焙烧温度对氧化锌纳米棒光催化生产H2O2活性的影响

doi:10.1016/S1872-2067(21)63832-9

催化学报 ›› 2022, Vol. 43 ›› Issue (2): 226-233.DOI: 10.1016/S1872-2067(21)63832-9

焙烧温度对氧化锌纳米棒光催化生产H₂O₂活性的影响

江梓聪^a^,^b, 张勇^c, 张留洋^a(), 程蓓^a(), 王临曦^d

^a武汉理工大学材料复合新技术国家重点实验室, 湖北武汉 430070
^b先进能源科学与技术广东省实验室佛山分中心(佛山仙湖实验室), 广东佛山 528200
^c湖北理工学院化学与化工学院, 湖北黄石 435003
^d中国地质大学材料与化学学院太阳燃料实验室, 湖北武汉 430074

收稿日期:2021-03-30 接受日期:2021-04-28 出版日期:2022-02-18 发布日期:2021-05-20
通讯作者: 张留洋,程蓓
基金资助:
国家自然科学基金(51872220);国家自然科学基金(51932007);国家自然科学基金(51961135303);国家自然科学基金(U1905215);国家自然科学基金(21871217);国家自然科学基金(U1705251);仙湖实验室基金(XHD2020-001)(XHD2020-001);中央高校基本科研业务费专项资金资助(武汉理工大学)(WUT: 2020Ⅲ027)

Effect of calcination temperatures on photocatalytic H₂O₂-production activity of ZnO nanorods

Zicong Jiang^a^,^b, Yong Zhang^c, Liuyang Zhang^a(), Bei Cheng^a(), Linxi Wang^d

^aState Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, Hubei, China
^bFoshan Xianhu Laboratory of the Advanced Energy Science and Technology Guangdong Laboratory, Xianhu Hydrogen Valley, Foshan 528200, Guangdong, China
^cCollege of Chemistry and Chemical Engineering, Hubei Polytechnic University, Huangshi, 435003, Hubei, China
^dLaboratory of Solar Fuel, Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430074, Hubei, China

Received:2021-03-30 Accepted:2021-04-28 Online:2022-02-18 Published:2021-05-20
Contact: Liuyang Zhang, Bei Cheng
Supported by:
This work was supported by the National Natural Science Foundation of China(51872220);This work was supported by the National Natural Science Foundation of China(51932007);This work was supported by the National Natural Science Foundation of China(51961135303);This work was supported by the National Natural Science Foundation of China(U1905215);This work was supported by the National Natural Science Foundation of China(21871217);This work was supported by the National Natural Science Foundation of China(U1705251);the Innovative Research Funds of Foshan Xianhu Laboratory of the Advanced Energy Science and Technology Guangdong Laboratory(XHD2020-001);the Fundamental Research Funds for the Central Universities(WUT: 2020Ⅲ027)

摘要/Abstract

摘要：

过氧化氢作为一种对环境友好的、重要的化学原料, 被广泛用于化学工业、漂白剂和废水处理等领域. 近几十年来, 过氧化氢主要通过蒽醌工艺生产. 然而, 该方法需要多步蒽醌加氢和氧化反应, 导致较高的生产成本和能量消耗, 同时伴随着大量的二氧化碳排放. 另一种替代策略是在贵金属催化剂的辅助下, 由氢气和氧气的混合气体在高温下直接合成. 但是, 氢气和氧气的混合气体在高温下存在爆炸的危险, 从而限制了其大规模应用. 因此, 探索一种低能耗、温和条件下生产过氧化氢具有重要的意义.
太阳能驱动光催化生产过氧化氢是解决上述问题的理想途径. 通常认为, 过氧化氢是由直接双电子还原(E(O₂/H₂O₂) = 0.68 V vs. NHE)或间接单电子O₂还原(E(O₂/•O₂ ^-)= -0.33 V vs. NHE)产生的. 氧化锌半导体具有很的稳定性好、环保和成本低等优点, 因此经常被用于二氧化碳的光催化还原、污水处理和气体传感器等领域. 氧化锌的导带电势(E_CB = -0.5 V vs. NHE)比氧还原电势更负, 意味着它在热力学上满足光催化过氧化氢生产的要求. 然而, 目前关于氧化锌的光催化生产过氧化氢的研究尚未受到较多的关注.
本文采用简单的水热法制备了一维氧化锌纳米棒, 在不同温度下热处理后, 对其形貌和结构、光学性质和电化学性质进行了表征. 同时, 系统地研究了以乙醇为牺牲剂光催化生产过氧化氢的性能. 结果表明, 随着焙烧温度的升高, 氧化锌纳米棒内部的氧空位被空气中的氧气重新填充, 其催化生成过氧化氢的活性先升高后降低. 经300 ºC焙烧的氧化锌光催化产过氧化氢的活性最好, 为285 μmol L ^-1 h ^-1. 同时, 对过氧化氢的生成机理研究结果表明, 该过程中为间接单电子O₂还原过程. 氧气先与一个电子反应生成超氧自由基, 再与两个质子和一个电子反应生成过氧化氢分子. 综上, 本文为氧化锌纳米棒光催化产过氧化氢的机理研究提供了新认识, 并提出了一种有前途的过氧化氢生产策略.

