MnOx/CeO2-ZrO2复合氧化物的构筑及其在碳烟氧化中的应用

doi:10.15541/jim20240532

无机材料学报 ›› 2025, Vol. 40 ›› Issue (11): 1300-1308.DOI: 10.15541/jim20240532

• 研究快报 • 上一篇

MnO_x/CeO₂-ZrO₂复合氧化物的构筑及其在碳烟氧化中的应用

刘盼盼¹(), 姚鹏¹, 刘栩孜¹, 屈丽², 曾路¹, 宋兆华¹, 焦毅¹(), 王健礼¹^,², 陈耀强¹^,²

1.四川大学新能源与低碳技术研究院, 成都 610065
2.四川大学化学学院, 成都 610065

收稿日期:2024-12-23 修回日期:2025-04-19 出版日期:2025-11-20 网络出版日期:2025-05-09
通讯作者: 焦毅, 副研究员. E-mail: jiaoyiscu@163.com
作者简介:刘盼盼(2000-), 男, 硕士研究生. E-mail: liupanpan@stu.scu.edu.cn

MnO_x/CeO₂-ZrO₂ Composite Oxides: Construction and Application in Soot Oxidation

LIU Panpan¹(), YAO Peng¹, LIU Xuzi¹, QU Li², ZENG Lu¹, SONG Zhaohua¹, JIAO Yi¹(), WANG Jianli¹^,², CHEN Yaoqiang¹^,²

1. Institute of New Energy and Low-Carbon Technology, Sichuan University, Chengdu 610065, China
2. College of Chemistry, Sichuan University, Chengdu 610065, China

Received:2024-12-23 Revised:2025-04-19 Published:2025-11-20 Online:2025-05-09
Contact: JIAO Yi, associate professor. E-mail: jiaoyiscu@163.com
About author:LIU Panpan (2000-), male, Master candidate. E-mail: liupanpan@stu.scu.edu.cn
Supported by:
Advanced Materials-National Science and Technology Major Project(2024ZD0606500);National Natural Science Foundation of China(21902110);Sichuan Provincial Science Foundation(2023NSFSC0093)

摘要/Abstract

摘要：

汽油机尾气碳烟颗粒严重威胁着生态环境和人类健康, 而催化型汽油颗粒物过滤器(cGPF)是一种有效的净化技术, 其核心为催化剂涂层。本研究采用不同制备方法构筑了MnO_x/CeO₂-ZrO₂复合氧化物, 在低O₂浓度下考察了其碳烟氧化性能, 旨在开发具有卓越催化活性、稳定性以及抗水性的碳烟氧化催化剂涂层。结果表明, 通过浸渍法制备的MnO_x/CeO₂-ZrO₂(MCZ-IM)在1% O₂中, 其T₅₀(碳烟转化率达50%所需的温度)为329 ℃; 在0.5% O₂中, 其T₅₀为370 ℃。相较于高能球磨法(MCZ-HB)和共沉淀法(MCZ-CP)制备的催化剂, MCZ-IM展现出更优的综合性能。构效关系表明, 低O₂浓度下碳烟氧化性能与催化剂的织构和结构性质呈弱相关, 而与活性氧物种(AOS)——超氧(O₂^-)和过氧(O₂^2-)阴离子的生成及迁移密切相关, 其中涉及氧化还原性能、储释氧能力以及氧空位数量。MCZ-IM在氧物种的吸附、活化和脱附方面更具优势, 因此浸渍法被认为是提高AOS生成和迁移的更优方法。本研究不仅提供了一种适用于实际运行条件下颗粒物(PM)氧化催化剂的制备策略, 而且深入揭示了低O₂浓度环境中AOS的迁移机制。

关键词: MnO_x/CeO₂-ZrO₂, 催化剂, 碳烟, 活性氧物种

Abstract:

