Small Methods最新文献

Refined Protocol for Improving Accuracy and Reliability in Urea Quantification During Electrochemical C─N Coupling Reactions.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-24 DOI: 10.1002/smtd.202401336

Weidong Dai, Shiyong Mou, Siyuan Liu, Peng Xu, Chiyao Tang, Keying Wu, Xing'an Dong, Lei Xiao, Chang Long, Fan Dong

{"title":"Refined Protocol for Improving Accuracy and Reliability in Urea Quantification During Electrochemical C─N Coupling Reactions.","authors":"Weidong Dai, Shiyong Mou, Siyuan Liu, Peng Xu, Chiyao Tang, Keying Wu, Xing'an Dong, Lei Xiao, Chang Long, Fan Dong","doi":"10.1002/smtd.202401336","DOIUrl":"https://doi.org/10.1002/smtd.202401336","url":null,"abstract":"Promoted by the growing demand for sustainable carbon and nitrogen cycling, electrochemical C─N coupling in urea synthesis has attracted intensive interest. Urea quantification provides the basis for an in-depth understanding of structure-performance correlations and the iterative optimization of performance. However, current urea quantification methods have non-negligible drawbacks, largely bringing about false positive or negatives risks. Herein, the most accessible and commonly used quantification techniques, namely the diacetylmonoxime-thiosemicarbazide and Urease-based methods, are comprehensively re-assessed. The adverse impacts caused by nitrite, metallic impurities, and standard curve protocol are thoroughly identified. Most importantly, direct problem-solving strategies are proposed to rule out those confounding factors by chemical pre-reduction, galvanic replacement, and refinement of the standard curve protocol, respectively. This refined urea quantification method can solidify the reproduction of urea electrosynthesis studies and thus promote the sound development of this emerging field.","PeriodicalId":229,"journal":{"name":"Small Methods","volume":" ","pages":"e2401336"},"PeriodicalIF":10.7,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690477","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Selective Nitrogen Doping at Hole Edges of Holey Graphene: Enhancing Ionic Transport Mechanisms for High-Performance Supercapacitors.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-24 DOI: 10.1002/smtd.202402038

John Peter Isaqu, Chun-Wei Huang, Jui-Kung Chih, Bo Yan Huang, Mohanapriya Subramani, I-Yu Tsao, Bor Kae Chang, Ching Yuan Su

{"title":"Selective Nitrogen Doping at Hole Edges of Holey Graphene: Enhancing Ionic Transport Mechanisms for High-Performance Supercapacitors.","authors":"John Peter Isaqu, Chun-Wei Huang, Jui-Kung Chih, Bo Yan Huang, Mohanapriya Subramani, I-Yu Tsao, Bor Kae Chang, Ching Yuan Su","doi":"10.1002/smtd.202402038","DOIUrl":"https://doi.org/10.1002/smtd.202402038","url":null,"abstract":"Developing highly holey graphene with controllable doping enhances ionic transport and conductivity, boosting the performance of energy storage devices like supercapacitors. However, the method for precise site-selective doping and the effects of heterogeneous atomic doping at pore edges on ion transport remain not fully understood. This study presents a method to achieve precisely and selectively high nitrogen doping (N-doping) at the hole edges of porous graphene (N-EHG) through a two-step process. Compared to untreated graphene (HG) and basal plane-doped graphene (N-BHG), N-EHG demonstrates superior charge storage capacity and ionic conductivity. Analyzing the porous structure, size distribution, and hydrophilicity influenced by the carbon-oxygen ratio, N-EHG shows a specific surface area of 509 m2 g-1, significantly higher than HG's 100 m2 g-1. Electrochemical results revealed that N-BHG and N-EHG achieved high gravimetric capacitances of 482.3 and 624.4 F g-1, respectively, due to enhanced ion diffusion, exceeding HG by ≈12- and 15.6-fold. Furthermore, the assembled coin-cell retains over 99% capacitance after 15,000 cycles, demonstrating exceptional stability. Both N-EHG and N-BHG show diffusion-governed charge storage, with N-EHG benefitting further from edge-state N-doping. Density Functional Theory (DFT) calculations reveal a lower energy barrier for ion diffusion and strong K⁺ adsorption on edge pyridinic-N, where increased electrode charge creates a negative center on N-dopants, enhancing K⁺ binding. These findings underscore the potential of edge-state N-doping in holey graphene for advanced energy storage applications.","PeriodicalId":229,"journal":{"name":"Small Methods","volume":" ","pages":"e2402038"},"PeriodicalIF":10.7,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143690481","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Impact of Geometry on Chemical Analysis Exemplified for Photoelectron Spectroscopy of Black Silicon.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-23 DOI: 10.1002/smtd.202401929

