Growth and Spectral Property of KTb3F10 Single Crystal

doi:10.15541/jim20250230

Abstract

Abstract:

KTb₃F₁₀ (KTF) crystal, characterized by its high Tb³⁺ ion concentration, low thermo-optic coefficient and low phonon energy, exhibits significant potential for efficient laser emission in the green and yellow wavelength ranges. However, challenges such as incongruent melting behavior, hygroscopicity of raw materials, high-temperature compositional volatility, and corrosive nature of fluorides have severely hindered the growth of high-quality KTF crystals. This study aims to develop an effective approach to address these issues, achieve the growth of high-quality KTF crystals, and characterize their optical properties. An optimized vertical Bridgman method integrated with a laser-sealed platinum crucible technique under vacuum was employed. This innovative approach effectively shielded the raw materials from water and oxygen contamination while suppressing compositional deviation during crystal growth through a sealed environment. As a result, blank KTF crystals with dimensions of φ16 mm×30 mm were successfully grown, and their relevant spectral properties were characterized. X-ray rocking curve of the (111) plane showed a full width at half maximum of 0.08°, indicating high crystalline perfection. Thermal analysis indicated significant volatilization of KTF at high temperatures. Spectral tests revealed an average transmittance of >90% in the 400-1600 nm range and an absorption coefficient of <0.007 cm^-1 at 1064 nm, demonstrating minimal optical loss suitable for high-power laser applications. Fluorescence lifetime was 4.82-4.99 ms for the Tb³⁺ion at the ⁵D₄ energy level, which is 3-5 times longer than that in oxide matrices. This superiority is attributed to the suppression of non-radiative relaxation by the low-phonon fluoride matrix, enhancing the energy storage efficiency for laser emission. Based on above data, this study has successfully established a viable growth method for KTF crystals, providing a new technical pathway for the controllable synthesis of KTF and other ternary fluoride materials. All these results provide valuable insights for the high-efficiency application of KTF crystals in yellow-green laser emission.

Key words: KTb₃F₁₀, vertical Bridgman method, spectral property, fluorescence lifetime

CLC Number:

LIU Guojin, HUANG Changbao, YU Xuezhou, QI Huabei, HU Qianqian, NI Youbao, WANG Zhenyou, WU Haixin. Growth and Spectral Property of KTb₃F₁₀ Single Crystal[J]. Journal of Inorganic Materials, 2026, 41(3): 370-376.

Figures/Tables 13

Fig. 1 Phase diagram of KF-TbF3 binary systems[23]

Fig. 2 Results of KTF crystal growth (a) KTF blank crystal sliced along the central axis; (b) Oriented (111) plane sample

Fig. 3 Cell structure of KTF crystal[26]

Fig. 4 XRD patterns and Rietveld refinement results of KTF single crystal powder

Table 1 Crystallographic data from structural refinement of KTF single crystal

Cell parameter	a/nm	V/nm³	Density/(g·cm^-3)	R_wp/%	R_p/%	χ²
KTF single crystal	1.1662(4)	1.58591(16)	5.478	11.05	7.48	1.41
PDF#04-006-4631	1.168	1.59341	5.885	11.05	7.48	1.41

Fig. 5 X-ray rocking curve of (111) plane for KTF single crystal

Fig. 6 TG-DSC thermal analysis curves of KTF single crystal

Fig. 7 UV-Vis-NIR transmission spectrum of KTF single crystal

Fig. 8 Absorption spectrum of KTF single crystal

Fig. 9 Energy levels and characteristic transitions of Tb3+ ions

Fig. 10 Fluorescence emission spectra of Tb3+ in KTF crystal Colorful figure is available on website

Fig. 11 Fluorescence decay curves of KTF crystal under 351 nm excitation at different emission wavelengths (a) 488 nm; (b) 545 nm; (c) 584 nm; (d) 622 nm. All curves were fitted using a single-exponential function

Table 2 Energy level 5D4 lifetime (τexpt) of Tb3+ in different crystals

Crystal	τ_expt/ms	Ref.	Crystal	τ_expt/ms	Ref.
KTb₃F₁₀	4.82-4.99	This work	Tb: KY₃F₁₀	4.8	[11]
Tb_0.81Ca_0.19F_2.81	6.9	[30]	Tb: Y₂Mg₂Al₂Si₂O₁₂	0.58-1.72	[32]
Tb: LiYF₄	4.9	[31]	Tb: SrGd₂Al₂O₇	1.56-2.80	[33]
Tb: LiLuF₄	~5.0	[8]

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Growth and Spectral Property of KTb₃F₁₀ Single Crystal

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