Controlled synthesis and optimization of submicron vaterite calcium carbonate particles: Correlating reaction parameters with polymorph selection and submicron particle size regulation--颗粒学报PARTICUOLOGY

Controlled synthesis and optimization of submicron vaterite calcium carbonate particles: Correlating reaction parameters with polymorph selection and submicron particle size regulation

Yue Sun^{a b c}, Shuxuan Wang^{b c}, Chunlai Yang^{b c d}, Yaru Qin^a *, Xingwu Zou^{b c *}, Bo Li ^{b c}, Fei Shao^{b c}

a Qinghai Provincial Key Laboratory of Nanomaterials and Technology, School of Chemistry and Materials Science, Qinghai Minzu University, Xining, 810007, China
b Key Laboratory of Green and High-end Utilization of Salt Lake Resources, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, Xining, 810008, China
c Qinghai Engineering and Technology Research Center of Comprehensive Utilization of Salt Lake Resources, Xining, 810008, China
d University of Chinese Academy of Sciences, Beijing, 100049, China

10.1016/j.partic.2026.04.008

Volume 114, July 2026, Pages 222-235

Received 3 February 2026, Revised 10 April 2026, Accepted 12 April 2026, Available online 30 April 2026, Version of Record 8 May 2026.

E-mail: yaruqin@qhmu.edu.cn; zouxingwu@isl.ac.cn

Highlights

• Novel valorization of industrial ammonia-stripped calcium liquor for sustainable vaterite synthesis.

• Systematic elucidation of key parameters regulating vaterite polymorph, particle size and stability.

• Establishes parameter-structure-property relationship via multi-characterization and situ monitoring.

• Achieves high-performance (0.69 μm, 25.73 nm mesopores) under mild optimal conditions.

• Provides an eco-efficient and scalable route for functional inorganic particles and waste recycling.

Abstract

This study employed an optimized solution mixing method using ammonia-stripped calcium liquor (industrial waste) as the calcium source, systematically investigating the effects of key parameters (reactant molar ratios, stirring rate, reaction time, temperature, etc.) on the crystal phase, morphology, and particle size of submicron vaterite calcium carbonate particles (vaterite PCC). Results showed that high-purity submicron-vaterite was obtained under optimal conditions: n(Ca²⁺):n(CO₃²⁻) = 1:3, stirring at 800 rpm, reaction at room temperature for 10 min, and Na⁺ additive with n(Na⁺):n(Ca²⁺) = 3:1. The product featured an average particle size of ∼0.69 μm, a narrow size distribution (Span = 0.44). Prolonged reaction time or increased temperature induced vaterite-to-calcite transformation. The selection of ammonia-stripped calcium liquor/CaCl₂ and (NH₄)₂CO₃ as Ca/C sources is for their stable Ca²⁺ release and mild CO₃²⁻ supply, and the formation of vaterite PCC is significantly affected by pH, heating conditions and water chemistry of the reaction system. This work provides a feasible route for industrial waste valorization and large-scale vaterite PCC production, with potential in medicine and functional additives.

Graphical abstract

Keywords

Vaterite; Solution mixing method; Submicron calcium carbonate; Polymorph control; Industrial waste valorization

文章导读