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In situ/operando characterization techniques for electrochemical CO_(2)reduction

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Science China Chemistry 2023年第2期66卷 315-323页

作者： Xinning Song Liang Xu xiaofu sun Buxing Han Beijing National Laboratory for Molecular Sciences CAS Key Laboratory of Colloid and Interface and ThermodynamicsCAS Research/Education Center for Excellence in Molecular SciencesInstitute of ChemistryChinese Academy of SciencesBeijing100190China College of Science China Agricultural UniversityBeijing100193China School of Chemical Sciences University of Chinese Academy of SciencesBeijing100049China Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular EngineeringEast China Normal UniversityShanghai200062China

Utilizing CO_(2)as a carbon feedstock for producing fuels and useful chemicals is attractive due to the advantages of being abundant,nontoxic,and *** CO_(2)reduction(CO_(2)RR)provides an avenue to close the anthropogenic carbon ***,the reaction process of multi-electronic products of CO_(2)RR is quite *** is hard to yield a target product with high selectivity,high current density,low overpotential,and good stability *** recent years,in situ/operando characterization techniques have played important roles in the catalysis field via establishing the structure-reactivity/selectivity relationships of catalysts and thereby obtaining information about *** a result,it is necessary to apply in situ/operando characterization technologies to clarify the reaction pathway of CO_(2)*** this mini-review,we discuss recent progress on the in situ/operando characterizations for electrochemical CO_(2)RR,including microscopies,infrared spectroscopy,Raman spectroscopy,X-ray photoelectron spectroscopy,and X-ray absorption fine ***,the capabilities of these in situ/operando characterizations and the remaining challenges are also discussed.

关键词： carbon dioxide electrocatalysis in situ/operando characterization catalyst design reaction mechanism

Electrochemical reduction of CO_2 to CO using graphene oxide/carbon nanotube electrode in ionic liquid/acetonitrile system

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Science China Chemistry 2016年第5期59卷 551-556页

作者： Qinggong Zhu Jun Ma Xinchen Kang xiaofu sun Jiayin Hu Guanying Yang Buxing Han Beijing National Laboratory for Molecular Sciences CAS Key Laboratory of Colloid Interface and Chemical Thermodynamics Institute of Chemistry Chinese Academy of Sciences

Electrochemical reduction of CO_2 to CO is an interesting topic. In this work, we prepared metal-free electrodes by depositing graphene oxide(GO), multi-walled carbon nanotube(MWCNT), and GO/MWCNT composites on carbon paper(CP) using electrophoretic deposition(EPD) method. The electrodes were characterized by different methods, such as X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS). The electrochemical reduction of CO_2 to CO was conducted on the electrodes in 1-butyl-3-methylimidazolium tetrafluoroborate([Bmim]BF4)/acetonitrile(Me CN) electrolyte, and the composition of the electrolyte influenced the reaction significantly. It was demonstrated that GO/MWCNT-CP electrode was very effective for the reaction in IL(90 wt%)/Me CN binary mixture, the Faradaic efficiency of CO and current density were even higher than those on Au and Ag electrodes in the same electrolyte.

关键词： carbon dioxide electrochemical reduction carbon monoxide electrophoretic deposition carbon based materials

Selective electroreduction of carbon dioxide to formic acid on electrodeposited SnO_2@N-doped porous carbon catalysts

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Science China Chemistry 2018年第2期61卷 228-235页

作者： Lu Lu xiaofu sun Jun Ma Qinggong Zhu Congyi Wu Dexin Yang Buxing Han Beijing National Laboratory for Molecular Sciences CAS Key Laboratory of Colloid and Interface and Thermodynamics CAS Research/Education Center for Excellence in Molecular Sciences Institute of Chemistry Chinese Academy of Sciences School of Chemistry and Chemical Engineering University of Chinese Academy of Sciences

Electrocatalytic reduction of CO_2 is a promising route for energy storage and utilization. Herein we synthesized SnO_2 nanosheets and supported them on N-doped porous carbon (N-PC) by electrodeposition for the first time. The SnO_2 and N-PC in the SnO_2@N-PC composites had exellent synergistic effect for electrocatalytic reduction of CO_2 to HCOOH. The Faradaic efficiency of HCOOH could be as high as 94.1% with a current density of 28.4 mA cm-2 in ionic liquid-MeCN system. The reaction mechanism was proposed on the basis of some control experiments. This work opens a new way to prepare composite electrode for electrochemical reduction of CO_2.

