尿素诱导温和相变策略调控α-MnO2微结构以增强新兴污染物催化臭氧氧化效能

doi:10.1016/S1872-2067(25)64889-3

催化学报 ›› 2026, Vol. 84: 175-188.DOI: 10.1016/S1872-2067(25)64889-3

尿素诱导温和相变策略调控α-MnO₂微结构以增强新兴污染物催化臭氧氧化效能

朱培新^a, 肖梦瑶^a, 陈茜茜^c(), 罗旌崧^d, 房中^d, 陈龙^d, 赵慧楠^a, 何春^a^,^b, 田双红^a^,^b()

^a 中山大学环境科学与工程学院, 广东广州 510275
^b 广东省环境污染治理与修复重点实验室, 广东广州 510275
^c 香港城市大学材料科学与工程学院, 香港九龙 610200
^d 中化学南方建设投资有限公司, 广东广州 516000

收稿日期:2025-09-01 接受日期:2025-09-15 出版日期:2026-05-18 发布日期:2026-04-16
通讯作者: *电子信箱: xixichen@cityu.edu.hk, chenxixi8117@163.com (陈茜茜),
tshuangh@mail.sysu.edu.cn (田双红).
基金资助:
国家重点研发计划(2024YFC3712500);国家自然科学基金(22376229);广东省基础与应用基础研究基金(2023A1515010037)

Microstructure modulation of α-MnO₂ via mild urea-induced phase transition for enhanced catalytic ozonation of emerging contaminants

Peixin Zhu^a, Mengyao Xiao^a, Xixi Chen^c(), Jingsong Luo^d, Zhong Fang^d, Long Chen^d, Huinan Zhao^a, Chun He^a^,^b, Shuanghong Tian^a^,^b()

^a School of Environmental Science & Engineering, Sun Yat-sen University, Guangzhou 510275, Guangdong, China
^b Guangdong Provincial Key Laboratory of Environmental Pollution Control and Remediation, Guangzhou 510275, Guangdong, China
^c Department of Materials Science and Engineering, City University of Hong Kong, Hong Kong 610200, China
^d China National Chemical Southern Construction Investment Co., Ltd., Guangzhou 516000, Guangdong, China

Received:2025-09-01 Accepted:2025-09-15 Online:2026-05-18 Published:2026-04-16
Contact: *E-mail: xixichen@cityu.edu.hk, chenxixi8117@163.com (X. Chen),
tshuangh@mail.sysu.edu.cn (S. Tian).
About author:First author contact:CRediT authorship contribution statement
Peixin Zhu: Methodology, Software, Writing - original draft. Mengyao Xiao: Investigation, Data curation. Xixi Chen: Supervision, Conceptualization, Data curation, Writing - review & editing. Jingsong Luo: Resources, Funding acquisition. Zhong Fang: Resources, Funding acquisition. Long Chen: Resources, Funding acquisition. Huinan Zhao: Supervision, Conceptualization, Writing - review & editing. Chun He: Supervision, Conceptualization, Writing - review & editing. Shuanghong Tian: Supervision, Conceptualization, Writing - review & editing, Funding acquisition.
Supported by:
National Key Research and Development Program of China(2024YFC3712500);National Natural Science Foundation of China(22376229);Guangdong Basic and Applied Basic Research Foundation(2023A1515010037)

摘要/Abstract

摘要：

以抗生素为代表的新兴污染物由于具有难降解特性, 难以被传统工艺彻底去除, 广泛残留于水环境中, 其生物毒性对生态环境和人体健康构成严重威胁. 非均相催化臭氧氧化因其反应条件温和、操作简便、适应性强且二次污染少等特点, 在难降解废水处理中极具应用价值. 该技术的核心在于催化剂表面对臭氧的吸附与活化, 而氧空位(Ov)的构建能够有效增强臭氧的吸附与电子转移. 晶面工程是改变电子结构并产生大量金属氧化物缺陷的有效方法.因此, 通过微观结构调控设计具有丰富缺陷的高效催化剂, 成为催化臭氧氧化领域的重要研究方向. 本研究通过一种温和的尿素辅助热处理策略, 成功构建了富含氧空位的α-MnO₂(310)/Mn₃O₄异质结催化剂, 同时实现了异质结与晶面工程的协同调控, 为开发高效稳定的臭氧催化剂提供了新思路.

