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ZrO2/SiO2
JOURNAL OF THE AMERICAN CERAMIC SOCIETY · 2025 ·Vol. 109 ·期 1 ·e70386 · IF 3.8

Architecting dual heterogeneous structures to achieve robust mechanical properties in ZrO2-SiO2 nanocrystalline ceramics

Le Fu,Wenjun Yu,Bohan Wang,Zihua Lei,Mingxi Deng,Guanghua Liu,Gemei Cai

Heterostructured materials hold great potential for achieving superior mechanical properties. However, the majority of current studies on heterostructured ceramics have predominantly focused on layered systems. Here, we report a new 3YSZ-(ZrO 2 -SiO 2 ) dual-heterostructured ceramic composites (DHCCs) comprising 3 mol% yttria-stabilized zirconia (3YSZ) domains and ZrO 2 -SiO 2 domains. The DHCCs exhibited a dual-level hierarchical structure. Specifically, the 3YSZ domain consisted of submicron ZrO 2 grains, while the ZrO 2 -SiO 2 domain was composed of ZrO 2 nanograins dispersed within an amorphous SiO 2 matrix. To fabricate the DHCCs, hybrid powders were first synthesized by a chemical co-precipitation method, followed by sintering to produce dense DHCCs. The phase composition, microstructure, and mechanical properties of the DHCCs were characterized. Compared with the homogeneously structured ZrO 2 -SiO 2 ceramic, the DHCCs exhibited an 85.6% increase in strength and a 47.2% improvement in fracture toughness. Finally, the underlying strengthening and toughening mechanisms of the DHCCs were elucidated. These findings demonstrate that architecting dual-heterogeneous structures represents an effective strategy for achieving robust mechanical properties.

CAS / MDL: 13520-92-8 78-10-4
研究领域: 材料科学 · 陶瓷 · 机械工程 · 纳米材料 · 结构材料
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MATERIALS CHARACTERIZATION · 2025 · IF 5.5

Constructing structure-function integrated ZrO2-SiO2 ceramic nanocomposites through incorporation of CNTs and Ti3AlC2

Wenjun Yu,Zihua Lei,Wenqian Pan,Yang Li,Songlin Ran,Le Fu

In this study, we sought to develop structure-function integrated ZrO 2 -SiO 2 ceramic nanocomposites by simultaneously incorporating one-dimensional (1D) carbon nanotubes (CNTs) and three-dimensional (3D) Ti 3 AlC 2 MAX phase. The CNTs and Ti 3 AlC 2 were introduced into the ZrO 2 -SiO 2 precursor powder via a straightforward wet ball milling process. CNTs maintained excellent structural stability during sintering, whereas the Ti 3 AlC 2 decomposed into Al and TiC. The flexural strength of the nanocomposite was enhanced by 34 % attributed to the pull-out strengthening effect of the CNTs. The uniformly distributed 1D CNTs and the in-situ formed 3D TiC particles created an interconnected network within the ceramic matrix, thereby providing efficient pathways for electron transport. Consequently, the electrical conductivity and electromagnetic wave absorption properties of the nanocomposites were markedly improved. This study demonstrates an effective approach to developing structure-function integrated ceramic composites by exploiting the dimensional differences and synergistic interactions between the filler phases.

CAS / MDL: 13520-92-8 196506-01-1
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JOURNAL OF THE AMERICAN CERAMIC SOCIETY · 2024 · IF 3.5

Layered ZrO2/SiO2 aerogel composite fibrous flexibility membrane for thermal insulation and sound absorption

Mengmeng Yang,Yang Ding,Zhaofeng Chen,Qiong Wu,Lihao Liu,Tianlong Liu,Manna Li,Kai Xu,Lu Le,Lixia Yang