Jens U Neurohr, Anton Wittig, Hendrik Hähl, Friederike Nolle, Thomas Faidt, Samuel Grandthyll, Karin Jacobs, Michael A Klatt, Frank Müller

引用次数: 0

Filter-Assisted ICP-MS Tumor Liquid Biopsy Enabled by Dual-Target-Regulated Functional DNA Nanospheres Cascade Amplification.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-22 DOI: 10.1002/smtd.202500314

Yiman Wu, Yue Wang, Li Yan, Ke Huang, Kai Chang, Piaopiao Chen

{"title":"Filter-Assisted ICP-MS Tumor Liquid Biopsy Enabled by Dual-Target-Regulated Functional DNA Nanospheres Cascade Amplification.","authors":"Yiman Wu, Yue Wang, Li Yan, Ke Huang, Kai Chang, Piaopiao Chen","doi":"10.1002/smtd.202500314","DOIUrl":"https://doi.org/10.1002/smtd.202500314","url":null,"abstract":"An ultrasensitive ICP-MS aptasensor is developed utilizing a label-free, simple filter membrane-assisted separation technique combined with nucleic acid signal amplification for the analysis of circulating tumor cells (CTCs) in lung cancer clinical samples. The approach is based on the high-affinity interaction between aptamers and PD-L1 and mucin 1, which are overexpressed on the cell surface, in conjunction with functional Y-DNA nanospheres and catalytic hairpin assembly amplifications, enabling the simultaneous detection of two proteins. Additionally, a four-armed nanostructure with significant spatial site resistance is self-assembled by introducing streptavidin with biotinylated-hairpin structures, improving the separation efficiency of the filter membrane. This structural design enables the effective isolation of biotin-T-Hg2+-T and biotin-C-Ag+-C from free Hg2+ and Ag+, facilitating highly sensitive dual-protein detection via ICP-MS. The limits of detection reached ag mL-1 levels for proteins and single-cell levels for A549 cells. CTCs are extracted from whole blood samples of lung cancer patients within 45 min through a simple centrifugation procedure. Quantification of CTCs is performed in 37 clinical samples, demonstrating results consistent with clinical diagnoses. The assay exhibits a specificity of 100% and a sensitivity of 94.5%.","PeriodicalId":229,"journal":{"name":"Small Methods","volume":" ","pages":"e2500314"},"PeriodicalIF":10.7,"publicationDate":"2025-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143676669","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Advanced Fabrication of Ultrathin Ruthenium Films Using Synergistic Atomic Layer Deposition and Etching.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-21 DOI: 10.1002/smtd.202402166

Jeongbin Lee, Jung-Tae Kim, Jieun Oh, Dongjun Lee, Seo-Hyun Lee, Hyekyung Kim, Jiwoo Oh, Younseon Wang, Woo-Hee Kim