本研究通过控制制备条件(温度值和尿素投加量), 通过尿素诱导相变调控α-MnO₂微结构, 成功构建了富含Ov的α-MnO₂(310)/Mn₃O₄异质结材料(Mn400-0.125U), 该材料由48.6%的α-MnO₂(310)和51.4%的Mn₃O₄组成. 通过X-射线衍射(XRD)、扫描电镜、透射电镜(TEM)、X-射线光电子能谱(XPS)、固相电子自旋共振与Raman等表征手段, 证明了该材料中因为α-MnO₂的(310)晶面氧空位形成能低耦合异质结界面效应而产生了大量的Ov. 此外, 通过H₂-程序升温还原、电化学阻抗谱与循环伏安法的测试结果可知, Mn400-0.125U具有优异的氧化还原能力与电导率, 有利于提升臭氧氧化性能. 因此, Mn400-0.125U在催化臭氧氧化去除新污染物的过程中表现出优异的性能, 其对磺胺甲噁唑(SMZ)的降解速率常数高达7.7×10^‒2 min^‒1, 分别是α-MnO₂(310), Mn₃O₄和单独臭氧氧化体系的1.8倍、1.6倍和3.3倍. 该材料还具有超低投加量(0.1 g/L)、较宽pH适应性(3.5-10.5)和强抗水体基质干扰能力(去除率损失≤12.4%)等显著操作优势. 在连续五次循环实验中, Mn400-0.125U催化臭氧氧化SMZ的去除率维持在86.9%以上, 并且通过其反应前后的XRD, TEM, 高分辨TEM与XPS对比发现, Mn400-0.125U在反应过后具有显著的结构和化学稳定性, 证实了Mn400-0.125U的卓越运行稳定性. 机理实验和理论计算共同表明, 材料中丰富的Ov与其适宜的亲水性协同作用, 实现了臭氧的无能垒活化和分解, 并通过链式反应产生多种活性物种. Mn400-0.125U在催化臭氧氧化SMZ的过程中以电子转移、表面氧原子(O*)和单线态氧(¹O₂)为主的非自由基途径起主导作用, 而自由基途径(•O₂^‒/•OH)的贡献很小, 仅起到了次要作用.

综上, 本研究建立了一种简便的晶面工程耦合异质结协同调控方法, 用于制备富含氧空位等缺陷的锰氧化物, 并将其应用于新型污染物的催化臭氧氧化处理. 该研究成果为设计高性能非均相催化剂及深入理解表面缺陷促进的氧化机制提供了理论和实验依据.

关键词: 晶面调控, 异质结, 锰基催化剂, 氧空位, 催化臭氧化

Abstract:

While facet engineering and heterostructure construction are recognized as effective strategies for enhancing catalytic performance through defect creation, their integration remains scarce and challenging. This study develops a mild urea-assisted thermal strategy to construct an oxygen vacancy (OV)-rich α-MnO₂(310)/Mn₃O₄ heterojunction (Mn400-0.125U), comprising 48.6% α-MnO₂ with preferentially exposed (310) facets and 51.4% Mn₃O₄. The low OV formation energy on (310) facets coupled with heterojunction interfaces effects leads to a high OV concentration. Mn400-0.125U demonstrated exceptional catalytic ozonation performance, achieving a sulfamethoxazole degradation rate constant (7.7×10^-2 min^-1), which is 1.8-, 1.6-, and 3.3-fold higher than those of α-MnO₂, Mn₃O₄, and single ozonation, respectively. Operational advantages include ultralow catalyst dosage (0.1 g/L), broad pH adaptability (3.5-10.5), and remarkable resilience against aqueous matrix interference (≤ 12.4% efficiency loss). Both experimental and theoretical calculations demonstrate that the abundant OVs, combined with the proper hydrophilicity of Mn400-0.125U, synergistically trigger barrier-free activation and decomposition of ozone, subsequently generating a series of reactive species via chain reactions. A hybrid oxidation regime was identified where the non-radical pathway mediated by electron-transfer, O* (surface oxygen atoms), and ¹O₂predominates over radical pathways (•O₂^-/•OH). This work establishes a facile coupled modulation protocol for creating defect-rich manganese oxides applied in catalytic ozonation of emerging contaminants.

