Chemical Research in Chinese Universities

Chemical Research in Chinese Universities Vol.39 No.4 August 2023

2023, 39(4): 0-0.

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Recent Advances in CO₂ Reduction Reaction to Value-added C1 Products by Single-atom Catalysts

LI Boyang, OU Honghui, CHEN Shenghua, SU Ya-Qiong, WANG Dingsheng

2023, 39(4): 527-544. doi:10.1007/s40242-023-3001-9

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The CO₂reduction reaction driven by sustainable electrical energy to value-added hydrocarbons is highly attractive because it can address both energy and environmental issues. The precise and rational development of corresponding electrocatalysts is of great importance to these kinds of reactions. Single-atom catalysts with unique electronic structures and coordination environments have become promising candidates, which may offer enhanced electrocatalytic performance. Herein, we summarize the recent development in the efficient fabrication of single-atom catalysts and their further application in CO₂ reduction. The various strategies for SACs preparation and characterization methods are highlighted to give a comprehensive understanding of the relationship between metal active sites and catalytic ability. The reaction mechanisms of electronic CO₂ reduction over single-atom catalysts are elaborated. Finally, the challenges and perspectives for the implementation of single-atom catalysts in CO₂ reduction are discussed.

Rare-earth Nanomaterials for Potential Brain Disease Theranostics

WEI Zheng, LIU Yawei, WANG Fan, LIU Kai, ZHANG Hongjie

2023, 39(4): 545-556. doi:10.1007/s40242-023-3125-y

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Brain diseases with high mortality cause severe threats to human health and life. Non-invasively high-resolution imaging technologies contribute to obtaining detailed brain structures to figure out the pathogenesis. In addition, timely visualization benefits the early warning and diagnosis of brain diseases. Rare-earth-based nanoparticles(RENPs) with excellent optical properties are highlighted for the diagnosis and treatment of brain diseases in recent years. Their tunable down-conversion fluorescence enables the high-resolution NIR-II fluorescence imaging of the brain. Besides, the excellent up-conversion luminescence can be applied to designing fluorescent probes to visualize brain diseases. Importantly, the surface of RENPs can be tailored to cross the blood-brain barrier, target the disease site in the brain and deliver drugs specifically, providing an effective tool for treating brain diseases. Excitingly, RENPs can be combined with emerging therapies, such as phototherapy, gas therapy and sonodynamic therapy, significantly improving the therapeutic effects of glioblastoma. This review summarizes the rational design, functionalization strategies and application of RENPs in brain imaging, diagnosis and therapy. Furthermore, a brief perspective on existing challenges and further development of RENPs is presented.

Current Understanding on the Unique Relaxation Dynamics of Sub-nanometer Materials and Their Structure-Property Relationships

XUE Binghui, LAI Yuyan, YANG Junsheng, YIN Jiafu, YIN Panchao

2023, 39(4): 557-567. doi:10.1007/s40242-023-3090-5

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Sub-nanometer materials(SNMs) define the emergent functional material system with their characteristic dimensions at sub-1 nm scale and they can be generally constructed with the sub-1 nm molecular clusters as the basic structural units. Due to their extremely small sizes, the sub-nm scale particles possess diffusive dynamics in their bulk with an energy level close to typical thermal fluctuation. Meanwhile, the volume fraction of surface structures becomes dominant and the dynamics of surface structures can be distinguishable from their diffusive dynamics. The research on the dynamics of SNM is key to the understanding of their unique properties in comparison to small molecule and nano-material systems. This review paper summarizes recent progresses in the studies of relaxation dynamics of SNM upon the combinatory application of X-ray/neutron scattering, dielectric spectroscopy and rheometric technology. The functional materials inspired by the dynamics investigations with applications in mechanical strengthening, ion conduction, and gas separation are also reviewed. In the end, challenges and outlooks on the theories, characterizations and the prediction of possible new functionalities of SNMs are discussed.

