Carbonate-Suppressed Hydrothermal Synthesis of Tetragonal BaTiO3 Nanoparticles

Woo Jun Sung; Tae Yeong Song; Do-Kyun Kwon

doi:10.3740/MRSK.2025.35.12.574

All Issue

2025 Vol.35, Issue 12 Preview Page Next Page

Research Paper

Carbonate-Suppressed Hydrothermal Synthesis of Tetragonal BaTiO₃ Nanoparticles

27 December 2025. pp. 574-581

PDF XML

Abstract

We demonstrate a carbonate-suppressed hydrothermal route for synthesizing tetragonal BaTiO₃ (BT) nanoparticles using barium acetate as the Ba source. Commercial TiO₂ (P25) was converted to BT in KOH at 240 °C for 6 h without post-annealing. Relative to conventional Ba(OH)₂ routes, the acetate precursor markedly reduced BaCO₃ formation and narrowed the particle-size distribution. Systematic tuning of the Ba/Ti ratio (≥ 1.3) further optimized nucleation and growth, yielding uniform ~100 nm particles at Ba/Ti = 1.7 with the highest tetragonality (c/a ≈ 1.0076), as verified by XRD (002/200 splitting) and corroborated by Raman signatures of the tetragonal phase. Trace carbonate, when present, could be removed by mild weak-acid washing (e.g., acetic or citric acid) as effectively as with strong acids, but with improved process safety and practicality. The combined use of barium acetate, controlled Ba/Ti chemistry, and gentle carbonate removal yields phase-pure, highly tetragonal BT nanoparticles from low-cost precursors in a short dwell time, offering a scalable pathway to MLCC-grade powders.

Keywords

barium titanate (BaTiO₃)

hydrothermal synthesis

tetragonality

nanoparticles

carbonate suppression

References

Z. Tian, X. Wang, L. Shu, T. Wang, T.-H. Song, Z. Gui and L. Li, J. Am. Ceram. Soc., 92, 830 (2009).

10.1111/j.1551-2916.2009.02979.x

K. Hong, T. H. Lee, J. M. Suh, S.-H. Yoon and H. W. Jang, J. Mater. Chem. C, 7, 9782 (2019).

10.1039/C9TC02921D

D.-H. Yoon, J. Ceram. Process. Res., 7, 343 (2006).

A. Beauger, J. C. Mutin and J. C. Niepce, J. Mater. Sci., 18, 3041 (1983).

10.1007/BF00700786

M. Stockenhuber, H. Mayer and J. A. Lercher, J. Am. Ceram. Soc., 76, 1185 (1993).

10.1111/j.1151-2916.1993.tb03738.x

G. J. Choi, S. K. Lee, K. J. Woo, K. K. Koo and Y. S. Cho, Chem. Mater., 10, 4104 (1998).

10.1021/cm980520h

M. H. Frey and D. A. Payne, Chem. Mater., 7, 123 (1995).

10.1021/cm00049a019

H. P. Beck, W. Eiser and R. Haberkorn, J. Eur. Ceram. Soc., 21, 687 (2001).

10.1016/S0955-2219(00)00270-3

H. Shimooka and M. Kuwabara, J. Am. Ceram. Soc., 79, 2983 (1996).

10.1111/j.1151-2916.1996.tb08739.x

J. O. Eckert Jr, C. C. Hung‐Houston, B. L. Gersten, M. M. Lencka and R. E. Riman, J. Am. Ceram. Soc., 79, 2929 (1996).

10.1111/j.1151-2916.1996.tb08728.x

C.-T. Xia, E.-W. Shi, W.-Z. Zhong and J.-K. Guo, J. Eur. Ceram. Soc., 15, 1171 (1995).