{"title":"Advanced Fabrication of Ultrathin Ruthenium Films Using Synergistic Atomic Layer Deposition and Etching.","authors":"Jeongbin Lee, Jung-Tae Kim, Jieun Oh, Dongjun Lee, Seo-Hyun Lee, Hyekyung Kim, Jiwoo Oh, Younseon Wang, Woo-Hee Kim","doi":"10.1002/smtd.202402166","DOIUrl":"https://doi.org/10.1002/smtd.202402166","url":null,"abstract":"Atomic-level surface preparation, using additive and subtractive atomic layer processes, has gradually become crucial for the more active process variations and highly selective process requirements. Precise control of surface roughness and coverage is a critical consideration in the fabrication of metal thin films. Herein, the fabrication of ultrathin, smooth Ru films with a thickness reduced to below 3 nm is reported. This process involves etching back after depositing a thick Ru film using a synergistic combination of atomic layer deposition (ALD) and atomic layer etching (ALE) techniques. The surface smoothing effect, while preserving surface coverage, is validated by initially performing the ALD process for Ru with (ethylbenzyl)(1-ethyl-1,4-cyclohexadienyl)Ru(0) precursor and O2 gas, followed by the ALE process with 2,4-pentanedione and O2 radicals. Under optimized conditions for atomically flat Ru surfaces, the surface quality of Ru films processed by ALD, and the combined ALD/ALE methods are compared. Consequently, it is demonstrated for the first time that the combined ALD/ALE process effectively reduces both thickness and asperities while smoothing the surface and maintaining nearly complete surface coverage down to the ≈1 nm scale. This approach enables the production of advanced electronic devices with precise control over surface properties at the Ångström level.","PeriodicalId":229,"journal":{"name":"Small Methods","volume":" ","pages":"e2402166"},"PeriodicalIF":10.7,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143672963","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A Fused Diketopyrrolopyrrole Derivative for Single-Crystal Visible-NIR Organic Phototransistor.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-21 DOI: 10.1002/smtd.202402250

Tianqiang Cui, Nan Luo, Zhilei Zhang, Jie Liu, Yanan Sun, Dawei Liu, Yamin Zhang, Xiangfeng Shao, Hao-Li Zhang, Lang Jiang, Zitong Liu

{"title":"A Fused Diketopyrrolopyrrole Derivative for Single-Crystal Visible-NIR Organic Phototransistor.","authors":"Tianqiang Cui, Nan Luo, Zhilei Zhang, Jie Liu, Yanan Sun, Dawei Liu, Yamin Zhang, Xiangfeng Shao, Hao-Li Zhang, Lang Jiang, Zitong Liu","doi":"10.1002/smtd.202402250","DOIUrl":"https://doi.org/10.1002/smtd.202402250","url":null,"abstract":"Organic phototransistors (OPTs) have garnered significant attention due to their potential in wearable and flexible electronics. However, achieving high carrier mobility and broadband response in organic semiconductors for OPTs remains a challenge. In this work, a new fused diketopyrrolopyrrole (FDPP) derivative is reported, 2,9-bis(4-hexylphenyl)-7H,14H-thieno[3',2':7,8]indolizino[2,1-a]thieno[3,2-g]indolizine-7,14-dione (FDPP-p-C6), synthesized through N-cyclization of DPP with an adjacent thiophene unit. This N-cyclization ensures backbone planarity, while the hexyl side chains remain distant from the fused core, minimizing steric hindrance and promoting efficient intermolecular stacking. Consequently, single crystals of FDPP-p-C6 exhibit a planar backbone and a typical herringbone packing arrangement, facilitating charge transport. The single-crystal organic field-effect transistors (OFETs) demonstrate p-type charge transport, achieving maximum mobility of 0.20 cm2 V-¹ s-¹. Additionally, the single-crystal OPTs show promising performance, with high responsivity across a broad spectral range and a photoresponsivity of 2.2 × 103 A W-¹ along with a specific detectivity, derived from the noise current, of 2.8 × 1010 Jones. This study highlights the potential of FDPP as a key material for advancing single-crystal OFET and OPT technologies, propelling relevant research forward.","PeriodicalId":229,"journal":{"name":"Small Methods","volume":" ","pages":"e2402250"},"PeriodicalIF":10.7,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143672942","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Oral Delivery Strategies for Biological Drugs.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-21 DOI: 10.1002/smtd.202401355

Huiling Zeng, Mingyang Ma, Xiuju Peng, Yangyang Xie, Angel Xie, Bo Deng, Jiang Ouyang, Wei Tao, Pei Yang, Wei He