Nanoclusters as Synthons for Unit-Cell-Size Comparable One-Dimensional Nanostructures

FU Hao, DU Yaping

2023, 39(4): 568-579. doi:10.1007/s40242-023-3121-2

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The unit-cell-size comparable ultrathin nanowires(UCNWs) with typical cross-sectional dimension of around one nanometer, comparable to the unit-cell-size of inorganic materials, exhibit unique properties different from traditional nanomaterials. However, their facile and general synthesis is still a great challenge, since it not only demands the anisotropic growth in one direction, but also needs to completely restrict the growth in the other two dimensions. In this review, we summarize and introduce a strategy to prepare UCNWs using nanoclusters as synthons, which is promising to be a general synthesis method for UCNWs. We start with the introduction to the definition and characteristics of UCNWs. Subsequently, the key problems of UCNWs synthesis are analyzed from the perspective of thermodynamics and the strategy of using nanoclusters as synthons is proposed. Then, the related works about synthesis of UCNWs using magic-size clusters(MSCs) and polyoxometalate(POM) clusters as synthons are introduced and carefully discussed. Finally, challenges and opportunities are also elaborately discussed. This review is anticipated to provide a panoramic sketch and future directions toward the general synthesis of UCNWs.

Sub-nanomaterials for Photo/Electro-catalytic CO₂ Reduction: Achievements, Challenges, and Opportunities

WANG Xinyi, ZHAO Zhenwei, ZAHRA Kiran, LI Junjun, ZHANG Zhicheng

2023, 39(4): 580-598. doi:10.1007/s40242-023-3123-0

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With the increasing dilemma of energy crisis and climate change caused by excessive greenhouse gas emissions, it is an effective way to design low-cost and efficient catalysts to recycle CO₂ into value-added chemicals and fuels to solve these problems. Downsizing catalysts close to a single crystal cell, sub-nanomaterials(SNMs) show unique size-dependent properties and great potential applications in CO₂ reduction reaction (CO₂RR) compared with conventional nanomaterials. In this review, basic principles of CO₂RR and brief classification of SNMs are elucidated. Then, recent advances of SNMs in photo/electro-catalytic CO₂ reduction are comprehensively summarized. Finally, the current challenges and future outlooks are emphasized to pave the development of CO₂RR on SNMs. It is anticipated that this review would provide new insights to this unique scale and guided information on rational construction of SNMs for photo/electro-catalytic CO₂RR.

Rational Design of Nanostructured MnO₂ Cathode for High-performance Aqueous Zinc Ion Batteries

LI Qi, ZHAO Yajun, WANG Yueyang, Abdalla Kovan KHASRAW, ZHAO Yi, SUN Xiaoming

2023, 39(4): 599-611. doi:10.1007/s40242-023-3126-x

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Aqueous Zn-MnO₂ batteries hold a promising potential for grid-scale energy storage applications due to their intrinsic safety, low fabrication cost, environmental friendliness and high theoretical energy densities. Developing novel nanostructured cathode materials with high discharge voltage, large capacity and excellent structural stability is one of the critical ways to achieve the high-performance aqueous Zn batteries. Enlighten by that, comprehending principles of materials design and identifying the challenges faced by the state-of-the-art MnO₂ hosts are vital preconditions. Rather than a simple comparison, this review mainly focuses on design strategies regarding to MnO₂-based materials, including defect engineering, interfacial engineering, and pre-intercalation engineering. In addition, the energy storage mechanisms of MnO₂-based cathodes are discussed to clarify the complicated chemical reactions during battery cycling. Challenges and perspectives are outlined to guide the further development of advanced Zn-MnO₂ batteries.

Progress of Porphyrin-based Nanoassemblies for Cancer Theranostics

WANG Mengyue, HUANG Guan, YOU Zhongqi, JIA Rixin, ZHONG Yong, BAI Feng

2023, 39(4): 612-623. doi:10.1007/s40242-023-3127-9

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Porphyrins are indispensable in almost all forms of life. As photosensitizers, porphyrins have excellent imaging, photodynamic, photothermal, chemotherapeutic, and enzymatic properties, and play vital roles in biological diagnosis and therapy. However, the hydrophobicity of porphyrin molecules and the poor therapeutic effect of a single component on complex tumor systems hinder the applications of porphyrin monomers. Porphyrin assemblies could solve the problem of hydrophilicity and have good biocompatibility. First, this review briefly introduces the porphyrin self-assembly method, and the co-assembly of porphyrin and porphyrin, porphyrin and polymer, porphyrin and polypeptide, porphyrin and inorganic nanocrystals. The synergistic effect of co-assembly could solve the hydrophilia problem and achieve the enhanced functionalization. Then, the widened red shift of the spectrum, the increased yield, the increased drug loading, and the increased singlet oxygen yields are discussed. The research progresses of porphyrin-based assemblies in the direction of biological diagnosis and treatment are also reviewed. Finally, future perspectives and potential future research on the challenges are addressed.

