Cu3Mo2O9/MoO3纳米复合材料制备及三甲胺气敏性能研究

毕文杰; 杨爽; 周静; 金伟; 陈文

doi:10.7498/aps.72.20230720

摘要

水产品的新鲜度极大地影响着人类的生命及身体健康, 水产品在存放过程中会释放出以三甲胺为代表的胺类气体, 通过检测这类气体的浓度可以监控水产品的新鲜度. 本文以具有优良气体敏感性能的MoO₃纳米带作为基体, 通过引入Cu₃Mo₂O₉纳米颗粒制备Cu₃Mo₂O₉/MoO₃复合材料, 具有非常好的三甲胺气体敏感性能、快速响应/恢复时间及长期稳定性. 结果表明, 采用这种复合材料制备的气敏元件在50—240 ℃, 质量分数为5×10^–6时对三甲胺气体的响应可达到R_air/R_gas = 13.9, 最小检测极限的体积分数为2×10^–7. 分布在MoO₃纳米带表面的Cu₃Mo₂O₉颗粒与基体形成异质结界面, 利用Cu₃Mo₂O₉的强氧吸附能力与催化效应促进电子与空穴的分离, 显著改善了复合材料的电子输运性能和气敏特性, 为制备高性能MoO₃基气敏材料提供了新的策略.

关键词:

Abstract

Aquatic products contain an incredibly high nutritional value for the human body and gradually become indispensable ingredients on the Chinese table. Trimethylamine (TMA) from the deterioration of aquatic products can serve as an indicator to measure fish freshness. It is a challenge to develop an instant, fast, convenient, and efficient gas sensor for fish freshness. In this study, a novel Cu₃Mo₂O₉/MoO₃ composite gas sensing material is prepared by introducing Cu₃Mo₂O₉ nanoparticles on the surface of MoO₃ nanobelts. The results of SEM and TEM images show that the Cu₃Mo₂O₉ nanoparticles are uniformly dispersed. Then, the TMA sensing performance of a resistance-type gas sensor based the prepared Cu₃Mo₂O₉/MoO₃ composite is tested at optimal operating temperature (240 °C). the results show that the sensor possesses good response (13.9) at low concentration (5×10^–6), with excellent low detection limit (2×10^–7). The response time is also significantly shortened. The high sensing performance of Cu₃Mo₂O₉/MoO₃ composite is attributed to the heterojunction interface, which promotes the separation of electrons from holes through its strong oxygen adsorption and catalytic effect. This significantly improves the electron transport properties and gas sensing characteristics of the composite material. Electrons flow from MoO₃ nanoribbons to Cu₃Mo₂O₉, and the Fermi level reaches equilibrium. This process results in the formation of an electron loss layer underneath MoO₃, and the charge transfer channel narrows, which is consistent with previous result. When trimethylamine dissociates on the nanoribbons to release electrons, the balance of the fermi lever is disrupted, and electrons flow from MoO₃ to Cu₃Mo₂O₉. As a result, the charge transfer channel becomes thinner, resulting in resistance modulation and increased sensitivity. In addition, the enhancement of trimethylamine sensing performance of Cu₃Mo₂O₉/MoO₃ nanocomposite can be explained by the enhancement of gas adsorption and diffusion: MoO₃ nanoribbons as a skeleton can effectively disperse Cu₃Mo₂O₉ particles and increase the adsorption capacity of gas molecules. And the enhanced response of Cu₃Mo₂O₉/MoO₃ may be due to the good catalytic effect of Cu₃Mo₂O₉, which is conducive to oxygen adsorption. This work provides a new strategy for preparing high-performance MoO₃-based gas sensing materials.

Keywords:

作者及机构信息

武汉理工大学材料科学与工程学院, 材料复合新技术国家重点实验室, 武汉　430070

通信作者: 周静, zhoujing@whut.edu.cn

基金项目: 国家自然科学基金(批准号: 62171331)、武汉理工大学三亚科教创新园开放基金(批准号: 2020KF0026)和湖北省自然科学基金(批准号: 2020CFB188)资助的课题.

Authors and contacts

State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, School of Materials Science and Engineering, Wuhan University of Technology, Wuhan 430070, China

Corresponding author: Zhou Jing, zhoujing@whut.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 62171331), the Open Fund of the Sanya Science and Education Innovation Park of Wuhan University of Technology, China (Grant No. 2020KF0026), and the Hubei Provincial Natural Science Foundation of China (Grant No. 2020CFB188).