As promising candidates for widespread application, advanced ceramic fiber mats with robust mechanical properties are urgently needed. However, the brittleness, fatigue failure, and large density of ceramic fiber pose significant obstacles to its practical application. Herein, a novel SiO 2 aerogel/ZrO 2 composite nanofibrous membrane (SZCNFM) with excellent flexibility was prepared by introducing SiO 2 aerogel nanoparticles into ZrO 2 nanofiber via simple co-electrospinning. The developed tetragonal zirconia phase without changing up to 1200°C endows SZCNFM material with excellent thermal stability. Furthermore, the as-prepared membranes exhibit fatigue resistance ability which can maintain 98% of the original stress after 100 buckling cycle tests. The addition of mesoporous structure aerogel reduces the heat transfer of the nanofibrous membrane, giving its low thermal conductivity (30 mW/m/K) and low-frequency sound absorption (noise reduction coefficient of 0.52). Combined with the high-temperature resistance, low thermal conductivity and excellent sound-absorption ability make it a promising material for heat insulation and acoustic absorption.

研究领域: 材料科学 · 热学工程 · 声学工程
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JOURNAL OF THE EUROPEAN CERAMIC SOCIETY · 2021 · IF 5.302

Doping of tantalum, niobium, and hafnium in a translucent ZrO2-SiO2 nanocrystalline glass-ceramic

Le Fu,Fuqing Jiang,Bo Li,Yongxin Cheng,Guofu Xu,Jiwu Huang,Håkan Engqvist,Wei Xia

The addition of dopant(s) is an effective strategy to regulate the microstructure and properties of ZrO 2 -based ceramics. In this study, we investigated the effects of ternary element alloying, namely tantalum (Ta), niobium (Nb), and hafnium (Hf) elements, on the microstructure and transformability of ZrO 2 nanocrystallites in a ZrO 2 -SiO 2 nanocrystalline glass-ceramic (NCGC) during sintering and thermal treatments. The ternary dopants enhanced the transformability of tetragonal ZrO 2 (t-ZrO 2 ) nanocrystallites during sintering, i.e., the dopants acted as t-ZrO 2 destabilizer. The Ta, Nb and Hf elements dissolved in ZrO 2 nanocrystallites, forming ZrO 2 solid solution. Meanwhile, lamella nanotwins were formed within many ZrO 2 nanocrystallites. No obvious segregation of dopants was detected at ZrO 2 grain boundaries. t-ZrO 2 and monoclinic (m) ZrO 2 nanocrystallites were metastable in thermal treatments process, with “t” to “m” and the reverse “m” to “t” polymorphic transformation occurred simultaneously. Meanwhile, t-ZrO 2 and m-ZrO 2 nanocrystallites had a great tendency to grow larger during thermal treatments.

研究领域: 材料科学 · 陶瓷工程
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CERAMICS INTERNATIONAL · 2024 ·Vol. 50 ·期 7 ·12539-12548 · IF 5.1

ZrO2/SiO2/C nanofiber aerogels with enhanced mechanical and thermal insulation properties fabricated by freeze casting

Wei Dang,Ziang Li,Bowen Wang,Zhuoli Xu,Xinyuan Zhang,Fuping Li,Kang Zhao,Jun Ma,Yufei Tang

Because of the inherent high-temperature resistance, the application of ZrO 2 nanofiber aerogels in thermal insulation is promising. However, the contradiction between mechanical and thermal insulation properties has limited its applications. In the present work, nanofiber aerogels of ZrO 2 /SiO 2 /C with enhanced thermal insulation and compressive strength were successfully prepared by freeze-casting using tetraethoxysilane (TEOS) as a binder. The effect of TEOS content on the microstructure, compressive and thermal insulation properties was investigated. The porosity of the fabricated aerogels is higher than 97.3 %. The pore structure exhibits hierarchical characteristics, with honeycomb pores on the micro-scale and mesopores on the nano-scale. Part of the SiO 2 phases generated by TEOS hydrolysis bond ZrO 2 nanofiber to form fiber junctions, while the others cover the surface of ZrO 2 nanofibers forming core-shell structure. With the increase of TEOS content, ZrO 2 /SiO 2 /C nanofiber aerogels showed a slightly decrease in thermal conductivity to a lower value of 0.032 W m −1  K −1 and an increase in compressive stress to 11.9 KPa. The thermal insulation mechanism and deformation mode during compression of aerogels were analyzed. This study not only provide ZrO 2 /SiO 2 /C nanofiber aerogels with both enhanced mechanical and thermal insulation properties, but also can guide the design and fabrication of other ceramic aerogels with excellent properties.

