碳化钼催化氨分解制氢: Mo/C比调控与相变动力学机制研究

doi:10.1016/S1872-2067(25)64726-7

催化学报 ›› 2025, Vol. 74: 365-376.DOI: 10.1016/S1872-2067(25)64726-7

碳化钼催化氨分解制氢: Mo/C比调控与相变动力学机制研究

孙博文^a^,¹, 穆思允^a^,¹, 陈冰冰^a^,^*(), 胡国骏^a, 高瑞^b^,^*(), 石川^a^,^*()

^a大连理工大学化学学院, 精细化工国家重点实验室, 辽宁大连 116024
^b内蒙古大学化学化工学院, 内蒙古呼和浩特 010021

收稿日期:2024-12-31 接受日期:2025-04-17 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: chuanshi@dlut.edu.cn (石川),gaorui@imu.edu.cn (高瑞),chenbb@dlut.edu.cn (陈冰冰).
作者简介:¹共同第一作者.
基金资助:
国家重点研发计划(2021YFA1501102);国家自然科学基金(21932002);国家自然科学基金(22276023);国家自然科学基金(22402019);国家自然科学基金(22172083);前沿科学中心基金(DUT22LAB602);辽宁滨海实验室资助项目(LBLF-2023-06)

Hydrogen production via ammonia decomposition on molybdenum carbide catalysts: Exploring the Mo/C ratio and phase transition dynamics

Bowen Sun^a^,¹, Siyun Mu^a^,¹, Bingbing Chen^a^,^*(), Guojun Hu^a, Rui Gao^b^,^*(), Chuan Shi^a^,^*()

^aState Key Laboratory of Fine Chemicals, School of Chemistry, Dalian University of Technology, Dalian 116024, Liaoning, China
^bCollege of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021, Inner Mongolia, China

Received:2024-12-31 Accepted:2025-04-17 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: chuanshi@dlut.edu.cn (C. Shi), gaorui@imu.edu.cn (R. Gao), chenbb@dlut.edu.cn (B. Chen).
About author:¹Contributed equally to this work.
Supported by:
National Key R & D Program of China(2021YFA1501102);National Natural Science Foundation of China(21932002);National Natural Science Foundation of China(22276023);National Natural Science Foundation of China(22402019);National Natural Science Foundation of China(22172083);Fundamental Research Funds for the Central Universities(DUT22LAB602);Liaoning Binhai Laboratory Project(LBLF-2023-06)

摘要/Abstract

摘要：

氨(NH₃)作为无碳氢能载体, 具有储氢密度高(17.8 wt%), 能量密度大(3000 Wh/kg), 及制造和运输技术成熟等优势. 通过氨分解制氢(ADR)是分布式氢能供应的重要途径. 然而, 该技术面临非贵金属催化剂活性不足与结构失稳的挑战. 尽管氮化钼(Mo₂N, MoN)在ADR中研究广泛, 但同属间隙化合物的碳化钼(α-MoC, β-Mo₂C)的催化行为与构效关系尚不明确.

碳化钼的独特性质在于其多相结构, 不同晶相的催化行为有明显差异. 在涉及氨的反应中, 碳化钼的动态结构变化对反应机理和反应效率至关重要. 本文聚焦于碳化钼(α-MoC和β-Mo₂C)催化剂在氨分解反应中的应用, 系统探究了不同Mo/C比例对催化性能及结构演变的影响. 实验通过程序升温碳化法制备了立方相α-MoC和六方相β-Mo₂C, X射线光电子能谱结果表明, 二者表面Mo/C比例存在显著差异(β-Mo₂C的Mo/C为1.48, α-MoC为0.73). 催化性能测试表明, 具有高Mo/C比的β-Mo₂C在450 °C下的周转频率为1.3 s^-1, 是α-MoC(0.1 s^-1)的十余倍, 且表观活化能更低(89.8 vs. 107.4 kJ/mol). 此外, 在600 °C的ADR稳定性评价中, α-MoC略微下降后维持稳定. β-Mo₂C在15 h内很快失活22.3%, 但在随后100 h的测试过程中实现了稳定的氨转化. 随后的表征结果表明, α-MoC和β-Mo₂C都发生了拓扑相变, 其中α-MoC相变为Mo₂N, β-Mo₂C相变为MoN. 进一步研究表明, 表面Mo/C比例的提升直接促进了氢气产率, 其机制源于β-Mo₂C更优的氮物种结合能力. 通过氨气脉冲和程序升温氮气脱附表面反应结合密度泛函理论计算证实, 氮物种的结合步骤为ADR的速率控制步骤, β-Mo₂C通过降低该步骤能垒(1.68 vs. 2.33 eV)显著加速N₂脱附. 此外, 碳化钼向氮化钼的相变是由于氮物种无法脱附而在催化剂表面累积, 进而向体相迁移的结果, 高温反应(810 °C)下, N物种缔合脱附速率加快, β-Mo₂C可维持碳化物相, 避免因氮渗透导致相变, 而α-MoC在H₂/NH₃气氛中易发生结构崩塌.