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参考文献

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施引文献

图 1 (a) MoO₃纳米带、Cu₃Mo₂O₉颗粒及Cu₃Mo₂O₉/MoO₃纳米复合材料的XRD图谱; (b) Cu₃Mo₂O₉/MoO₃纳米复合材料的TEM图像; (c)—(e) 元素映射图像: Cu₃Mo₂O₉/MoO₃纳米复合材料的Mo, O, Cu图像

Fig. 1. (a) XRD patterns of MoO₃ nanobelts, Cu₃Mo₂O₉ particle, and Cu₃Mo₂O₉/MoO₃ nanocomposites; (b) TEM image of Cu₃Mo₂O₉/MoO₃ nanocomposites; (c)–(e) Mo, O and Cu element mapping images of Cu₃Mo₂O₉/MoO₃ nanocomposites.

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图 2 (a), (b) 纯MoO₃纳米带和Cu₃Mo₂O₉/MoO₃纳米复合材料的SEM图像; (c) Cu₃Mo₂O₉/MoO₃纳米复合材料的TEM图像 (插图为MoO₃纳米带和Cu₃Mo₂O₉颗粒的HRTEM图)

Fig. 2. (a), (b) SEM image of pure MoO₃ nanobelts and Cu₃Mo₂O₉/MoO₃ nanocomposites; (c) TEM image of Cu₃Mo₂O₉/MoO₃ nanocomposites (Inset shows HRTEM patten of the MoO₃ nanobelts and Cu₃Mo₂O₉ particle).

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图 3 MoO₃与Cu₃Mo₂O₉/MoO₃复合材料的XPS图像　(a) 全谱; (b) Cu 2p; (c) Mo 3d; (d) O 1s

Fig. 3. XPS images of MoO₃ and Cu₃Mo₂O₉/MoO₃ composites: (a) Full spectrum; (b) Cu 2p; (c) Mo 3d; (d) O 1s.

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图 4 (a) 不同工作温度下MoO₃纳米带、Cu₃Mo₂O₉颗粒和Cu₃Mo₂O₉/MoO₃纳米复合材料对体积分数为5×10^–6 的TMA的响应; (b) 190 ℃下MoO₃纳米带、Cu₃Mo₂O₉颗粒和Cu₃Mo₂O₉/MoO₃纳米复合材料对不同浓度TMA的响应折线图

Fig. 4. (a) Response of MoO₃ nanobelts, Cu₃Mo₂O₉ particle, and Cu₃Mo₂O₉/MoO₃ nanocomposites to TMA with a volume fraction of 5×10^–6 at different working temperatures; (b) the corresponding line chart of MoO₃ nanobelts, Cu₃Mo₂O₉ particle, and Cu₃Mo₂O₉/MoO₃ nanocomposites to different concentrations of TMA at 190 ℃.

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图 5 (a) MoO₃纳米带、Cu₃Mo₂O₉颗粒和Cu₃Mo₂O₉/MoO₃纳米复合材料在190 ℃下对不同浓度TMA的实时响应/恢复曲线; (b) Cu₃Mo₂O₉/MoO₃纳米复合材料对体积分数为5×10^–6的TMA的响应/恢复时间

Fig. 5. (a) Real-time response/recovery curves of MoO₃ nanobelts, Cu₃Mo₂O₉ particle, and Cu₃Mo₂O₉/MoO₃ nanocomposites to different concentrations of TMA at 190 ℃; (b) response/recovery time of Cu₃Mo₂O₉/MoO₃ nanocomposites to TMA with a volume fraction of 5×10^–6.

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图 6 Cu₃Mo₂O₉/MoO₃纳米复合材料在190 ℃下对体积分数为5×10^–6 的TMA的动态响应(a)及长期稳定性(b)

Fig. 6. Dynamic response (a) and long-term stability (b) of Cu₃Mo₂O₉/MoO₃ nanocomposites to trimethylamine with a volume fraction of 5×10^–6 at 190 ℃.

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图 7 Cu₃Mo₂O₉/MoO₃纳米复合材料对不同气体的响应比较

Fig. 7. Response comparison of Cu₃Mo₂O₉/MoO₃ nanocomposites to various.