High-entropy Metal Oxide-polyoxometalate-palladium Sub-1 nm Nanowires for Semi-hydrogenation Reaction of Alkynes

LIU Junli, NIE Siyang, WU Liang, WANG Xun

2023, 39(4): 624-629. doi:10.1007/s40242-023-3112-3

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Palladium and palladium-based nanomaterials have shown great catalytic potential in the semi-hydrogenation reaction of alkynes. However, the scarcity of noble metals, harsh reaction conditions, selectivity and over reduction of products limit the development of these kinds of catalysts. It is a smart strategy to fabricate the single-site palladium-based catalyst by introducing palladium into one-dimensional(1D) hybrid sub-1 nm nanowires (SNWs). Herein, we successfully synthesized several kinds of high-entropy metal oxide-polyoxometalate-Pd(HEO-POM-Pd) SNWs, which as the catalysts performed excellent catalytic activity and stereoselectivity in the semi-hydrogenation reaction of alkynes at room temperature, providing a promising avenue to design and prepare noble metal single-site catalysts at the sub-1 nm scale.

Hollow Multishelled Structural Li-rich Cathode with Al Doping Enabling Capacity and Voltage Stabled Li-ion Batteries

ZHAO Xiaolang, YANG Mei, WANG Jiangyan, WANG Dan

2023, 39(4): 630-635. doi:10.1007/s40242-023-3128-8

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Li-rich layered oxide cathode materials have drawn great attention due to their high specific capacity and relatively low cost. However, their implementation is hindered by capacity and discharge voltage decay as well as poor rate performance. Herein, by combining the concepts of geometrical and atomic structure design, hollow multishelled structural Li-rich cathode material doped with aluminum element(Li-rich HoMS-Al) is developed to solve the above challenges. Li-rich HoMS-Al is synthesized through a facile sequential templating approach with the shell number, element molar ratio and Al doping amount accurately controlled. HoMS can effectively buffer the stress/strain during cycling, as well as shorten the ion and electron diffusion path, while Al doping can inhibit the phase transition of the material and reduce the surface oxygen precipitation. As a result, it achieved a high specific capacity, stable voltage and capacity during cycling, exhibiting an initial discharge specific capacity up to 300.6 mA·h·g^-1 at 0.1 C(1 C=300 mA/g) and maintaining 246.3 mA·h·g^-1 after 100 cycles.

CeO₂ Supported on Reduced Graphene Oxide as Li-O₂ Battery Cathode

FU Zerui, WANG Shu, YU Haohan, NIE Meilin, FENG Xilan, ZUO Xintao, FU Lichao, LIU Dapeng, ZHANG Yu

2023, 39(4): 636-641. doi:10.1007/s40242-023-3107-0

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Li-O₂ battery(LOB) has an ultrahigh specific capacity(3500 W·h/kg), however, its slow kinetics of oxygen reduction reaction(ORR) and oxygen evolution reaction(OER) at cathode often leads to a high overpotential, a limited discharge capacity, and a poor cycling performance. Therefore, it is important to design and prepare cathode materials with a excellent catalytic activity. In this study, CeO₂ nanoparticles(NPs) supported on reduced graphene oxide(rGO) have been prepared and employed as cathode. Compared with either CeO₂ NPs or rGO, CeO₂/rGO cathode greatly improves the discharge capacity(10644 mA·h/g at a current density of 100 mA/g) and the cycling performance(95 cycles at 200 mA/g with a limited capacity of 500 mA·h/g) by virtue of the good conductivity of rGO and the oxygen storage/release capability of CeO₂.