关键词： CO2 reduction electrocatalyst ionic liquid porous carbon green chemistry

Efficient nitrate electroreduction over Mn-doped Cu catalyst via regulating N-containing intermediates adsorption configuration

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Science China Chemistry 2024年第6期67卷 1969-1975页

作者： Limin Wu Shunhan Jia Libing Zhang Ruhan Wang Jiaqi Feng xiaofu sun Buxing Han Beijing National Laboratory for Molecular Sciences CAS Laboratory of Colloid and Interface and ThermodynamicsCAS Research/Education Center for Excellence in Molecular SciencesCenter for Carbon Neutral ChemistryInstitute of ChemistryChinese Academy of SciencesBeijing100190China School of Chemical Sciences University of Chinese Academy of SciencesBeijing100049China College of Chemical Engineering and Environment China University of PetroleumBeijing102249China Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular EngineeringEast China Normal UniversityShanghai200062China

The electrochemical reduction of NO_(3)^(-)to NH_(3)holds promise for economic and environmental benefits,presenting an energyefficient alternative to the traditional Haber-Bosch ***,challenges exist due to its sluggish kinetics,multiple intermediates,and various reaction *** this study,Mn-doped-Cu catalyst was synthesized and employed for electrochemical NO_(3)^(-)-to-NH_(3)*** doping of Mn into Cu resulted in exceptional performance,achieving a FE of 95.8%and an NH_(3)yield rate of 0.91 mol g^(-1)h^(-1)at-0.6 V in a neutral electrolyte at low NO_(3)^(-)*** experimental studies and theoretical calculations revealed that the Mn dopant enhanced the kinetic rate of NO_(2)~--to-NH_(3)and induced a distinct configuration of**** alteration decreased the energy barrier of*NO-to-*NOH,consequently promoting the conversion of NO_(3)^(-)-to-NH_(3).

关键词： nitrate reduction electrocatalysis ammonia synthesis N-intermediate green chemistry

CO_(2)/NO_(x)-involved Electrochemical C-N Coupling Reactions

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Chemical Research in Chinese Universities 2024年第5期40卷 764-775页

作者： SUI Xiqing WU Limin JIA Shunhan JIN Xiangyuan sun xiaofu HAN Buxing Beijing National Laboratory for Molecular Sciences Key Laboratory of Colloid and Interface and ThermodynamicsCenter for Carbon Neutral ChemistryInstitute of ChemistryChinese Academy of SciencesBeijing100190P.R.China School of Chemical Sciences University of Chinese Academy of SciencesBeijing100049P.R.China Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular EngineeringEast China Normal UniversityShanghai200062P.R.China

With the excessive use of fossil fuels leading to significant CO_(2)emissions,and the continuous increase of NOx in water bodies and soils,the use of electrochemical methods for the conversion of CO_(2)and NOx has garnered widespread attention as a green chemical approach due to its advantages of being environmentally friendly,low-carbon,and straightforward.C—N bonds are widely present in many value-added chemicals,such as urea,amides,and ***,traditional methods for constructing C—N bonds typically involve thermochemical ***,using electrochemical methods to catalyze the reduction of CO_(2)and NOx for C—N bond formation has emerged as a green and sustainable *** paper summarizes the research progress of electrochemical C—N bond construction involving CO_(2)and NOx from the perspectives of reaction mechanisms and catalytic system construction,reviews the electrochemical synthesis of urea,amines,amides,and oximes through electrochemical C—N bond construction,and finally analyzes the current problems and challenges in the field,providing prospects for its future development.

关键词： CO_(2)reduction NOx reduction C-N coupling Electrocatalysis

Multicomponent catalyst design for CO2/N2/NOx electroreduction

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Industrial Chemistry & Materials

Industrial Chemistry & Materials 2023年第1期1卷 93-105页

作者： Shunhan Jia Limin Wu Liang Xu xiaofu sun Buxing Han Beijing National Laboratory for Molecular Sciences CAS Key Laboratory of Colloid and Interface and ThermodynamicsCAS Research/Education Center for Excellence in Molecular SciencesInstitute of ChemistryChinese Academy of SciencesBeijing100190China School of Chemical Sciences University of Chinese Academy of SciencesBeijing100049China Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular EngineeringEast China Normal UniversityShanghai200062China

Electroreduction of small molecules such as CO2,N2,and NO3−is one of the promising routes to produce sustainable chemicals and fuels and store renewable energy,which could contribute to our carbon neutrality *** multicomponent electrocatalysts,integrating the advantages of individual components of catalysts,are of great importance to achieve efficient electroreduction of small molecules via activation of inert bonds and multistep *** this review,some basic issues in the electroreduction of small molecules including CO2,N2,and NO3−are briefly *** then discuss our fundamental understanding of the rule of interaction in multicomponent electrocatalysts,and summarize three models for multicomponent catalysts,including type I,“a non-catalytically active component can activate or protect another catalytic component”;type II,“all catalytic components provide active intermediates for electrochemical conversion”;and type III,“one component provides the substrate for the other through conversion or adsorption”.Additionally,an outlook was considered to highlight the future directions of multicomponent electrocatalysts toward industrial applications.