Key words: Facet engineering, Heterojunction, Manganese-based catalysts, Oxygen vacancy, Catalytic ozonation

朱培新, 肖梦瑶, 陈茜茜, 罗旌崧, 房中, 陈龙, 赵慧楠, 何春, 田双红. 尿素诱导温和相变策略调控α-MnO₂微结构以增强新兴污染物催化臭氧氧化效能[J]. 催化学报, 2026, 84: 175-188.

Peixin Zhu, Mengyao Xiao, Xixi Chen, Jingsong Luo, Zhong Fang, Long Chen, Huinan Zhao, Chun He, Shuanghong Tian. Microstructure modulation of α-MnO₂ via mild urea-induced phase transition for enhanced catalytic ozonation of emerging contaminants[J]. Chinese Journal of Catalysis, 2026, 84: 175-188.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64889-3

https://www.cjcatal.com/CN/Y2026/V84/I5/175

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Fig. 1. (a) Schematic diagram of modulating the microstructure of α-MnO2. (b) Photograph of the modulated catalysts. XRD patterns of the catalysts modulated by urea-assisted thermal treatment at 400 °C (c) and 200 °C (d) with different urea dosage. Characteristic diffraction peaks at 18.1°, 28.9°, 37.6°, 42.0°, 49.9°, 60.2°, and 65.1° are corresponded to the (200), (310), (211), (301), (411), (521), and (022) planes of tetragonal α-MnO2 (JCPDS 44-0141). Characteristic diffraction peaks emerged at 18.0°, 31.0°, 32.3°, 36.1°, 44.4°, 59.8°, and 65.4° are indexed to the (101), (200), (103), (211), (220), (224), and (323) planes of tetragonal Mn3O4 (JCPDS 24-0734).

Fig. 2. SEM images of the pristine MnO2 (a), the modulated Mn400-0U (b), Mn400-0.125U (c), and Mn400-0.250U (d). TEM (e1-e2) and HRTEM (e3-e4) images of Mn400-0.125U (α-MnO2/Mn3O4). (e5) HRTEM images of Mn400-0.125U (α-MnO2/Mn3O4) after cycled reaction. (f1-f4) EDS elemental mapping images of Mn400-0.125U (α-MnO2/Mn3O4). Water contact angle measurements on Mn400-0U (α-MnO2) (g1), Mn400-0.125U(g2), and Mn400-0.250U (Mn3O4) (g3).

Fig. 3. XPS spectra of Mn 2p (a), O 1s (b), and N 1s (c) of Mn400-0U, Mn400-0.125U and Mn400-0.250U. ESR profiles (d) and Raman spectra (e) of Mn400-0U, Mn400-0.125U and Mn400-0.250U.

Table 1 Oxygen vacancies analysis of the catalysts indicated by XPS, ESR, and Raman.

Sample	[O_ads]/ [O_total]	[Mn²⁺+Mn³⁺] /[Mn_total]	ESR Intensity(a.u.) g = 2.003	Raman v₂/v₃(Mn-O)
Mn400-0U	21.9%	53.1%	0.24	1.254
Mn400-0.125U	34.3%	68.2%	0.72	1.087
Mn400-0.250U	30.0%	57.3%	0.33	1.202

Fig. 4. H2-TPR (a), EIS (b) and CV (c) curves of Mn400-0U, Mn400-0.125U and Mn400-0.250U.

Fig. 5. Removal of SMZ (a,b) and pseudo first-order kinetics fitting (c) for SMZ removal in ozonation and catalytic ozonation. Effects of catalyst dosage of Mn400-0.125U (d), initial solution pH (e,f), and water matrices (g) on the removal of SMZ or the pseudo first-order reaction constant of SMZ removal by catalytic ozonation. (h) Stability assessments by recyclability of Mn400-0.125U.

Fig. 6. (a) Evolution of ozone concentration along with the time in ozonation and catalytic ozonation. Effect of scavengers (b) and pseudo first-order kinetics fitting (c) for SMZ removal in Mn400-0.125U/O3 system. ESR spectra of DMPO-?OH (d), DMPO/DMSO-?O2? (e) and TEMP-1O2 adducts (f) in ozonation and catalytic ozonation.

Fig. 7. Optimized geometry structures and the calculated energy of M310-O3 (a), M310-OV-O3 (b), M310-OV-H2O-O3 (c), M101-O3 (d), and M101-H2O-O3 (e).