关键词: 光催化反应, 过氧化氢生产, 氧化锌纳米棒, 煅烧温度, 氧还原

Abstract:

Photocatalytic hydrogen peroxide (H₂O₂) production from O₂ and H₂O is an ideal process for solar-to-chemical energy conversion. Herein, ZnO nanorods are prepared via a simple hydrothermal method for photocatalytic H₂O₂ production. The ZnO nanorods exhibit varied performance with different calcination temperatures. Benefiting from calcination, the separation efficiency of photo-induced carriers is significantly improved, leading to the superior photocatalytic activity for H₂O₂ production. The H₂O₂ produced by ZnO calcined at 300 °C is 285 μmol L ^-1, which is over 5 times larger than that produced by untreated ZnO. This work provides an insight into photocatalytic H₂O₂ production mechanism by ZnO nanorods, and presents a promising strategy to H₂O₂ production.

Key words: Photocatalysis, Hydrogen peroxide production, ZnO nanorod, Calcination temperature, Oxygen reduction

江梓聪, 张勇, 张留洋, 程蓓, 王临曦. 焙烧温度对氧化锌纳米棒光催化生产H₂O₂活性的影响[J]. 催化学报, 2022, 43(2): 226-233.

Zicong Jiang, Yong Zhang, Liuyang Zhang, Bei Cheng, Linxi Wang. Effect of calcination temperatures on photocatalytic H₂O₂-production activity of ZnO nanorods[J]. Chinese Journal of Catalysis, 2022, 43(2): 226-233.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63832-9

https://www.cjcatal.com/CN/Y2022/V43/I2/226

图/表 12

Fig. 1. FESEM (a), TEM (b), HRTEM (c) images and corresponding SAED pattern (d) of Zn300.

Fig. 2. XRD patterns of ZnO nanorods calcined by different temperatures.

Fig. 3. UV-vis diffuse reflection spectra (a) and EPR patterns (b) of ZnO nanorods calcined at different temperatures.

Table 1 Effects of calcination temperatures on physical properties of ZnO nanorods.

Sample	Calcination temperature (°C)	Relative crystallinity	A_BET (m² g^-1)
Zn90	untreated	1	3.0
Zn200	200	1.1	2.7
Zn300	300	1.1	2.3
Zn400	400	1.2	2.6
Zn500	500	1.3	3.4

Fig. 4. (a) N2 adsorption-desorption isotherms of samples under standard temperature and pressure; (b) Thermogravimetry curve of ZnO nanorods in air.

Fig. 5. (a) Photocatalytic H2O2 production over different samples; (b) Photocatalytic decomposition of H2O2 over different samples after 1 h of irradiation; (c) Kf and Kd for photocatalytic H2O2 production; (d) The cyclic stability test of ZnO nanorods calcined at 300 °C.

Table 2 Comparison with other photocatalysts for H2O2 production.

photocatalyst	Reaction solution	Light source	H₂O₂ production activity (μmol g^-1 h^-1)	Ref.
Ag@U-CN-NS	water	300 W XL	67.50	[64]
C,O doped CN	water	300 W XL	32.00	[65]
CN/rGO@BPQDs	water	300 W XL	60.56	[66]
AQ-a-CN	10 vol% PP	AM 1.5	361	[6]
DCN	20 vol% IPA	AM 1.5	96.8	[67]
ACN	10 vol% IPA	300 W XL	174	[63]
SN-GQD/TiO₂	PE (10 mg/L)	500 W XL	902	[68]
ZnO nanorods	10 vol% EA	300 W XL	570	This work

Fig. 6. Transient photocurrent response (a) and Nyquist plots (b) of EIS over different samples.

Table 3 The fitted parameters obtained from decay curves over different samples.

Sample	τ₁ (ns) (Rel. %)	τ₂ (ns) (Rel. %)	τ_A (ns)
Zn90	1.75 (21.79)	20.44 (78.21)	16.37
Zn200	2.02 (26.16)	20.18 (73.84)	15.43
Zn300	3.12 (19.51)	23.61 (80.49)	19.61
Zn400	0.35 (8.11)	17.62 (91.89)	16.21
Zn500	0.23 (28.43)	20.62 (71.57)	14.88

Fig. 7. Time-resolved photoluminescence spectra over Zn90 and Zn300.

Fig. 8. EPR spectra recorded for •O2- over the Zn90 and Zn300 under the dark and Xe lamp irradiation for 5 min.

Fig. 9. (a) Mott-Schottky plots of Zn300 at the frequency of 1000, 2000 and 3000 Hz; (b) The possible mechanism for photocatalytic H2O2 production in ZnO nanorods.

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焙烧温度对氧化锌纳米棒光催化生产H₂O₂活性的影响

Effect of calcination temperatures on photocatalytic H₂O₂-production activity of ZnO nanorods

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