超临界水热合成纳米钛酸钡结晶机理研究

张文进; 王树众; 刘慧; 刘辉; 陈双平; 邓雪涛; 杨健乔; 李紫成

doi:10.7652/xjtuxb202606019

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超临界水热合成纳米钛酸钡结晶机理研究

更新时间：2026-06-12

- 超临界水热合成纳米钛酸钡结晶机理研究
- Study of Crystallization Mechanism of Nano-BaTiO₃ by Supercritical Hydrothermal Synthesis
- 西安交通大学学报 2026年60卷第6期页码：223-233
- 作者机构：
  
  西安交通大学能源与动力工程学院，710049，西安
- 作者简介：
  
  作者简介：张文进（1998—），男，博士生；
  王树众（通信作者），男，教授，博士生导师。
- 基金信息：
  
  国家自然科学基金资助项目(52176162);陕西省重点研发计划资助项目。(2024GX-YBXM-314)
- DOI：10.7652/xjtuxb202606019
  中图分类号： TM912.9;O781
- 收稿：2025-09-19，
  
  纸质出版：2026-06-10
- 稿件说明：
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张文进, 王树众, 刘慧, 等. 超临界水热合成纳米钛酸钡结晶机理研究[J]. 西安交通大学学报, 2026,60(6):223-233.

ZHANG Wenjin, WANG Shuzhong, LIU Hui, et al. Study of Crystallization Mechanism of Nano-BaTiO₃ by Supercritical Hydrothermal Synthesis[J]. Journal of Xi'an Jiaotong University, 2026, 60(6): 223-233. DOI: 10.7652/xjtuxb202606019.
张文进, 王树众, 刘慧, 等. 超临界水热合成纳米钛酸钡结晶机理研究[J]. 西安交通大学学报, 2026,60(6):223-233. DOI： 10.7652/xjtuxb202606019.

ZHANG Wenjin, WANG Shuzhong, LIU Hui, et al. Study of Crystallization Mechanism of Nano-BaTiO₃ by Supercritical Hydrothermal Synthesis[J]. Journal of Xi'an Jiaotong University, 2026, 60(6): 223-233. DOI: 10.7652/xjtuxb202606019. DOI：

摘要

针对传统方法制备钛酸钡纳米粉体存在粒径可控性差、团聚严重与四方相含量受限等问题，依托连续流超临界水热合成装置，阐明了反应温度对纳米钛酸钡结晶行为的调控规律与机理，建立了成核速率与超临界过饱和度的量化关系，并确定了获得高四方相与窄分布粒径的最优温区。采用X射线衍射、扫描电子显微镜、透射电子显微镜和拉曼光谱对产物进行晶型、结晶度和粒径分布表征，结果表明：反应温度通过影响超临界水的物化性质，显著影响钛酸钡的结晶度、晶粒尺寸和晶相组成，主导钛酸钡的成核-生长竞争机制，其中最佳反应温度范围为380～400℃，可实现高四方相含量、小晶粒尺寸和窄粒径分布；超临界水的高过饱和度、低黏度和高扩散系数共同提高了成核速率，有效抑制了晶粒生长，实现了纳米级粒径控制；超临界水热合成过程中，随着温度升高，钛酸钡的结晶由均相成核逐渐向非均相成核转变，晶粒生长受扩散和团聚动力学共同调控。该研究为高性能纳米钛酸钡的可控合成提供了新思路，对高致密度和高介电电子陶瓷的关键粉体原料设计具有一定的指导意义。

Abstract

To address the challenges of poor particle size controllability，severe agglomeration，and limited tetragonal phase content in the conventional synthesis of BaTiO

nanoparticles，a continuous flow supercritical hydrothermal synthesis apparatus was employed to elucidate the regulatory effects and mechanisms of reaction temperature on the crystallization behavior of nanoBaTiO

，establish a quantitative relationship between nucleation rate and supercritical supersaturat

ion，and determine the optimal temperature window for obtaining high tetragonal-phase fraction and narrow particle size distribution.The products were characterized by X-ray diffraction，scanning electron microscopy，transmission electron microscopy，and Raman spectroscopy to assess crystal phase composition，crystallinity，and particle size distribution.The results indicated that reaction temperature，by altering the physicochemical properties of supercritical water，significantly affected the crystallinity，grain size，and phase composition of BaTiO

and dominated the nucleation-growth competition mechanism；an optimal reaction temperature range of 380-400℃was identified in which high tetragonal-phase content，small grain size，and narrow particle size distribution were achieved. The high supersaturation，low viscosity，and high diffusivity of supercritical water were found to jointly increase the nucleation rate，effectively suppress grain growth，and enable nanoscale particle size control.During the supercritical hydrothermal synthesis，with increasing temperature，the crystallization mode of BaTiO

was observed to shift from homogeneous nucleation toward heterogeneous nucleation，and grain growth was governed by both diffusion and agglomeration kinetics.This study provides new insights for the controllable synthesis of high-performance nano-BaTiO

and offers guidance for the design of key powder precursors for high-density，high-dielectric electronic ceramics.

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