10.1016/0955-2219(95)00101-8

M. Wu, J. Long, G. Wang, A. Huang, Y. Luo, S. Feng and R. Xu, J. Am. Ceram. Soc., 82, 3254 (1999).

10.1111/j.1151-2916.1999.tb02235.x

M. Li, L. Gu, T. Li, S. Hao, F. Tan, D. Chen, D. Zhu, Y. Xu, C. Sun and Z. Yang, Crystals, 10, 202 (2020).

10.3390/cryst10030202

E. Ciftci, M. N. Rahaman and M. Shumsky, J. Mater. Sci., 36, 4875 (2001).

10.1023/A:1011828018247

K. H. Ahn, Y.-H. Lee, M. Kim, H.-S. Lee, Y.-S. Youn, J. Kim and Y.-W. Lee, Ind. Eng. Chem. Res., 52, 13370 (2013).

10.1021/ie401161x

J.-M. Han, M.-R. Joung, J.-S. Kim, Y.-S. Lee, S. Nahm, Y.-K. Choi and J.-H. Paik, J. Am. Ceram. Soc., 97, 346 (2014).

10.1111/jace.12755

J. J. Lee, K. J. Park, K. H. Hur, S. C. Yi and S. M. Koo, J. Am. Ceram. Soc., 89, 3299 (2006).

10.1111/j.1551-2916.2006.01220.x

P. Pinceloup, C. Courtois, A. Leriche and B. Thierry, J. Am. Ceram. Soc., 82, 3049 (1999).

10.1111/j.1151-2916.1999.tb02201.x

S. K. Lee, T. J. Park, G. J. Choi, K. K. Koo and S. W. Kim, Mater. Chem. Phys., 82, 742 (2003).

10.1016/j.matchemphys.2003.07.003

C. Chen, H. Hao, T. Wang, J. Cheng, Z. Luo, L. Zhang, M. Cao, Z. Yao and H. Liu, Ceram. Int., 45, 7166 (2019).

10.1016/j.ceramint.2018.12.223

P. K. Dutta, R. Asiaie, S. A. Akbar and W. Zhu, Chem. Mater., 6, 1542 (1994).

10.1021/cm00045a011

D. Santa Cruz-Navarro, V. Mugica-Alvarez, M. Gutierrez-Arzaluz and M. Torres-Rodriguez, Appl. Sci., 10, 863 (2020).

10.3390/app10030863

S. Urek and M. Drofenik, J. Eur. Ceram. Soc., 18, 279 (1998).

10.1016/S0955-2219(97)00138-6

T.-M. Usher, B. Kavey, G. Caruntu and K. Page, ACS Appl. Nano Mater., 3, 9715 (2020).

10.1021/acsanm.0c01809

H. Zheng, K. Zhu, Q. Wu, J. Liu and J. Qiu, J. Cryst. Growth, 363, 300 (2013).

10.1016/j.jcrysgro.2012.11.019

X. Zhu, Z. Zhang, J. Zhu, S. Zhou and Z. Liu, J. Cryst. Growth, 311, 2437 (2009).

10.1016/j.jcrysgro.2009.02.016

H.-W. Lee, S. Moon, C.-H. Choi and D. K. Kim, J. Am. Ceram. Soc., 95, 2429 (2012).

10.1111/j.1551-2916.2012.05085.x

H. Hayashi, T. Nakamura and T. Ebina, J. Phys. Chem. Solids, 74, 957 (2013).

10.1016/j.jpcs.2013.02.010

Y. Shiratori, C. Pithan, J. Dornseiffer and R. Waser, J. Raman Spectrosc., 38, 1288 (2007).

10.1002/jrs.1764

İ. Kaya, V. Kalem and H. Akyildiz, Int. J. Appl. Ceram. Technol., 16, 1557 (2019).

10.1111/ijac.13225

R. Ashiri, Vib. Spectrosc., 66, 24 (2013).

Information

Publisher :Materials Research Society of Korea
Publisher(Ko) :한국재료학회
Journal Title :Korean Journal of Materials Research
Journal Title(Ko) :한국재료학회지
Volume : 35
No :12
Pages :574-581
Received Date : 2025-11-12
Revised Date : 2025-11-30
Accepted Date : 2025-12-01
DOI :https://doi.org/10.3740/MRSK.2025.35.12.574

Korean Journal of Materials Research ISSN:1225-0562(Print) 2287-7258(Online) 한국재료학회지

All Issue