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CHEMICAL ENGINEERING JOURNAL · 2021 · IF 13.273

Elastic and highly fatigue resistant ZrO2-SiO2 nanofibrous aerogel with low energy dissipation for thermal insulation

Xinxin Zhang,Xiaota Cheng,Yang Si,Jianyong Yu,Bin Ding

As promising candidates for a wide range of applications, advanced ceramic aerogels with robust mechanical properties are urgently needed. However, the generic structural characteristics of ceramic aerogels, such as brittleness, fatigue failure, and large energy dissipation, present a great obstacle to their practical applications. Herein, we report a universal strategy to demonstrate a ceramic nanofibrous aerogel with superior elasticity and high fatigue resistance, realized by assembling flexible ZrO 2 -SiO 2 nanofibers into fluffy lamellar arch-shaped cellular structured. The as-obtained ZrO 2 -SiO 2 nanofibrous aerogels can rapidly recover from 90% strain, and exhibit high compression strength of 950 kPa (90% strain) and temperature-invariant superelasticity (from −196 to 1100 °C). In particular, the aerogels exhibit a low energy loss coefficient (0.28) and high fatigue resistance with zero plastic deformation after 1000 compression and release cycles, surpassing the performance of previously reported ceramic aerogels. Furthermore, the low thermal conductivity (0.0268 W m −1 K −1 ) and excellent high-temperature thermal insulation make it a desirable candidate for heat insulators under harsh conditions. The successful synthesis of these structural ceramic materials with high superelasticity, excellent compressibility, and superior fatigue resistance simultaneously opens up avenues for further the development of mechanically robust aerogel materials.

研究领域: 材料科学 · 热力学工程
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CERAMICS INTERNATIONAL · 2023 · IF 5.2

Densification and microstructure of a ZrO2–SiO2 glass-ceramic prepared by using mesoporous particles as raw powder

Le Fu,Wenjun Yu,Bohan Wang

Ceramic sintering is an energy-consuming process. Reducing sintering temperature and shortening dwelling time are significant to the reduction of carbon footprint. It has been reported that utilizing mesoporous particles as raw powder for sintering is a promising strategy to achieve the above goal. The goal of this study is to verify if this strategy also works for the sintering of ZrO 2 –SiO 2 glass-ceramics. We synthesized mesoporous particles through a micelle-assisted co-precipitation process, followed by sintering by fast hot pressing (FHP) and pressureless sintering (PS) to obtain ZrO 2 –SiO 2 glass-ceramics. For comparison, solid particles without mesopores were synthesized by a sol-gel method and consolidated by the two sintering techniques. The densification behaviors of the two types of particles were comparatively investigated. Results showed that the mesopores collapsed at ∼850 °C during FHP due to the applied pressure, which resulted in a peak densification rate during the whole sintering process. The mesoporous particles (∼820 °C) had a lower densification starting temperature than that of the solid particles (∼910 °C). However, the mesoporous particles showed a longer densification process and a lower average densification rate than those of the solid particles. The samples sintered from mesoporous particles showed a heterogeneous microstructure, predominately consisting of ZrO 2 nanocrystallites embedded in a SiO 2 matrix, but in some regions ZrO 2 sub-microcrystallites were connected with each other by grain boundaries, without the presence of SiO 2 matrix. During PS, there was not significant differences in the densification between the mesoporous particles and the solid ones. These results demonstrated that the mesoporous particles did not show significant advantages over solid ones, in terms of the densification of ZrO 2 –SiO 2 glass-ceramics.