Heterogeneous Seeded Growth of Chiral Au Nanostructures on PbS Nanocrystals

TAN Lili, WEN Zhihao, GENG Zhiyong, JIN Yiran, WU Hao, WANG Peng-peng

2023, 39(4): 642-646. doi:10.1007/s40242-023-3064-7

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Chiral plasmonic nanoparticles have been widely prepared through the seed-mediated overgrowth. However, the synthesis of chiral plasmonic-based hetero-nanostructures with multiple components via heterogeneous nucleation and growth has posed significant challenges. In this work, we develop a novel approach for the synthesis of chiral Au/PbS nano-heterostructures. This approach utilizes PbS nano-octahedrons as seeds and chiral cysteine-phenylalanine as symmetry-breaking agents to enable the selective growth of chiral Au on the single vertex of PbS nano-octahedrons. The optical properties of the resulting composites can be tuned by independently controlling synthetic parameters, such as the handedness and concentration of enantiomers and Au precursor. The chiral composites coupling PbS with plasmonic nanoparticles exhibit enhanced photoelectric performance compared with the corresponding achiral counterparts as a result of the difference in extinction and interface contacts between Au and PbS. This study provides a rational design for the construction of functional chiral nanostructures, not only expanding their application in various fields, such as chiral catalysis, spin devices, and chiral sensing, but also triggering new or enhanced properties by the integration of chiral plasmonic effect with other functional features.

pH-Induced Size Regulation of Ru Nanocrystals and the Applications Towards Proton Exchange Membrane Water Electrolysis

LI Miao, HAO Yashi, YANG Zuobo, YUN Jimmy, LIANG Xin

2023, 39(4): 647-653. doi:10.1007/s40242-023-3084-3

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Ruthenium(Ru) and its derivatives have been widely studied as oxygen evolution reaction(OER) electrocatalysts in acidic water electrolysis due to their inherent electronic properties and high oxygen evolution activity. A facile pH-induced size regulation approach for Ru nanocrystals has been developed by introducing NaOH and CH₃COOH in a polyol system. The size of Ru particles decreases with the increase of the dosage of NaOH and increases at a certain dosage of CH₃COOH. The formation mechanism of ruthenium nanocrystals was investigated through a series of characterizations and kinetic experiments. The electrocatalytic activities of the electrocatalysts derived from these Ru particles were studied toward OER to investigate the influence of particle size on their electrocatalytic properties. Moreover, the prepared electrocatalysts were applied as anodic materials in the proton exchange membrane(PEM) electrolysis cell and demonstrated excellent performance.

Tuning Photodetection Band of MAPbX₃(X=Cl/Br/I) Perovskite Single Crystals by Sub-nano Carbon Dot Doping

ZHU Xia, AN Jiakun, CHEN Gaoyu, XING Chenyu, BAO Jianchun, XU Xiangxing

2023, 39(4): 654-659. doi:10.1007/s40242-023-3086-1

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Perovskite single crystals are prominent semiconductor materials due to their high carrier mobility, long carrier diffusion length, and large absorption coefficient. They can be used as optoelectronic functional materials for narrowband or broadband photodetectors. In this report, the photodetection band tunability was achieved by doping MAPbX₃(MA=methylammonium, X=Cl/Br/I) perovskite single crystals with sub-nano carbon dots (MAPbX₃-C). The sub-nano size and good dispersibility of the carbon dots ensured controllable doping. The absorption of the sub-nano carbon dots and trap states in the MAPbX₃-C single crystals resulted in the special responsivity spectrum features.

Fe-substituted Polyoxometalate-based Spherical Assemblies as Catalysts for Olefin Epoxidation

HUANG Xinjie, WANG Ziru, WANG Tian, WANG Wei, HE Peilei

2023, 39(4): 660-665. doi:10.1007/s40242-023-3092-3

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Fe-substituted polyoxometalate(Na₁₅[(P₂W₁₅O₅₆)₂Fe₃])(Fe-POM)- based composite (C₁₉H₄₂N)₁₅[(P₂W₁₅O₅₆)₂Fe₃](CTAB-Fe-POM) was successfully synthesized through an ion-exchanged method. Then, it was self-assembly in a mixed solvent to form surfactant encapsulated complex nanosphere(SECN). The as-prepared SECN was employed as the catalyst for the epoxidation of olefins with H₂O₂. Compared with (C₁₉H₄₂N)₆[α-P₂W₁₈O₆₂](CTAB-P₂W₁₈), SECN shows a higher activity in the epoxidation of cis-cyclooctene with a high yield(97.3%). The extraordinary performance could be attributed to the amphiphilic module of cetyltrimethylammonium bromide(CTAB), which improves the dispersion of the catalyst in CH₃CN and accelerates the catalytic reaction. And Fe atom can rapidly activate H₂O₂, forming the active intermediate Fe-OOH to realize the transfer of active “O”. Furthermore, the catalyst could be reused five times without significant loss of activity.

