Preparation Process of Ultra-High Purity Rare Earth Yttrium Fluoride

doi:10.19894/j.issn.1000-0518.250345

Chinese Journal of Applied Chemistry ›› 2025, Vol. 42 ›› Issue (12): 1608-1618.DOI: 10.19894/j.issn.1000-0518.250345

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Preparation Process of Ultra-High Purity Rare Earth Yttrium Fluoride

Xin-Yu WANG¹, Yang YU¹, Long TIAN¹, Fan-Ming ZENG², Valery-Konstantinovich SHELEG³, Marina-Anatolyevna KRAVCHUK³, Shu-Yan SONG¹(), Jing FENG¹(), Hong-Jie ZHANG¹()

^1.China-Belarus Belt and Road Joint Laboratory on Advanced Materials and Manufacturing，Changchun Institute of Applied Chemistry，Chinese Academy of Sciences，Changchun 130022，China
^2.Jilin Technology College of Electronic Information，Jilin 132021，China
^3.Belarusian National Technical University，Minsk 220013，Belarus

Received:2025-09-04 Accepted:2025-09-24 Published:2025-12-01 Online:2025-12-30
Contact: Shu-Yan SONG,Jing FENG,Hong-Jie ZHANG
Supported by:
the Strategic Priority Research Program of the Chinese Academy of Sciences(XDB1220000);the Financial Aid from the National Key Research and Development Program of China(2023YFB3507401);the Open Project of the Key Laboratory of Laser Device Technology of China North Industries Group Corporation Limited(KLLDT202313);the Changchun Science and Technology Development Plan Project(Z3GZZ09);the Open Topic Project of the Rare Earth Advanced Materials Technology Innovation Center （No.G2025-K-26（33）-48（70）） and the Joint Project(5EF0BC29)

Abstract

Abstract:

This paper conducts a systematic study on the preparation process of ultra-high-purity yttrium fluoride （YF₃）， with a focus on the pretreatment of raw materials and the screening of the optimal fluorinating agent. By altering parameters such as the ball milling time， rotational speed， and sintering temperature of Y₂O₃， and combining characterization methods including X-ray diffraction （XRD）， thermogravimetric analysis （TGA）， particle size testing， and Zeta potential measurement， the optimal pretreatment conditions were determined. The pretreated Y₂O₃ powder was subjected to fluorination with three fluorinating agents， namely NH₄HF₂， HF gas and KF. The properties of YF₃ prepared using different fluorinating agents were systematically compared via various characterization methods， including XRD， X-ray photoelectron spectroscopy （XPS）， TGA， particle size analysis， Zeta potential measurement， scanning electron microscopy （SEM）， inductively coupled plasma-mass spectrometry （ICP-MS）， and oxygen content determination. The results show that the YF₃ prepared using HF gas as the fluorinating agent exhibits the optimal comprehensive performance， with a complete crystal structure and adequate fluorination degree. The mass fractions of Fe， Nd and Cr impurities are 0.0021%， 0.0002%， and 6.65×10^-6%， respectively， while the mass fraction of oxygen is only 0.0052%. Moreover， the particles are well-dispersed with no obvious agglomeration. This research not only achieves raw material conservation and cost reduction but also successfully prepares ultra-high-purity yttrium fluoride applicable to high-end technical fields， providing a research gramework for the preparation of ultra-high-purity YF₃.

Key words: Ultra-high purity rare earth yttrium fluoride, Preparation of fluoride, Impurity content

CLC Number:

O614

Xin-Yu WANG, Yang YU, Long TIAN, Fan-Ming ZENG, Valery-Konstantinovich SHELEG, Marina-Anatolyevna KRAVCHUK, Shu-Yan SONG, Jing FENG, Hong-Jie ZHANG. Preparation Process of Ultra-High Purity Rare Earth Yttrium Fluoride[J]. Chinese Journal of Applied Chemistry, 2025, 42(12): 1608-1618.

Figures/Tables 11

Fig.1 XRD patterns of Y2O3 at different sintering temperatures （A） and a magnified view of 28.5~30（°） area （B）

Fig.2 TG-DSC curves of Y2O3

Fig.3 Particle size distribution diagram （A） and Zeta potential diagram （B） of Y2O3 at different sintering temperatures

Fig.4 Particle size distribution diagram of Y2O3 at 1300 ℃ under different ball milling times （A） and Zeta potential diagram （B）； Particle size distribution diagram of Y2O3 at 1300 ℃ under different rotational speeds （C） and Zeta potential diagram （D）

Fig.5 XRD patterns of YF3 prepared with three fluorinating agents

Fig.6 XPS spectra of YF3 prepared with NH4HF2 as the fluorinating agent： Y3d （A）， F1s （B） and survey （C）； XPS spectra of YF3 prepared with HF as the fluorinating agent： Y3d （D）， F1s （E） and survey （F）

Fig.7 Thermogravimetric curves of YF3 prepared with different fluorinating agents

Fig.8 Particle size distribution diagram （A） and Zeta potential diagram （B） of YF3 prepared with different fluorinating agents

Fig.9 Scanning electron microscope images of YF3 prepared with different fluorinating agents： NH4HF2 （A）， HF （B） and KF （C）

Table 1 Mass fraction of transition metals in YF3

YF₃	w（Fe）/%	w（Nd）/%	w（Cr）/%
Y₂O₃+NH₄HF₂	0.003 0	0.000 2	5.29×10^-6
Y₂O₃+HF	0.002 1	0.000 2	4.58×10^-6
Y₂O₃+KF	0.004 2	0.000 9	6.65×10^-6

Table 2 Analysis of oxygen content in YF3 prepared with different fluorinating agents

Preparation of YF₃ using different fluorinating agents	w（O）/%				Average/%
Y₂O₃+NH₄HF₂	0.007 1	0.005 5	0.008 6	0.006	0.006 8
Y₂O₃+HF	0.004 3	0.006 2	0.006 2	0.004 1	0.005 2
Y₂O₃+KF	0.018 2	0.013 4	0.015 4	0.010 4	0.014 4

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Preparation Process of Ultra-High Purity Rare Earth Yttrium Fluoride

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