Gasoline soot particles pose a severe threat to the ecological environment and human health, but they can be potentially filtered out by using catalytic gasoline particulate filter (cGPF), whose core component is a catalyst coating. To develop more effective catalyst coatings with excellent activity, stability, and water resistance, a kind of composite oxide MnO_x/CeO₂-ZrO₂ was synthesized using different methods, and its soot oxidation performance was evaluated under low O₂ concentrations. Herein, MnO_x/CeO₂-ZrO₂ prepared by impregnation (abbreviated as MCZ-IM) exhibits a T₅₀ (temperature required for 50% soot conversion) of 329 ℃ in 1% O₂ and 370 ℃ in 0.5% O₂, displaying better comprehensive performance when compared to catalysts prepared by high-energy ball milling (abbreviated as MCZ-HB) and co-precipitation (abbreviated as MCZ-CP). Structure-activity relationship reveals that soot oxidation under low O₂ concentrations is weakly correlated with textural and structural properties, but strongly depends on the generation and migration of active oxygen species (AOS), especially superoxide (O₂^-) and peroxide (O₂^2-) anions, which are linked to redox properties, oxygen storage and release capacity, as well as amount of oxygen vacancies. The impregnation method enhances oxygen species adsorption, activation and desorption more effectively, endowing it with a more effective approach to enhancing AOS generation and mobility. Therefore, this study not only provides a preparation strategy for particulate matter oxidation catalysts applicable to actual operating conditions, but also offers insights into the migration of AOS at low O₂ concentrations.

Key words: MnO_x/CeO₂-ZrO₂, catalyst, soot, active oxygen species

中图分类号:

O643

刘盼盼, 姚鹏, 刘栩孜, 屈丽, 曾路, 宋兆华, 焦毅, 王健礼, 陈耀强. MnO_x/CeO₂-ZrO₂复合氧化物的构筑及其在碳烟氧化中的应用[J]. 无机材料学报, 2025, 40(11): 1300-1308.

LIU Panpan, YAO Peng, LIU Xuzi, QU Li, ZENG Lu, SONG Zhaohua, JIAO Yi, WANG Jianli, CHEN Yaoqiang. MnO_x/CeO₂-ZrO₂ Composite Oxides: Construction and Application in Soot Oxidation[J]. Journal of Inorganic Materials, 2025, 40(11): 1300-1308.

图/表 13

参考文献 53

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Sample	Surface area^a /(m²•g^-1)	Pore volume^a /(mL•g^-1)	Mean pore diameter^a /nm	Crystallinity^b /%	Grain size^c /nm
CZ	110.3	0.26	9.40	52.1	7.2
MCZ-CP	145.9	0.34	9.64	40.2	5.1
MCZ-IM	79.2	0.22	11.30	45.6	7.4
MCZ-HB	81.3	0.22	10.80	44.8	7.6

Sample	Surface area^a /(m²•g^-1)	Pore volume^a /(mL•g^-1)	Mean pore diameter^a /nm	Crystallinity^b /%	Grain size^c /nm
CZ	110.3	0.26	9.40	52.1	7.2
MCZ-CP	145.9	0.34	9.64	40.2	5.1
MCZ-IM	79.2	0.22	11.30	45.6	7.4
MCZ-HB	81.3	0.22	10.80	44.8	7.6

Sample	Mass fraction/%
Sample	O	Mn	Zr	Ce
MCZ-CP	24.38	2.98	22.44	50.20
MCZ-IM	24.13	7.54	23.14	45.18
MCZ-HB	21.52	1.03	24.58	52.87

Sample	Mass fraction/%
Sample	O	Mn	Zr	Ce
MCZ-CP	24.38	2.98	22.44	50.20
MCZ-IM	24.13	7.54	23.14	45.18
MCZ-HB	21.52	1.03	24.58	52.87

