Ambient flash sintering of reduced graphene oxide/zirconia composites: Role of reduced graphene oxide

doi:10.1016/j.jmst.2020.04.051

摘要/Abstract

Abstract:

Fabrication of graphene/ceramic composites commonly requires a high-temperature sintering step with long times as well as a vacuum or inert atmosphere, which not only results in property degradation but also significant equipment complexity and manufacturing costs. In this work, the ambient flash sintering behavior of reduced graphene oxide/3 mol% yttria-stabilized ZrO₂ (rGO/3YSZ) composites utilizing rGO as both a composite component and a conductive additive is reported. When the sintering condition is carefully optimized, a dense and conductive composite can be achieved at room temperature and in the air within 20 s. The role of the rGO in the FS of the rGO/3YSZ composites is elucidated, especially with the assistance of a separate investigation on the thermal runaway behavior of the rGO. The work suggests a promising fabrication route for rGO/ceramic composites where the vacuum and furnace are not needed, which is of interest in terms of simplifying the fabrication equipment for energy and cost savings.

Key words: Flash sintering, Reduced graphene oxide, Zirconia, Ceramic matrix composites

. [J]. 材料科学与技术, 2021, 60(0): 70-76.

Weiwei Xiao, Na Ni, Xiaohui Fan, Xiaofeng Zhao, Yingzheng Liu, Ping Xiao. Ambient flash sintering of reduced graphene oxide/zirconia composites: Role of reduced graphene oxide[J]. J. Mater. Sci. Technol., 2021, 60(0): 70-76.

图/表 8

Fig. 1. SEM images of (a) 24h-rGO aerogel and (b) green body of the 5.5 vol.% rGO/3YSZ composites. (c) TG and DSC curves of rGO aerogel. (d) and (e) Change of field strength, current density, power density, linear shrinkage and surface temperature vs. time for a typical sintering experiment used to prepare the 5.5 vol.% rGO/3YSZ composites at room temperature in air under an initial field strength of 60 V/cm and a current limit of 160 mA/mm2. Photographs of (f) the samples in the different stages of the FS experiment and (e) the cross-section of the samples.

Fig. 2. (a) Raman spectra from the black and white parts in the 5.5 vol.% rGO/3YSZ sample sintered under 60 V/cm and 160 mA/mm2 for 20 s. The characteristic graphene ID peak is marked in green. Raman mapping using the graphene ID signal for (b1) a black area and (b2) a black/white interface area in the specimen. (c) BSE image of the polished surface and (d) SE image of the surface after hydrofluoric acid in the composite area.

Fig. 3. (a1)-(b3) SEM images, (c) the porosity and relative density and (d) the grain size distribution of black and white parts of the 5.5 vol.% rGO/3YSZ sample sintered for different holding times.

Fig. 4. Mechanical properties measured by nanoindentation for the 5.5 vol.% rGO/3YSZ sample sintered with the holding time of 20 s. In situ scanning probe imaging of indents formed after the application of 10 mN load in the region of (a) white 3YSZ and (b) black rGO/YSZ composites. (c) Modulus and hardness measured in the black and white regions.

Table 1 Green body electrical conductivity of the rGO/YSZ composite.

rGO (vol.%)	0	0.6	5.5	10.0
Conductivity (S/m)	1 × 10^-7	3 × 10^-6	0.2	13

Fig. 5. (a) FS of 0.6 vol.% rGO/YSZ composite at the elevated furnace temperature. (b) FS behavior of the 10.0 vol.% rGO/3YSZ composites at RT. (c) Plot of ln R vs. 10,000/T for the 5.5 vol.% rGO/3YSZ composite sample.

Fig. 6. (a) Electrical response and (b) surface temperature of rGO aerogel under different field strengths. (c) Comparison of the FS behavior of rGO aerogel and 5.5 vol.% rGO/3YSZ composite under the same field strength of 40 V/cm.

Fig. 7. Schematics of the FS process of the rGO/3YSZ composite.

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