ZrW 2 O 8 /ZrO 2 composites with tunable low/nearzero coefficients of thermal expansion (CTE) are promising candidates in several fields including aerospace, precision manufacturing and measurement, electronic circuit, etc., for counteracting the thermal expansion effect. However, bottleneck issues (such as the unstable decomposition of ZrW 2 O 8 phase, manufacturing size limitation, etc.) caused by conventional hightemperature sintering impede the development and application of ZrW 2 O 8 /ZrO 2 . To solve these scientific issues, a methodology integrating hydrothermal assembly with a cold sintering process (CSP) is exploited. The ZrW 2 O 8 /ZrO 2 composite powders with a mace-like structure, in which the spherical ZrO 2 nanoparticles peripherally embed on the rod-like ZrW 2 O 8 matrix particles, are hydrothermally assembled. Then, the relatively dense ZrW 2 O 8 /ZrO 2 composites with excellent low or even near-zero CTE are successfully achieved by CSP (as low as 190 °C) with a postannealing treatment (550 °C). The evolution of sintering densification, phase composition, and microstructure followed by the fundamental mechanism regarding the hydrothermal assembly of the macelike structure and densification of CSP are investigated in detail. This research not only effectively overcomes the bottleneck issues of ZrW 2 O 8 /ZrO 2 via integrating the hydrothermal assembly with the sintering technology at ultralow temperature but also develops a promising prospect for the fabrication of a broader range of metastable functional materials. KEYWORDS: ZrW 2 O 8 /ZrO 2 composites, ceramics, low/near-zero coefficients of thermal expansion, hydrothermal assembly, cold sintering process
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