研究领域: 材料科学 · 陶瓷工程
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JOURNAL OF THE AMERICAN CERAMIC SOCIETY · 2026 ·Vol. 109 ·期 9 ·e71194 · IF 4.2

Incorporation of Carbon Into ZrO2–SiO2 Powder Through Combustion Synthesis and Its Influences on the Sintered Ceramics

Le Fu,Bohan Wang,Zihua Lei,Mingxi Deng,Guanghua Liu

The in situ formation of carbon fillers has been demonstrated as an effective strategy to eliminate the agglomeration of carbon fillers in ceramic composites. In this study, combustion synthesis was employed to in situ incorporate carbon into a ZrO 2 –SiO 2 ceramic powder using CO 2 gas as the carbon source and magnesium powder as the exothermic medium. The resulting disordered carbon is uniformly distributed within the powder matrix. Furthermore, magnesium element is simultaneously incorporated into the powder as a byproduct. The co-presence of carbon and magnesium elements synergistically enhances the solid-state reaction between ZrO 2 and SiO 2 during sintering, facilitating the formation of ZrSiO 4 at a significantly reduced temperature of 1080°C. Meanwhile, the solid-state reaction significantly promotes the densification of the ceramic composite. The incorporated carbon exhibits strong bonding with the ceramic matrix and remains stable within the matrix up to at least 1000°C. Compared with conventional ZrSiO 4 , the ZrSiO 4 phase formed in this study exhibits much lower decomposition temperature in range of 1000°C–1200°C. Molten copper exhibits pronounced corrosion toward the ceramic composite, primarily through reactions with the SiO 2 phase released from the decomposition of ZrSiO 4 .

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CERAMICS INTERNATIONAL · 2022 · IF 5.532

New insights into the formation mechanism of zircon in a ZrO2–SiO2 nanocrystalline glass-ceramic: A TEM study

Le Fu,Bohan Wang,Wei Xia

We have previously observed that doping of Ca ions was beneficial to the formation of zircon (ZrSiO 4 ). It is well known that synthetic ZrSiO 4 is typically formed via a solid-state reaction between ZrO 2 and SiO 2 , in which the interfaces between the reactant and resultant play an important role. However, the interfaces are lacking detailed microstructural observation. This follow-up study aims at exploring the formation mechanism of ZrSiO 4 by inspecting the interfaces at the nano and atomic scales with TEM techniques. Results demonstrated that ZrSiO 4 was formed in the Ca-doped sample after sintering at 1200 °C, whereas, no ZrSiO 4 was formed in the undoped sample even after sintering at 1230 °C. The Ca-doped sample consisted of a continuous ZrSiO 4 matrix with dispersed ZrO 2 nanocrystallites . Doping of Ca ions promoted the formation of ZrSiO 4 by causing lattice distortion and oxygen vacancies in ZrO 2 lattices. Thin amorphous grain boundary complexions were found between ZrO 2 nanocrystallites and between ZrO 2 and ZrSiO 4 crystallites . These amorphous complexions acted as reaction sites and an intermediate metastable state for the solid-state reaction. A detailed formation mechanism of ZrSiO 4 at the nanometer scale and atomic scale has been proposed.