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图 8 Cu₃Mo₂O₉/MoO₃-3在190 ℃, 20%—60%相对湿度范围内对TMA的响应情况

Fig. 8. Response of Cu₃Mo₂O₉/MoO₃-3 composite sensor to trimethylamine at 190 ℃ and 20%–60% relative humidity.

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图 9 (a) Cu₃Mo₂O₉/MoO₃复合材料的紫外可见吸收光谱; (b) 用于MoO₃纳米带、Cu₃Mo₂O₉颗粒和Cu₃Mo₂O₉/MoO₃纳米复合材料带隙测量的Tauc图

Fig. 9. (a) UV-vis absorption spectra of Cu₃Mo₂O₉/MoO₃ nanocomposites; (b) Tauc plot for band gap measurement of MoO₃ nanobelts, Cu₃Mo₂O₉ particle, and Cu₃Mo₂O₉/MoO₃ nanocomposites.

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图 10 (a), (d), (g) Au, Cu₃Mo₂O₉和MoO₃的UPS光谱; (b), (e), (h) 计算的E_cut-off值; (c), (f), (i) 计算的E_Fermi值

Fig. 10. (a), (d), (g) UPS spectra of Au, Cu₃Mo₂O₉ and MoO₃; (b), (e), (h) calculated E_cut-off values, (c), (f), (i) calculated E_Fermi values.

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图 11 Cu₃Mo₂O₉/MoO₃纳米复合材料体系的能带图　(a) 平衡前 (b) 平衡后 (E_vac, 真空水平; E_f, 费米能级; E_c, 导带底部; E_v, 价电子带顶部; E_g, 带隙). (c) Cu₃Mo₂O₉/MoO₃纳米复合材料暴露于TMA的示意图

Fig. 11. Energy band diagrams of Cu₃Mo₂O₉/MoO₃ nanocomposites system: (a) Before and (b) after equilibrium (E_vac, the vacuum level; E_f, Fermi level; E_c, the bottom of conduction band; E_v, the top of valence band; E_g, band gap). (c) Schematic diagram of Cu₃Mo₂O₉/MoO₃ nanocomposites exposed to TMA.

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表 1 不同材料对TMA的气敏性能对比

Table 1. Comparison of gas-sensing performance of gas towards TMA.

材料	温度/℃	检测限/(10^–6)	S_{5 ppm}/(R_air·R_gas^–1)	响应/恢复时间/s	Ref.
W-MoO₃	280	5	约4	6/11	[35]
Ce-MoO	240	5	约5	10/20	[36]
MoO₃ nanobelts	100	1	1	—	[37]
MoO₃/NiO	350	1	3.59	—	[7]
CoMoO₄/MoO₃	220	5	约9.0	9/10	[8]
MoO₃/Bi₂Mo₃O₁₂	70	—	约3.3	7.1/—	[38]
Cu₃Mo₂O₉/MoO₃	190	0.2	13.9	7/25	本文