综上所述, 本研究阐明了碳化钼(α-MoC和β-Mo₂C)表面组成与相变动力学的内在关联, 通过调控Mo/C比例及优化反应温度, 实现了β-Mo₂C兼具高活性与抗相变的能力, 为设计高效稳定的氨分解催化剂提供了新思路.

关键词: 碳化钼, 相变, 氮化, 重组, 氨分解反应

Abstract:

The deployment of non-precious metal catalysts for the production of CO_x-free hydrogen via the ammonia decomposition reaction (ADR) presents a promising yet great challenge. In the present study, two crystal structures of α-MoC and β-Mo₂C catalysts with different Mo/C ratios were synthesized, and their ammonia decomposition performance as well as structural evolution in ADR was investigated. The β-Mo₂C catalyst, characterized by a higher Mo/C ratio, demonstrated a remarkable turnover frequency of 1.3 s^-1, which is over tenfold higher than that of α-MoC (0.1 s^-1). An increase in the Mo/C ratio of molybdenum carbide revealed a direct correlation between the surface Mo/C ratio and the hydrogen yield. The transient response surface reaction indicated that the combination of N^* and N^* derived from NH₃ dissociation represents the rate-determining step in the ADR, and β-Mo₂C exhibited exceptional proficiency in facilitating this pivotal step. Concurrently, the accumulation of N^* species on the carbide surface could induce the phase transition of molybdenum carbide to nitride, which follows a topological transformation. It is discovered that such phase evolution was affected by the Mo-C surface and reaction temperature simultaneously. When the kinetics of combination of N^* was accelerated by rising temperatures and its accumulation on the carbide surface was mitigated, β-Mo₂C maintained its carbide phase, preventing nitridation during the ADR at 810 °C. Our results contribute to an in-depth understanding of the molybdenum carbides’ catalytic properties in ADR and highlight the nature of the carbide-nitride phase transition in the reaction.

Key words: Molybdenum carbides, Phase transition, Nitridation, Recombination, Ammonia decomposition reaction

孙博文, 穆思允, 陈冰冰, 胡国骏, 高瑞, 石川. 碳化钼催化氨分解制氢: Mo/C比调控与相变动力学机制研究[J]. 催化学报, 2025, 74: 365-376.

Bowen Sun, Siyun Mu, Bingbing Chen, Guojun Hu, Rui Gao, Chuan Shi. Hydrogen production via ammonia decomposition on molybdenum carbide catalysts: Exploring the Mo/C ratio and phase transition dynamics[J]. Chinese Journal of Catalysis, 2025, 74: 365-376.

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https://www.cjcatal.com/CN/Y2025/V74/I7/365

图/表 6

Fig. 1. Characterization of the prepared α-MoC and β-Mo2C catalysts. (a) Schematic illustration of α-MoC and β-Mo2C catalysts prepared from MoO3 by different carburization pathway. XRD pattern (b), C 1s and Mo 3d (c) XPS spectra of α-MoC and β-Mo2C. (d) Surface Mo/C atomic ratios of Mo carbides calculated from Mo 3d and C 1s spectra. (e,f) HRTEM images of α-MoC and β-Mo2C samples.

Fig. 2. (a) Temperature-dependent NH3 conversion of α-MoC and β-Mo2C in pure NH3 at a WHSV of 30,000 mL/(g·h). H2 yield normalized by the specific surface area of catalysts (b) and TOFs comparison (c) at 450 °C over α-MoC and β-Mo2C catalysts at a WHSV of 30000 mL/(g·h). (d) XRD patterns of α-MoC-t (t = 30, 60, 90, and 120 min) treated with H2/Ar flow. (e) NH3 conversion for the α-MoC-t catalysts at a WHSV of 30000 mL/(g·h). (f) Dependence of H2 production rate at 550 °C (WHSV of 30000 mL/(g·h)) on surface Mo/C atomic ratio. (g) Stability tests of α-MoC and β-Mo2C catalysts at 600 °C with a space velocity of 60000 mL/(g·h).

Fig. 3. NH3-TPD (a) and H2-TPD (b) profiles over α-MoC and β-Mo2C catalysts. (c) NH3-pulse reaction at 400 °C for the α-MoC and β-Mo2C. (d) Subsequent to the NH3-pulse reaction, an N2-TPD test was then carried out.

Fig. 4. (a) XRD pattern of fresh and spent Mo carbide catalysts. (b) XRD pattern of α-MoC and β-Mo2C after NH3 stability testing at different temperatures. Reaction conditions: 50 mg catalyst, WHSV of 30000 mL/(g·h), pure NH3, total flow rate of 25 mL/min. (c) NH3-TPSR and corresponding CH4 signal for the α-MoC and β-Mo2C. The CH4 signal was detected by an infrared absorption spectrometer (SICK-MAIHAK-S710). (d,e) HRTEM images and EDS elemental maps of spent α-MoC and β-Mo2C. Reaction conditions for the catalytic test for (a), (d), and (e): 50 mg catalyst at 600 °C, WHSV of 60000 mL/(g·h), pure NH3, total flow rate of 50 mL/min.

Table 1 Physical properties of the fresh and spent catalysts.