CAS / MDL: 23519-77-9 78-10-4
研究领域: 材料科学 · 纳米技术
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JOURNAL OF CATALYSIS · 2019 · IF 7.723

Promoted chemoselective crotonaldehyde hydrogenation on zirconia-doped SiO2 supported Ag catalysts: Interfacial catalysis over ternary Ag–ZrO2–SiO2 interfaces

Haiqiang Lin,Hongyan Qu,Weikun Chen,Kang Xu,Jianwei Zheng,Xinping Duan,Hesheng Zhai,Youzhu Yuan

In gas-phase chemoselective hydrogenation of crotonaldehyde on Ag-based catalysts, zirconia doping on silica supports was found to improve catalytic performance in terms of unsaturated alcohol selectivity, hydrogenation activity, and stability. The surface modification of silica by zirconia doping favors the fine dispersion of Ag species due to the enhanced quantity and strength of surface acid sites, which enable construction of abundant catalytic sites effective for C O bond hydrogenation. High crotyl alcohol selectivity, exceeding 80%, and significant inhibition of monohydrogenation on the C C bond were observed on the optimal Ag/Zr–SiO 2 catalyst. Dynamic O 2 chemisorption measurement revealed that the pure Ag powders did not chemisorb O 2 irreversibly under 323 K, but SiO 2 or Zr–SiO 2 supported Ag catalysts did. The amounts of Ag active for O 2 chemisorption, which are at least one order of magnitude lower than that of surface Ag derived from TEM and XRD characterizations, match well with the perimeter interface Ag of hemispherical particles. A strong correlation between hydrogenation activity and O 2 uptake on those Ag/SiO 2 and Ag/Zr–SiO 2 catalysts with different Ag dispersions and deactivation degrees was observed, implying that the effective catalytic sites for crotonaldehyde chemoselective hydrogenation may originate from accessible interface sites with unique redox properties. Catalyst induction and deactivation were observed on both Ag/SiO 2 and Ag/Zr–SiO 2 catalysts in real catalytic operation. Changes in metal stable interface structure, rather than metal aggregation and coagulation, are assumed to be the main cause of irreversible catalyst deactivation, because the apparent Ag particle sizes changed slightly, but the oxygen chemisorption ability deteriorated considerably. Electropositive Ag sites interacting with neighboring oxygen from oxide supports at the ternary Ag–ZrO 2 –SiO 2 interface are proposed to account for highly selective C O bond hydrogenation to produce the desired unsaturated alcohol.

CAS / MDL: 20667-12-3 7440-22-4
研究领域: 化学工程 · 催化科学
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CERAMICS INTERNATIONAL · 2021 · IF 4.527

Effects of dopants with various valences on densification behavior and phase composition of a ZrO2–SiO2 nanocrystalline glass-ceramic

Bohan Wang,Guofu Xu,Jiwu Huang,Håkan Engqvist,Wei Xia,Le Fu

Effects of dopants with different valences on the densification behavior and phase composition of a ZrO 2 –SiO 2 nanocrystalline glass-ceramic (NCGC) during pressureless sintering were investigated in this study. The raw powder of Ca 2+ , La 3+ , Ce 4+ and Ta 5+ ions doped ZrO 2 –SiO 2 (referred to as Ca-ZS, La-ZS, Ce-ZS, Ta-ZS, respectively) and pure ZrO 2 –SiO 2 (PZS) sample were synthesized by sol-gel method, followed by pressureless sintering. Compared with the PZS sample, doping of Ca 2+ and La 3+ ions significantly promoted the densification of the NCGCs. The “densification promotion” effect was attributed to the formation of oxygen vacancies and the decrease of SiO 2 viscosity due to doping of aliovalent cations. The dopants with various valences showed significant effects on the phase compositions of the NCGCs during sintering. Doping of Ca 2+ ion accelerated the reaction kinetics between ZrO 2 nanocrystallites and amorphous SiO 2 to yield ZrSiO 4 . The La 3+ ion acted as destabilizer of t-ZrO 2 , which resulted in a rapid tetragonal (t) to monoclinic (m) ZrO 2 phase transformation during sintering, while in the Ta 5+ and Ce 4+ ions doped sample, the phase transformation occurred gradually. All the doping ions increased the lattice parameters and the volume of t-ZrO 2 unit cell, while the effects of the doping ions on the lattice parameters of m-ZrO 2 unit cell were more complex.

研究领域: 材料科学 · 无机化学
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