Direct Observation of Crystalline Distortions in Mechanically Exfoliated Low-symmetric 2D Materials

LU Huoqing, SHEN Wanfu, WANG Haile, LIU Jiabao, YU Yu, MA Guoteng, LIU Hongguang, WU Sen, HU Chunguang

2023, 39(4): 666-672. doi:10.1007/s40242-023-3095-0

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Low-symmetrical two-dimensional(LSTD) materials have been increasing rapidly as a new exciting branch of two-dimensional (2D) materials, and their intrinsic in-plane anisotropic properties have been widely applied for polar and even novel devices. From a measurement perspective, anisotropy is also a valuable gauge for examining the properties changes of LSTD materials but is less investigated. Herein we demonstrate that the direct imaging of optical anisotropy of LSTD materials is an advanced methodology, achieving simultaneous measurement of morphology and highly sensitive intrinsic property, to examine the properties changes in the process of device fabrication. To this end, a homemade azimuth-dependent reflectance difference microscopy (ADRDM) method was applied for the optical anisotropy imaging of LSTD materials. Taking few-layered black phosphorus(BP) as an example, we observed apparent crystalline deformations in different zones of a BP crystal, revealing existing property modifications that cannot be detected by only morphology measurements of atomic force microscopy and optical microscopy. Besides, a large crystalline distortion of 20° was observed in a folding-existed BP flake induced by transferring process. These results establish the attention on the possible property modifications in the process of mechanical exfoliation and sample transferring and suggest ADRDM is an effective tool for online examination of property changes of LSTD materials in the process of device fabrications.

Crystalline-Amorphous Ni₃Se₄-Ni Hydroxide Heterostructure as an Efficient Electrocatalyst for Oxidation Evolution Reaction

WANG Teng, HU Renquan, WEI Hao, WEI Zehui, YAN Meng, YANG Yong

2023, 39(4): 673-679. doi:10.1007/s40242-023-3108-z

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Developing low-cost Ni-based amorphous/crystalline composites with well-defined nanostructures is expected to achieve a highly efficient oxygen evolution reaction(OER) by exposing more active sites and enhancing the electrical conductivity, but it still remains a synthetic challenge. Here, a crystalline/amorphous composite composed of crystalline Ni₃Se₄ and amorphous Ni hydroxide with a multi-layered bowl-shaped nanostructure was synthesized by a simple one-step solvothermal method. By regulating the concentration of sulfate ions in the reaction solution, the single-layered nanosheets achieve a transformation into a multi-layered structure with more exposed active sites. In addition, the crystalline-amorphous heterostructure allows regulation of the interfacial electronic structures, and the decoration of Ni₃Se₄ can effectively enhance the electrical conductivity of composites. Benefiting from the interfacial synergy between Ni₃Se₄ and Ni hydroxide, the as-optimized Ni₃Se₄/Ni hydroxide as an OER catalyst displayed superior electrocatalytic activity with a low overpotential of 285 mV at a current density of 10 mA/cm², a small Tafel slope of 68.3 mV/dec and remarkable stability in alkaline solution. This work offers a novel and effective method for the design of functional crystalline/amorphous composites for energy conversion and storage.

One-pot Mild Hydrothermal Synthesis of the Nanosheets Constructed Cobalt Silicate Hydroxide Hierarchical Porous Hollow Submicron Spheres as Efficient Adsorbents for Organic Dyes Removal

JIA Xiaohao, SUN Panpan, LIU Aoqun, CHEN Jinxiu, WANG Jingyi, ZHANG Heng, ZHU Wancheng

