the furnace temperature drop rate is 20°C / h. The XRD pattern and transmission spectrum of the crystal are basically the same as in Example 1.

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Abstract

The invention discloses a growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals. The growth method is characterized in that the alpha-NaYF4 monocrystals are obtained through Steps (1)-(4); KF (potassium fluoride) is added in Step (1) as a cosolvent; in Step (2), raw materials are treated with HF (hydrogen fluoride) treatment for 1 to 5 hours at a high temperature ranging from 780 DEG C to 800 DEG C; a Pt (platinum) crucible is sealed in Step (3); in Step (4), the crystal growth is carried out through the Bridgman-Stockbarger Method with the cosolvent, that is, the sealed Pt crucible is placed in a molybdenum disilicide rod electric furnace to carry out the crystal growth through the Bridgman-Stockbarger Method; the crystal growth parameters are as follows: the furnace body temperature ranges from 950 DEG C to 980 DEG C, the inoculation temperature ranges from 820 DEG C to 860 DEG C, the temperature gradient of the solid-liquid interphase ranges from 50 DEG C per centimeter to 90 DEG C per centimeter, and the crucible descending speed ranges from 0.2 millimeter per hour to 2.0 millimeters per hour; after the crystal growth is completed, the furnace temperature is reduced to the room temperature at a rate of 20 to 80 DEG C per hour, so that the alpha-NaYF4 monocrystals with a larger size and a higher quality can be obtained. The growth method has the advantage that the transmittances of the crystals within the waveband of 200 to 8,700 nanometers all exceed 80 percent, so that the alpha-NaYF4 crystals achieve wider application prospects for mid-infrared optical devices.

Description

technical field [0001] The present invention relates to crystal growth, in particular to a cubic phase sodium yttrium fluoride (α-NaYF 4 ) single crystal growth method. Background technique [0002] NaYF 4 It is an excellent optical matrix material discovered in recent decades. It has the characteristics of low phonon energy, high luminous efficiency doped with rare earth ions, high transmittance in visible and infrared bands, and stable physical and chemical properties. In NaYF 4 Doped with rare earth ions in the matrix, NaYF 4 Combining the excellent optical properties of ions with the specificity of rare earth active ions, new materials with many excellent properties are obtained. In normal state, it has cubic phase (α-NaYF 4 ) and the hexagonal phase (β-NaYF 4 ) two crystal structures. For example, in the hexagonal phase β-NaYF 4 As the host, Yb and Er co-doped β-NaYF 4 The material is one of the up-conversion luminescent materials with the highest up-conversion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/12C30B11/00
CPCC30B29/12C30B11/00
Inventor 夏海平杨硕姜永章张加忠符立董艳明李珊珊张约品
Owner NINGBO UNIV
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