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[13]	Kathirvelan J, Vijayaraghavan R, Thomas A 2017 Sens. Rev. 37 147 Google Scholar
[14]	Gou Y, Yang L, Liu Z, Asiri A M, Hu J, Sun X P 2018 Inorg. Nano-Met. Chem. 57 147 Google Scholar
[15]	Wang W X, Jin W, Yang S, Jian Z L, Chen W 2021 Sens. Actuators B 15 129583 Google Scholar
[16]	Dutta D P, Rathore A, Ballal A, Tyagi A K 2015 RSC Adv. 10 10389 Google Scholar
[17]	Pan H, Jin L, Su H, Zhang B B, Zhang L, Zhang H T, Yang W Q 2017 J. Alloys Compd. 695 2965 Google Scholar
[18]	Shen S K, Zhang X F, Cheng X L, Xu Y M, Gao S, Zhao H, Zhou X, Huo L H 2019 ACS Appl. Nano Mater. 2 8016 Google Scholar
[19]	薄小庆, 刘唱白, 李海英, 刘丽, 郭欣, 刘震, 刘丽丽, 苏畅 2014 物理学报 63 176803 Google Scholar Bo X Q, Liu C B, Li H Y, Liu L, Guo X, Liu Z, Liu L L, Su C 2014 Acta Phys. Sin. 63 176803 Google Scholar
[20]	韩丹, 刘志华, 刘琭琭, 韩晓美, 刘东明, 禚凯, 桑胜波 2022 物理学报 71 010701 Google Scholar Han D, Liu Z H, Liu L L, Han X M, Liu D M, Gao K, Sang S B 2022 Acta Phys. Sin. 71 010701 Google Scholar
[21]	Wang J X, Zhou Q, Peng S D, Xu L N, Zeng W 2020 Front. Nanochem. 8 339 Google Scholar
[22]	Sui L L, Xu Y M, Zhang X F, Cheng X L, Gao S, Zhao H, Cai Z, Huo L H 2015 Sens. Actuators, B 208 73 Google Scholar
[23]	秦玉香, 王飞, 沈万江, 胡明 2012 物理学报 61 057301 Google Scholar Qin Y X, Wang F, Shen W J, Hu M 2012 Acta Phys. Sin. 61 057301 Google Scholar
[24]	刘志福, 李培, 程铁栋, 黄文 2020 物理学报 69 248101 Google Scholar Liu Z F, Li P, Cheng T D, Huang W 2020 Acta Phys. Sin. 69 248101 Google Scholar
[25]	李东珂, 贺冰彦, 陈坤权, 皮明雨, 崔玉亭, 张丁可 2019 物理学报 69 198101 Google Scholar Li D K, He B Y, Chen K Q, Pi M Y, Cui Y T, Zhang D K 2019 Acta Phys. Sin. 69 198101 Google Scholar
[26]	艾雯, 胡小会, 潘林, 陈长春, 王一峰, 沈晓冬 2019 物理学报 68 197101 Google Scholar Ai W, Hu X H, Pan L, Chen C C, Wang Y F, Shen X D 2019 Acta Phys. Sin. 68 197101 Google Scholar
[27]	Sakaushi K, Thomas J, Kaskel S, Eckert J 2013 Chem. Mater. 25 2557 Google Scholar
[28]	Rothschild A, Komem Y 2004 Appl. Surf. Sci 95 6374 Google Scholar
[29]	Yao M S, Tang W X, Wang G E, Nath B, Xu G 2016 Adv. Mater. 28 5229 Google Scholar
[30]	Lupan O, Postica V, Hoppe M, Wolff N, Polonskyi O, Pauporté T, Viana B, Majérus O, Kienle L, Faupel F, Adelung R 2018 Nanoscale 10 14107 Google Scholar
[31]	Majhi S M, Lee H J, Choi H N, Cho H Y, Kim J S, Lee C R, Yu Y T 2019 Cryst. Eng. Comm 21 5084 Google Scholar
[32]	Gao X, Li Y Q, Zeng W, Zhang C F, Wei Y M 2017 J. Mater. Sci. Mater. Electron. 28 18781 Google Scholar
[33]	Ji H C, Zeng W, Li Y Q 2019 Physica E 114 113646 Google Scholar
[34]	Lü J X, Chen X L, Chen S S, Li H, Deng H 2019 J. Electroanal. Chem. 842 161 Google Scholar
[35]	Li Z Q, Wang W J, Zhao Z C, Liu X R, Song P 2017 Mater. Sci. Semicond. Process. 66 33 Google Scholar
[36]	Li Z Q, Wang W J, Zhao Z F, Liu X R, Song P 2017 RSC Adv. 7 28366 Google Scholar
[37]	Yang S, Liu Y L, Chen W, Jin W, Zhou J, Zhang H, Galina S Z 2016 Sens. Actuators, B 226 478 Google Scholar
[38]	Zhang F D, Dong X, Cheng X L, Xu Y M, Zhang X F, Huo L H 2019 ACS Appl. Mater. Interfaces 11 11755 Google Scholar

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Cu₃Mo₂O₉/MoO₃纳米复合材料制备及三甲胺气敏性能研究

Research on synthesis of Cu₃Mo₂O₉/MoO₃ nanocomposite and trimethylamine gas sensing properties

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武汉理工大学材料科学与工程学院, 材料复合新技术国家重点实验室, 武汉　430070

通信作者: 周静, zhoujing@whut.edu.cn

Authors and contacts

State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, School of Materials Science and Engineering, Wuhan University of Technology, Wuhan 430070, China

Corresponding author: Zhou Jing, zhoujing@whut.edu.cn

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