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尿素诱导温和相变策略调控α-MnO₂微结构以增强新兴污染物催化臭氧氧化效能

Microstructure modulation of α-MnO₂ via mild urea-induced phase transition for enhanced catalytic ozonation of emerging contaminants

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[1]	孙承阳, 张浩晨, 刘晓晖, 王艳芹. 氧空位促进C-H键活化提高Ru/CeO₂上聚乙烯氢解活性[J]. 催化学报, 2026, 84(5): 337-346.
[2]	张宝龙, 孙彬, 刘兴朋, 刘文宇, 顾少楠, 周国伟. 缺陷工程促进TiO₂/Zn_0.5Cd_0.5S S型异质结电荷转移实现高效光催化析氢[J]. 催化学报, 2026, 84(5): 117-129.
[3]	邢赟, 刘磊, 孔文晶, 田俊泰, 刘鹏, 杨臣, 付名利, 叶代启. 铈活化泡沫金属载体实现高效乙酸丁酯氧化: 内在氧化还原循环与界面电子转移的双重作用[J]. 催化学报, 2026, 84(5): 390-400.
[4]	初铭涛, 张慧敏, 任变清, 曹景, 章腾, 宋平, 王子准, 韩策, 徐维林. 非晶-晶体异质结构Ru_MoNiN/Ni-MoO₂用于高效稳定的碱性析氢反应[J]. 催化学报, 2026, 84(5): 96-105.
[5]	谢瑶瑶, 谭昌龙, 毛梁, 唐紫蓉, 徐艺军. 缺陷工程Pt/Nb₂O₅光催化剂实现高效羟乙基自由基介导的苯并咪唑合成与析氢协同反应[J]. 催化学报, 2026, 83(4): 132-142.
[6]	R. Kavitha, C. Manjunatha, S. Girish Kumar. 基于氧化锌的S型异质结: 设计原理、制备方法及光催化活性[J]. 催化学报, 2026, 83(4): 54-95.
[7]	李建荣, 张万鹏, 肖航, 田明姣, 何炽. 通过调节负载于MnO₂上的银初始状态促进乙酸乙酯低温深度氧化: 银纳米颗粒和离子的内在作用[J]. 催化学报, 2026, 83(4): 388-399.
[8]	唐克山, 邓莞沂, 王宁远, 夏阳, 吴新鹤, 杨恒. 富含氧空位的三嗪基-COF/TiO₂ S-型异质结用于高效光催化CO₂还原[J]. 催化学报, 2026, 83(4): 244-257.
[9]	许凯强, 朱文君, Mahmoud Sayed, 韩生. 一维S型光催化剂的设计与制备[J]. 催化学报, 2026, 83(4): 24-53.
[10]	廖紫怡, 蒋岚, 杨扬, 王霖, 杨为佑, 侯慧林. 碱-氰基双调控的g-C₃N₄/BiOCl S-型异质结用于纯水中高效可见光驱动H₂O₂光合成[J]. 催化学报, 2026, 83(4): 143-161.
[11]	张王刚, 谢昊辰, 王虹亮, 田入峰, 刘雷, 王剑, 刘一鸣. 原子级晶格匹配的六方相WO₃/TiO₂ S型异质结用于高效光电催化甘油选择性制备二羟基丙酮[J]. 催化学报, 2026, 82(3): 161-173.
[12]	陈春园, 王中辽, 马颖, 翁波, 陈士夫, 孟苏刚. 硫掺杂-氮空位协同增强二维/三维S型异质结光催化合成H₂O₂[J]. 催化学报, 2026, 82(3): 278-291.
[13]	孙欣然, 霍孟田, 孙健航, 梁宇, 秦愷池, 张浩杨, 邢子豪, 常进法. 金属硫化物前驱体的牺牲转化生成活性羟基氧化物催化剂以增强析氧反应[J]. 催化学报, 2026, 82(3): 84-91.
[14]	杨瑞, 韩子敏, 高音, 冯国庆, 刘怀志, 黄艺吟, 汪钟凯, 王要兵. MoNi₄/MoO₂异质结构实现安倍级电流环己酮电氧化-产氢反应[J]. 催化学报, 2026, 81(2): 344-354.
[15]	刘青桦, 蔡培庆, 李恒帅, 冀学洋, 张大凤, 蒲锡鹏. 可见光驱动的CdS/CuWO₄ S型异质结析氢体系: 界面电荷转移与光热活化的双重协同增强[J]. 催化学报, 2026, 81(2): 299-309.