{"title":"Oral Delivery Strategies for Biological Drugs.","authors":"Huiling Zeng, Mingyang Ma, Xiuju Peng, Yangyang Xie, Angel Xie, Bo Deng, Jiang Ouyang, Wei Tao, Pei Yang, Wei He","doi":"10.1002/smtd.202401355","DOIUrl":"https://doi.org/10.1002/smtd.202401355","url":null,"abstract":"Biologics have low toxicity and are highly specific and biocompatible, offering advantages over small-molecule drugs. The administration of biologics in oral form provides a significant benefit in improving patient compliance. However, oral administration faces the challenge of a harsh gastrointestinal environment, including low pH, enzyme degradation, and poor intestinal epithelium permeability, which limits the bioavailability of biologics. As a result, the administration of biologics remains primarily in the parenteral form. This review introduces the physiological barriers encountered by oral biologics delivery, describes the oral biologics currently on the market or under clinical trials, as well as oral biologics-based technologies, and discusses the recent progress on novel oral delivery technologies such as nanoparticle-delivery systems, ionic liquids, and microneedles. Specifically, colon-targeted approaches for oral biologics delivery are also explored, as the colon could be a more optimal absorption site due to having less diverse proteolytic enzymes and relatively limited digestibility compared to the upper gastrointestinal tract (GIT). Lastly, the future research directions for oral biologics are highlighted and it is concluded that with an in-depth study of biological drugs and advancement in delivery methods, oral biologics can pioneer new opportunities.","PeriodicalId":229,"journal":{"name":"Small Methods","volume":" ","pages":"e2401355"},"PeriodicalIF":10.7,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143668726","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

H-Embedding Induced Electron Localization in Pd Lattice for Improving Electrochemical Hydrogen Purification.

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-21 DOI: 10.1002/smtd.202500249

Xuanwei Yin, Cong Wei, Chongyang Tang, Zenan Bian, Bo Liu, Xinqiang Wang, Yaxiong Yang, Yanyan Fang, Hongge Pan, Gongming Wang

{"title":"H-Embedding Induced Electron Localization in Pd Lattice for Improving Electrochemical Hydrogen Purification.","authors":"Xuanwei Yin, Cong Wei, Chongyang Tang, Zenan Bian, Bo Liu, Xinqiang Wang, Yaxiong Yang, Yanyan Fang, Hongge Pan, Gongming Wang","doi":"10.1002/smtd.202500249","DOIUrl":"https://doi.org/10.1002/smtd.202500249","url":null,"abstract":"Electrochemical hydrogen purification (EHP) technology with high-efficiency and easy-operation holds great potential in blended hydrogen transportation, which is currently restricted to proton exchange membrane system and Pt-based catalysts. As promising candidates used in alkaline anion exchange membrane system, Pd-based catalysts are hampered by the intense interaction between H* and delocalized 4d electrons, resulting in unsatisfactory catalytic activity. In this study, a marked enhancement of the alkaline membrane-based EHP performance is achieved, with hydrogen purity up to 99.96% separated from a CH4-H2 mixture, by strategically incorporating interstitial H atoms into Pd lattices for improving the anodic hydrogen oxidation reaction. Detailed characterizations and density functional theory calculations elucidate that the presence of interstitial H localizes free electrons into Pd-H covalent bonds, thereby weakening the interaction between surface-adsorbed H* and the catalytic surface. Moreover, operando spectroscopies and ab initio molecular dynamic simulations reveal that the enhanced interaction between the catalyst surface and interfacial water by electron delocalization, facilitates the desorption of H* to the interfacial water layer during catalysis. This research highlights the pivotal role of electronic localization in modulating the adsorption strength of key reaction intermediates for the design of efficient Pd-based catalysts.","PeriodicalId":229,"journal":{"name":"Small Methods","volume":" ","pages":"e2500249"},"PeriodicalIF":10.7,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143668746","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Challenges and Opportunities of Uranium Extraction From Seawater: a Systematic Roadmap From Laboratory to Industry (Small Methods 3/2025)

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-20 DOI: 10.1002/smtd.202570020

Tao Wang, Binbin Tao, Bin Zuo, Guoze Yan, Shaoqing Liu, Ruoyu Wang, Zhongzhou Zhao, Feifei Chu, Zhengtong Li, Yusuke Yamauchi, Xingtao Xu

引用次数: 0

Strain-Engineered 2D Materials: Challenges, Opportunities, and Future Perspectives (Small Methods 3/2025)

IF 10.7 2区材料科学

Small Methods Pub Date : 2025-03-20 DOI: 10.1002/smtd.202570018

Ajit Kumar Katiyar, Jong-Hyun Ahn

引用次数: 0