Sample	S_BET ^a (m²/g)	C^b (wt%)	N^b (wt%)	Phase structure ^c
α-MoC-fresh	126	8.94	—	α-MoC
α-MoC-spent-4 h	98	1.13	9.08	C doped Mo₂N
α-MoC-spent-120 h	79	0.58	7.02	Mo₂N
β-Mo₂C-fresh	13	5.78	—	β-Mo₂C
β-Mo₂C-spent-4 h	9	2.67	8.02	β-Mo₂C and MoN
β-Mo₂C-spent-120 h	7	0.70	9.96	MoN

Fig. 5. The energy profiles of NH3 dissociation on the catalysts of α-MoC and β-Mo2C. (a) the most favorable route of ADR. (b,c) The possible NHx coupling reactions, in which the corresponding structures are inserted and the Mo, C and N atom are marked in cyan, grey and blue, respectively.

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碳化钼催化氨分解制氢: Mo/C比调控与相变动力学机制研究

Hydrogen production via ammonia decomposition on molybdenum carbide catalysts: Exploring the Mo/C ratio and phase transition dynamics

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[1]	王尔玉, 褚艺淳, 张文君, 魏彦平, 司传领, Regina Palkovits, 吴新平, 陈祖鹏. 利用Pt-C₃N₄单原子催化剂实现木质纤维素光重整共生产H₂与乳酸[J]. 催化学报, 2025, 74(7): 308-318.
[2]	孙艳楠, 俞佳枫, 孙兴涛, 韩誉, 葛庆杰, 孙剑. 网状缺陷型碳化钼材料催化合成气经草酸二甲酯加氢合成乙醇[J]. 催化学报, 2025, 73(6): 234-241.
[3]	余文杰, 冯超, 李荣华, 张贝贝, 李严波. 用于光电化学水分解的氮化钽光阳极的研究进展[J]. 催化学报, 2025, 68(1): 51-82.
[4]	吴白婧, 李金芮, 罗小雪, 倪靖天, 卢伊婷, 邵敏华, 李存璞, 魏子栋. 电子催化剂直接固定N₂生成偶氮化合物[J]. 催化学报, 2025, 68(1): 386-393.
[5]	张棋祺, 苗慧, 王俊, 孙涛, 刘恩周. In_2.77S₄/K⁺掺杂g-C₃N₄自组装S型异质结光催化H₂O和O₂合成H₂O₂[J]. 催化学报, 2024, 63(8): 176-189.
[6]	杨冲亚, 王玮珏, 卓红英, 沈铮, 张天雨, 杨小峰, 黄延强. 晶相设计钌基纳米催化剂提高CO₂甲烷化活性[J]. 催化学报, 2024, 61(6): 226-236.
[7]	孟爱云, 马辛源, 温达, 钟威, 周双, 苏耀荣. 高选择性H₂O₂光合成: Ba原子注入面内高度有序结晶结构的g-C₃N₄纳米棒[J]. 催化学报, 2024, 60(5): 231-241.
[8]	王长安, 欧阳颖, 罗一斌, 高心茹, 高鸿毅, 王戈, 舒兴田. 相变储热材料强化催化反应过程的研究进展[J]. 催化学报, 2024, 60(5): 128-157.
[9]	孟令辉, 赵晨, 楚弘宇, 李渝航, 付会芬, 王鹏, 王崇臣, 黄洪伟. g-C₃N₄/PCN-224“壳-核”结构异质结压电-光催化协同高效制备过氧化氢[J]. 催化学报, 2024, 59(4): 346-359.
[10]	余治晗, 张岱南, 艾陈斌, 张建军, 向全军. 双连接工程D-π-A体系中光合作用生成H₂O₂的动态质子迁移[J]. 催化学报, 2024, 67(12): 71-81.
[11]	刘奔, 中川善直, 藪下瑞帆, 冨重圭一. Ir-Fe/BN催化剂上Ru物种在1,2-二醇氢解制仲醇反应中的促进作用[J]. 催化学报, 2024, 65(10): 89-102.
[12]	修子媛, 穆韡, 周欣, 韩晓军. 超薄氮化硼-铁-石墨烯三明治结构中的温和极化电场用于高效氮还原[J]. 催化学报, 2024, 65(10): 126-137.
[13]	Keshia Saradima Indriadi, 韩沛杰, 丁世鹏, 姚冰清, Shinya Furukawa, 何迁, 颜宁. 高分散的Pt促进氨分解中活性Fe_xN的形成[J]. 催化学报, 2023, 50(7): 297-305.
[14]	韦之栋, 严嘉玮, 郭伟琦, 上官文峰. 多面体SrTiO₃原位生长N缺陷PCN中的纳米叠层效应助力光催化完全分解水: 内建电场调控的协同机制[J]. 催化学报, 2023, 48(5): 279-289.
[15]	Sue-Faye Ng, 陈星竹, Joel Jie Foo, 熊墨, Wee-Jun Ong. 2D氮化碳: 通过调节非金属硼掺杂C₃N₅阐明宽酸性及碱性pH范围的光催化析氢的反应机理[J]. 催化学报, 2023, 47(4): 150-160.