Preparation of High-Purity Ultrafine Mg-Al Spinel Powder by Double Metal Alkoxide Method

doi:10.16552/j.cnki.issn1001-1625.2025.1188

Abstract

Abstract:

High-purity Mg-Al spinel （MgAl₂O₄） powder with an average grain size D₅₀ of 0.42 μm， low hard agglomeration， and purity higher than 99.99% （mass fraction） was successfully prepared by double metal alkoxide method combined with planetary ball milling technology. By optimizing the alkoxide hydrolysis conditions and ball milling mechanical parameters， the spinel phase powder was synthesized at low temperature and dispersed at the nanoscale， significantly reducing energy consumption. The obtained powder was sintered at 1 550 ℃ under vacuum for 4.0 h at 60 MPa combined with hot isostatic pressing （1 750 ℃， 200 MPa for 2.0 h） post-treatment. High optical quality MgAl₂O₄ transparent ceramics with linear transmittance of up to 83.5%@600 nm （close to the theoretical value of 86%） were successfully prepared. This study confirms that the double metal alkoxide method has significant advantages in preparing ultrafine powder that meet the stringent requirements of transparent ceramics， providing an important powder foundation for the development of high-performance spinel optical materials.

Key words: magnesium-aluminum spinel, transparent ceramics, high-purity powder, double metal alkoxide method, planetary ball milling, transmittance

CLC Number:

TQ174

WANG Ying, LEI Muyun, LING Hao, WANG Haili, LI Zhen, HUANG Cunxin. Preparation of High-Purity Ultrafine Mg-Al Spinel Powder by Double Metal Alkoxide Method[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2026, 45(6): 2122-2128.

Figures/Tables 7

Fig.1 FTIR spectra of Mg-Al spinel powder precursor with different water to alkoxide ratios

Fig.2 TG-DSC curves of Mg-Al spinel powder precursor

Fig.3 SEM images and XRD patterns of Mg-Al spinel powder precursor with different water to alkoxide ratios

Fig.4 SEM images of Mg-Al spinel powder at different temperatures and SCR2-25 Mg-Al spinel powder

Fig.5 D50 and SSA of Mg-Al spinel powder with different ball milling time

Fig.6 D50 of Mg-Al spinel powder with 4.0 h ball milling time （No.2）

Fig.7 Section SEM images and transmittance spectrum of Mg-Al spinel transparent ceramics

References 15

[1]	KREISBERG V A， IVAKIN Y D， DANCHEVSKAYA M N. Content and diffusion of water and gases in MgAl₂O₄ spinel crystals synthesized to produce ceramics［J］. Journal of the European Ceramic Society， 2019， 39（2/3）： 508-513. DOI URL
[2]	GANESH I. A review on magnesium aluminate （MgAl₂O₄） spinel： synthesis， processing and applications［J］. International Materials Reviews， 2013， 58（2）： 63-112. DOI URL
[3]	KIRSCH J C， LINDBERG W R， HARRIS D C， et al. Tri-mode seeker dome considerations［C］// Window and Dome Technologies and Materials IX. Orlando， Florida， USA. SPIE， 2005： 33-40.
[4]	REIMANIS I， KLEEBE H J. A review on the sintering and microstructure development of transparent spinel （MgAl₂O₄）［J］. Journal of the American Ceramic Society， 2009， 92（7）： 1472-1480. DOI URL
[5]	雷牧云，李祯，王颖，等. 镁铝尖晶石透明陶瓷吸收系数研究［J］. 人工晶体学报， 2024， 53（11）： 2013-2021.
	LEI M Y， LI Z， WANG Y， et al. Absorption coefficient of magnesium aluminate spinel transparent ceramics［J］. Journal of Synthetic Crystals， 2024， 53（11）： 2013-2021 （in Chinese）.
[6]	韩丹，章健，罗皓鸣，等. 反应烧结制备镁铝尖晶石透明陶瓷研究新进展［J］. 化工进展， 2024， 43（7）： 3637-3646. DOI
	HAN D， ZHANG J， LUO H M， et al. A review on preparation of spinel transparent ceramic by reactive sintering［J］. Chemical Industry and Engineering Progress， 2024， 43（7）： 3637-3646 （in Chinese）. DOI
[7]	SU J Y， ZHANG X Y， LI X， et al. Synthesis and luminescence properties of Yb³⁺， Tm³⁺ and Ho³⁺ co-doped SrGd₂（WO₄）₂（MoO₄）₂ nano-crystal ［J］. Advanced Powder Technology， 2020， 31（2）： 1051-1059. DOI URL
[8]	王建斌，王战民，冯海霞，等. 原料特性对镁铝尖晶石烧结致密化影响的研究进展［J］. 耐火材料， 2023， 57（3）： 259-264. DOI
	WANG J B， WANG Z M， FENG H X， et al. Research progress on the influence of raw material characteristics on the sintering densification of magnesium aluminate spinel［J］. Refractories， 2023， 57（3）： 259-264 （in Chinese）.
[9]	谭婷. 微波辅助溶液燃烧合成纳米MgAl₂O₄粉体的研究［D］. 武汉：华中科技大学， 2009.
	TAN T. Study on microwave-assisted solution combustion synthesis of nano MgAl₂O₄ powder［D］. Wuhan： Huazhong University of Science and Technology， 2009 （in Chinese）.
[10]	王朔，余俊，赵惠忠，等. 微波辅助溶液燃烧法制备MgAl₂O₄粉体［J］. 耐火材料， 2014， 48（6）： 421-423.
	WANG S， YU J， ZHAO H Z. Synthesis of MgAl₂O₄ powders by microwave-assisted combustion［J］. Refractories， 2014， 48（6）： 421-423 （in Chinese）.
[11]	肖剑翔，黄慧超，敖敏，等. 铝源种类对制备镁铝尖晶石的影响［J］. 中国陶瓷， 2023， 59（12）： 43-50.
	XIAO J X， HUANG H C， AO M， et al. Influence of aluminum source the preparation of magnesium aluminum spinel［J］. Journal of Chinese Ceramics， 2023， 59（12）： 43-50 （in Chinese）.
[12]	MÜLLER M M， STRICKER K， KLEEBE H J. Gas-phase triggered phase evolution in pressure-less sintered LiF doped Mg-Al spinel［J］. Journal of the European Ceramic Society， 2021， 41（10）： 5400-5404. DOI URL
[13]	雷牧云，李祯，张微，等. 镁铝尖晶石透明陶瓷的研究进展［J］. 人工晶体学报， 2023， 52（12）： 2108-2124.
	LEI M Y， LI Z， ZHANG W， et al. Research progress on magnesium aluminate spinel transparent ceramic［J］. Journal of Synthetic Crystals， 2023， 52（12）： 2108-2124 （in Chinese）.
[14]	王康，田洪翼，杨威，等. 镁铝尖晶石透明陶瓷的研究进展［J］. 现代技术陶瓷， 2023， 44（2）： 77-116.
	WANG K， TIAN H Y， YANG W， et al. Research progress on magnesia-alumina spinel ceramics［J］. Modern Technology Ceramics， 2023， 44（2）： 77-116 （in Chinese）.
[15]	孙魁. 高透过性镁铝尖晶石透明陶瓷的制备和组织性能研究［D］. 武汉：武汉理工大学， 2021.
	SUN K. Preparation and microstructure properties of high transmittance magnesia-alumina spinel transparent ceramics［D］. Wuhan： Wuhan University of Technology， 2021 （in Chinese）.