关键词： Green chemistry Green carbon science Electroc atalysis Synergetic effect

Electrochemical Transformation of CO_(2)to Value-Added Chemicals and Fuels

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CCS Chemistry 2022年第10期4卷 3213-3229页

作者： Shunhan Jia Xiaodong Ma xiaofu sun Buxing Han Beijing National Laboratory for Molecular Sciences CAS Key Laboratory of Colloid and Interface and ThermodynamicsCAS Research/Education Center for Excellence in Molecular SciencesInstitute of ChemistryChinese Academy of SciencesBeijing 100190 School of Chemical Sciences University of Chinese Academy of SciencesBeijing 100049 Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular EngineeringEast China Normal UniversityShanghai 200062

CO_(2)is the main greenhouse gas and a renewable carbon *** transformation of CO_(2)(CO_(2)ET)to value-added chemicals and fuels is one of the promising routes to reduce CO_(2)emission and contributes to sustainability and carbon *** this review,we discuss recent developments on apparatuses used in CO_(2)ET,electrocatalytic reactions of CO_(2)with water,organics,nitrogen,and nitrogen-containing compounds to synthesize chemicals and fuels by the construction of different chemical bonds(e.g.,C–H,C–C,C–O,and C–N),and related reaction ***,an outlook was considered to highlight the opportunities and challenges in CO_(2)ET.

关键词： carbon dioxide green chemistry green carbon science electro-organic synthesis catalysis

Sm and S Co-doping to Construct Homo-hetero Cu Catalysts for Synergistic Enhancing CO_(2) Electroreduction

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Chinese Journal of Chemistry 2023年第12期41卷 1443-1449页

作者： Jiyuan Liu Pengsong Li Jiahui Bi Yong Wang Qinggong Zhu xiaofu sun Jianling Zhang Zhimin Liu Buxing Han Beijing National Laboratory for Molecular Sciences CAS Laboratory of Colloid and Interface and Thermodynamics CAS Research/Education Center for Excellence in Molecular Sciences Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China School of Chemical Science University of Chinese Academy of Sciences Beijing 100049 China Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular Engineering East China Normal University Shanghai 200062 China

Copper(Cu)is recognized as one of the most efficient metal catalysts that can perform the electrocatalytic CO_(2) reduction reaction(CO_(2)RR)and its surface oxidation state determines the reaction *** Cuδ+(0<δ<1)species,are well known active sites in CO_(2)RR to produce hydrocarbons and ***,Cuδ+active sites are difficult to control,and it is very easy to be reduced to Cu^(0) under CO_(2)RR operating ***,we report a homo-hetero doping strategy to construct an efficient samarium(Sm)and sulfur(S)co-doping catalyst(Smx-CuSy)for CO_(2)RR to formic acid(HCOOH).At optimum conditions,Smx-CuSy delivered a high HCOOH Faradaic efficiency(FE)of 92.1%at the current density of 300 mA·cm^(–2) using 1 mol/L KOH aqueous solution as electrolyte,and the reduction potential was as low as–0.52 V *** hydrogen electrode(RHE).The co-doping of Sm and S resulted in excellent CO_(2)RR performance owing to the synergistic effect of the homo-hetero *** homo-doping of S could effectively adjust the electronic structure of Cu in favor of the formation of abundant Cu^(δ+)*** existence of hetero-Sm species could not only stabilize the Cu^(δ+)sites,but also increase the concentration of H ions to form a favorable catalytic environment for HCOOH generation.

关键词： Carbon dioxide Electrochemistry Lanthanides Homo-hetero doping Copper

Asymmetric Cu Sites for Enhanced CO_(2)Electroreduction to C_(2+)Products

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CCS Chemistry 2024年第5期6卷 1231-1239页

作者： Weiwei Guo Xingxing Tan Shunhan Jia Shoujie Liu Xinning Song Xiaodong Ma Limin Wu Lirong Zheng xiaofu sun Buxing Han Beijing National Laboratory for Molecular Sciences Key Laboratory of Colloid and Interface and ThermodynamicsCenter for Carbon Neutral ChemistryInstitute of ChemistryChinese Academy of SciencesBeijing 100190 Institute of Molecular Metrology College of Chemistry and Chemical EngineeringQingdao UniversityQingdao 266071 School of Chemical Sciences University of Chinese Academy of SciencesBeijing 100049 School of Materials Science and Engineering Anhui UniversityHefei 230601 Institute of High Energy Physics Chinese Academy of SciencesBeijing 100049 Shanghai Key Laboratory of Green Chemistry and Chemical Processes School of Chemistry and Molecular EngineeringEast China Normal UniversityShanghai 200062

Cu-based electrocatalysts can have excellent activity for the generation of C_(2+)products from a CO_(2)reduction reaction(CO_(2)RR).Cuδ+species is crucial in tuning the performance of the ***,we discovered that Si-doped Cu catalysts had excellent performance for electrochemical CO_(2)to C_(2+)products.A high Faradaic efficiency(FE)of 84.7%was achieved with a current density of 289mA cm^(−2)in the flow-cell *** situ experimental results showed that the significant reconstruction occurred during the electrolysis,resulting in the formation of the asymmetric Cu sites(Cu^(0)-Cu^(+)).The ratio of Cu^(0)and Cu^(+)could be tuned by changing Si *** experiments and theoretical calculations demonstrated that the asymmetric Cu sites caused by the appropriate Si doping promoted CO_(2)activation and strengthened the adsorption of^(*)CO *** was beneficial to the subsequent^(*)CO–^(*)CO dimerization step,and thus,accounted for the enhancement of C_(2+)selectivity.

关键词： carbon dioxide electrocatalysis asymmetric Cu sites C-C coupling green chemistry