微通道合成法制备高纯四方相钛酸钡的工艺研究

谭玲; 胥金秀; 李道玉; 黄森虹; 王小慧; 胡一杰; 辛亚男

doi:10.7513/j.issn.1004-7638.2025.01.012

微通道合成法制备高纯四方相钛酸钡的工艺研究

doi: 10.7513/j.issn.1004-7638.2025.01.012

谭玲^{1, 2,},
胥金秀^{1, 2},
李道玉^{1, 2},
黄森虹^{1, 2},
王小慧^{1, 2},
胡一杰^{1, 2},
辛亚男^{1, 2, ,}

1.
攀钢集团研究院有限公司, 钒钛资源综合利用国家重点实验室, 四川攀枝花 617000
2.
成都先进金属材料产业技术研究院股份有限公司, 四川成都 610305

详细信息

作者简介:
谭玲，1993年出生，女，四川巴中人，博士研究生，从事纳米粉体制备及应用性能研究，E-mail：tanling1009@163.com

通讯作者:
辛亚男，1989年出生，男，山东聊城人，博士，正高级工程师，从事钒钛基功能材料开发研究，E-mail：917031125@163.com

中图分类号: TF123,TQ174
计量
- 文章访问数: 57
- HTML全文浏览量: 23
- PDF下载量: 12
- 被引次数: 0
出版历程
- 收稿日期: 2023-11-03
- 刊出日期: 2025-02-27

Preparation of high purity tetragonal barium titanate by microchannel synthesis method

TAN Ling^{1, 2
,},
XU Jinxiu^{1, 2},
LI Daoyu^{1, 2},
HUANG Senhong^{1, 2},
WANG Xiaohui^{1, 2},
HU Yijie^{1, 2},
XIN Yanan^{1, 2
, ,}

1.
State Key Laboratory of Vanadium and Titanium Resources Comprehensive Utilization, Pangang Group Research Institute Co., Ltd., Panzhihua 617000, Sichuan, China
2.
Department of Advanced Functional Materials, Chengdu Institute of Advanced Metallic Material Technology and Industry Co., Ltd., Chengdu 610305, Sichuan, China

摘要

摘要: 四方相钛酸钡的工业生产方法主要为固相法和水热合成法，但存在颗粒大、粒径分布不均匀及四方相含量低等问题。以氯化钡、氯化钛和草酸为原料，采用微通道合成法成功制备了四方相钛酸钡粉末，并与传统共沉淀法进行了对比。XRD、SEM及TEM结果均表明，以微通道合成法制备的产品纯度更高、粒径更小、颗粒分布更均匀，其平均粒径可达110 nm左右，粒径分布范围仅为±16 nm。该方法工艺简单、易于实现批量生产，为高纯度、小尺寸四方相钛酸钡的工业化生产奠定基础。
- 微通道合成法 /
- 四方相 /
- 钛酸钡 /
- 高纯度 /
- 小粒径
Abstract: The industrial technologies of tetragonal barium titanate mainly include solid-state method and hydrothermal synthesis method, but there are problems such as large particles, uneven particle size distribution, and low tetragonal phase content. Tetragonal barium titanate was successfully prepared by microchannel synthesis method using barium chloride, titanium chloride, and oxalic acid as raw materials, as well as compared with traditional co-precipitation method. The results of XRD, SEM and TEM indicate that the product is a high-purity, small particle size, and uniformly distributed tetragonal barium titanate, with an average particle size of 110 nm and a particle size distribution range of ± 16 nm. This method with simple synthesis process is easy to achieve mass production and lays the industrial production of high-purity and small-sized tetragonal barium titanate.
- microchannel synthesis method /
- tetragonal /
- barium titanate /
- high purity /
- small particle size

HTML全文

图 1 （a）微通道合成法流程示意及（b）微通道反应器实物

Figure 1. Schematic diagram of microchannel synthesis process (a) and microchannel reactor (b)

下载: 全尺寸图片幻灯片

图 2 不同方法/条件合成钛酸钡样品的XRD谱图

Figure 2. XRD patterns of BaTiO₃ by different methods or conditions

下载: 全尺寸图片幻灯片

图 3 传统共沉淀法(a)~(c)顺流，（d)~(f）并流所得钛酸钡样品SEM图

Figure 3. SEM images of BaTiO₃ with traditional coprecipitation methods by down-flow(a, b, c) and co-current flow (d, e, f)

下载: 全尺寸图片幻灯片

图 4 微通道合成法（a)~(c)草酸正常量，（d)~(f）草酸大大过量所得钛酸钡样品SEM图

Figure 4. SEM images of BaTiO₃ by microchannel synthesis method with normal amount of oxalic acid (a, b, c)and with a significant excess of oxalic acid (d, e, f)

下载: 全尺寸图片幻灯片

图 5 草酸大大过量时微通道合成法所得钛酸钡样品及其元素分布

Figure 5. The BaTiO₃ by microchannel synthesis method with a significant excess of oxalic acid and its element distribution

下载: 全尺寸图片幻灯片

表 1 钛酸钡样品的XRD谱图数据拟合结果

Table 1. Fitting results of XRD patterns of BaTiO₃ nm

类别	传统共沉淀法		微通道法
类别	顺流	并流	草酸正常量	草酸过量
a	0.39954	0.39954	0.39968	0.39966
b	0.39954	0.39954	0.39968	0.39966
c	0.40301	0.40305	0.40272	0.40277

下载: 导出CSV

表 2 钛酸钡样品粒径统计结果

Table 2. The statistical results of particle size of BaTiO₃ nm

类别	平均粒径	粒径最小值	粒径最大值	标准差
传统共沉淀法-顺流	232	114	385	71
传统共沉淀法-并流	253	137	484	66
微通道法-草酸正常量	133	83	183	23
微通道法-草酸过量	111	75	145	16

下载: 导出CSV

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