Catalyst	Ce³⁺/Ce	Ce⁴⁺/Ce	Mn⁴⁺/Mn	(O₂^2-+O₂^-)/O_T	O₂^-/O_T
CZ	0.21	0.79	—	0.28	0.09
MCZ-CP	0.14	0.86	0.36	0.35	0.11
MCZ-IM	0.15	0.85	0.39	0.34	0.17
MCZ-HB	0.17	0.83	0.32	0.31	0.06

MnO_x/CeO₂-ZrO₂复合氧化物的构筑及其在碳烟氧化中的应用

MnO_x/CeO₂-ZrO₂ Composite Oxides: Construction and Application in Soot Oxidation

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Catalyst	Method	Reaction condition (gas and flow rate)	Heating rate/ (℃•min^-1)	Catalyst and soot mass ratio	Contact mode	T₅₀/T_max/℃	Ref.
MCZ-IM	Incipient wetness impregnation	1% O₂	5	10 : 1	Tight	329	This work
MCZ-IM	Incipient wetness impregnation	0.5% O₂(500 mL/min)	5	10 : 1	Tight	370	This work
M10-CZ	Co-precipitation	0.5% O₂ (500 mL/min)	5	10 : 1	Loose	520	[S1]
Mn₂O₃	Flame spray pyrolysis	1% O₂ + 2% H₂O (500 mL/min)	3.3	15 : 1	Tight	321	[S4]
10LM-CZ	Co-precipitation and citric acid complexation impregnation	1% O₂ (100 mL/min)	5	10 : 1	Tight	362	[S5]
0.57Mn-CeO₂	Nitrate aerosol pyrolysis	10% O₂ (100 mL/min)	10	4 : 1	Tight	355	[S6]
5 Mn-CP	Solution combustion synthesis	Air (100 mL/min)	10	10 : 1	Tight	365	[S7]
CM5	EDTA-Citrate	Air (100 mL/min)	10	10 : 1	Tight	360	[S8]
Ce_0.5Mn_0.5O₂	Sol-gel	12% O₂(100 mL/min)	15	4 : 1	Tight	383	[S9]
CMO_st	Solvothermal	-	10	19 : 1	Tight	442	[S10]
CM	Co-precipitation	Air (100 mL/min)	10	4 : 1	Tight	396	[S11]
CMC	Co-precipitation	Air (100 mL/min)	-	4 : 1	Tight	363	[S12]
Ce_0.9Mn_0.1	Solid-phase grinding	10% O₂ (50 mL/min)	10	10 : 1	Tight	389	[S13]
Mn-Fib Ce	Plasma-assisted deposition	18% O₂ + 0.1%NO (20 mL/min)	5	20 : 1	Tight	384	[S14]

Sample	Element	Atomic fraction/%				Mass fraction/%
Sample	Element	Area 1	Area 2	Area 3	Average	Area 1	Area 2	Area 3	Average
MCZ-CP	O	62.48	66.22	69.82	66.17	21.55	24.14	27.45	24.38
	Mn	2.49	2.85	2.92	2.75	2.52	3.06	3.37	2.98
	Zr	15.70	11.73	10.37	12.60	26.47	20.91	19.94	22.44
	Ce	19.33	19.20	16.89	18.47	49.45	51.90	49.24	50.20
MCZ-IM	O	60.16	63.95	68.43	64.18	21.21	24.43	26.76	24.13
	Mn	6.91	8.73	4.92	6.86	7.16	9.81	5.66	7.54
	Zr	16.25	12.07	9.86	12.73	28.02	22.54	18.86	23.14
	Ce	16.68	15.25	16.80	16.24	43.61	43.22	48.72	45.18
MCZ-HB	O	61.05	65.04	63.64	63.24	20.63	22.36	21.58	21.52
	Mn	0.89	0.91	1.30	1.03	0.88	0.92	1.30	1.03
	Zr	19.84	11.62	12.91	14.79	32.79	19.54	21.41	24.58
	Ce	18.23	22.43	22.15	20.94	45.70	57.19	55.71	52.87

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