2023, 39(4): 680-689. doi:10.1007/s40242-023-3117-y

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Uniform Co₃Si₂O₅(OH)₄ hierarchical porous hollow submicron spheres(HPSSs, diameter: 100—220 nm; BET: 353.6 m²/g) constructed by ultrathin nanosheets are successfully prepared via a facile mild one-pot hydrothermal synthesis(140 °C, 12 h) in the presence of ethylene glycol by using CoCl₂·6H₂O, NH₄Cl, NH₃·H₂O and Na₂SiO₃·9H₂O as the raw materials. Meanwhile, a probable in situ etching and growth mechanism of the Co₃Si₂O₅(OH)₄ hierarchical porous submicron spheres(HPSSs) is proposed. When employed as the adsorbents, the Co₃Si₂O₅(OH)₄ HPSSs exhibit satisfactory adsorption performances for probe anionic dye Congo Red(CR) and cationic dye Rhodamine B(RhB), and the maximum adsorption capacities for CR and RhB are confirmed as 576 and 470 mg/g, respectively, higher than those of many other reported typical adsorbents. Both the adsorption isotherms and kinetics for CR and RhB follow the Langmuir and pseudo-second-order models. When the mimic industrial wastewater simultaneously containing CR and RhB is examined, the Co₃Si₂O₅(OH)₄ HPPSs can enable a fast removal efficiency as 99.9% within 3 min. In addition, the adsorption mechanism of the probe dyes on the HPSSs is discussed, and the satisfactory recycling performances also reveal the as-synthesized Co₃Si₂O₅(OH)₄ HPSSs as highly efficient adsorbents for the removal of CR and RhB from mimic wastewater.

Heavy Rare Earth Element Gd Enhancing Thermoelectric Performance in p-Type Polycrystalline SnSe via Optimizing Carrier Transport and Density of States

XU Pengfei, HUA Yezhen, JIN Kangpeng, XU Biao

2023, 39(4): 690-696. doi:10.1007/s40242-023-3120-3

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Tin selenide(SnSe) material exhibits very excellent thermoelectric properties in both p- and n-type single crystals, benefiting from advantageous electronic structure and ultra-low lattice thermal conductivity. However, poor mechanical properties and time-consuming production limit its practical application, and polycrystalline SnSe has attracted great attention in recent years. Herein, the SnSe microplates are prepared by a facile solvothermal method and compacted by spark plasma sintering (SPS). With enhanced electrical conductivity(σ) and optimized Seebeck coefficient(S) benefited from the Sn vacancies and increased density of states effective mass by the incorporating of heavy rare earth element Gd, an enhanced power factor(PF) value of about 0.86 mW/(m·K²) is realized in the p-type polycrystalline Sn_0.985Gd_0.015Se sample. Combined with the medium total thermal conductivity κ_tot and lattice thermal conductivity κ_lat of 0.7 and 0.56 W/(m·K), respectively, an enhanced peak dimensionless figure of merit(ZT) of ca. 1.1 was achieved at 873 K along vertical to the SPS pressing direction. The average ZT was also improved as compared to that of the pristine SnSe sample.

Optimized Preparation of CuS@SiO₂ Core-Shell Nanoparticles with Strong LSPR Absorption and Excellent Photostability for Highly Efficient Solar-driven Interfacial Water Evaporation

MENG Chenchen, HUANG Min, LI Yunchao

2023, 39(4): 697-704. doi:10.1007/s40242-023-3124-z

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Covellite copper sulfide nanocrystals(CuS NCs) are typical p-type semiconductors, showing strong optical absorption in the near-infrared(NIR) region thanks to their notable localized surface plasmon resonance(LSPR) properties. However, their LSPR properties and compositions are both highly susceptible to the external environment, which severely limits their practical applications. Until now, it remains a technical challenge to improve the structural and optical stability without sacrificing the LSPR performance of CuS NCs. Herein, to solve such a challenge, CuS@SiO₂ NPs with various silica shell thicknesses(CSNs-X nm) were synthesized in a well-controlled fashion via optimizing reverse microemulsion coating protocol. Compared with the pristine CuS NCs, the as-prepared CuS@SiO₂ NPs exhibited comparable LSPR properties but much higher photostability, enabling resistance to various harsh environments(e.g., high-power irradiation, strong reduction, and oxidation environment). Impressively, when used in solar-driven interfacial water evaporation, all the CuS@SiO₂ NPs exhibited excellent water evaporation performance with efficiencies beyond 70%(as high as 75.2% for CSN-23 nm) after 20 continuous testing cycles. Evidently, this paper is greatly helpful in better designing and fabricating high-performance plasmonic materials for practical photoelectrical, photothermal, and photocatalytic applications.

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