Microwave-assisted synthesis of WS2 nanowires through tetrathiotungstate precursors

Abstract

Tungsten disulfide (WS₂) nanowires have been synthesized through a microwave-assisted chemical route that uses tungstic acid, elemental sulfur and monoethanolamine as starting reagents for obtaining a precursor solution of tetrathiotungstate ions. Acidification of the precursor solution yields amorphous precipitates, which lead to the formation of nanowires of WS₂ with thickness of about 5–10 nm when heated at 750 °C under argon atmosphere for 1.5 h. Phase and the microstructure of the prepared powders have been investigated through x-ray powder diffraction and high-resolution transmission electron microscopy, respectively. Optical absorption of the WS₂ powders reveals a red shift of the exciton bands compared to bulk WS₂.     

Enhanced Field Emission of WS2 Nanotubes

Results on electron field emission from free standing tungsten disulfide (WS₂) nanotubes (NTs) are presented. Experiments show that the NTs protruding on top of microstructures are efficient cold emitters with turn‐on fields as low as 1 V/μm and field enhancement of few thousands. Furthermore, the emission current shows remarkable stability over more than eighteen hours of continuous operation. Such performance and long‐term stability of the WS₂ cathodes is comparable to that reported for optimized carbon nanotube (CNTs) based emitters. Besides this, it is found that the WS₂ cathodes prepared are less sensitive than CNTs in chemical reactive ambients. The high field enhancement and superior reliability achieved indicates a potential for vacuum nanoelectronics and flat panel display applications.     

High Edge Selectivity of In Situ Electrochemical Pt Deposition on Edge‐Rich Layered WS2 Nanosheets

Recent studies show that the Pt electrode can be slowly dissolved into the acidic media and regenerate on the working electrode along with the long‐time hydrogen evolution reaction (HER) test. However, to date, the relationship between the Pt deposition and the intrinsic properties of the working electrode remains elusive. Herein, for the first time, the edge selectivity of in situ electrochemical Pt deposition on layered 2H‐WS₂ nanosheets, whose edge surface with rich dangling bonds is chemically active to regulate their properties, especially the interfacial reaction occurring between the electrode surface and the adjacent thin layer of the solution, is theoretically elucidated and experimentally verified by controlling the cathode polarization test using Pt wire as the counter electrode in H₂SO₄ solution. It is revealed that the layered WS₂ nanosheets with rich exposed edges show much stronger interaction with Pt atoms because the terminated S₂^2? or S^2? ligands on the edge exhibit much lower binding energy for Pt atoms compared with the apical S^2? ligands on the terrace surface. The in situ electrochemical Pt‐deposited WS₂ nanosheets with rich exposed edges can act as a highly active hybrid electrocatalyst to accelerate HER kinetics and exhibit commercial Pt‐like HER performance, especially in the alkaline media.     

Engineering Valley Polarization of Monolayer WS2: A Physical Doping Approach

The emerging field of valleytronics has boosted intensive interests in investigating and controlling valley polarized light emission of monolayer transition metal dichalcogenides (1L TMDs). However, so far, the effective control of valley polarization degree in monolayer TMDs semiconductors is mostly achieved at liquid helium cryogenic temperature (4.2 K), with the requirements of high magnetic field and on‐resonance laser, which are of high cost and unwelcome for applications. To overcome this obstacle, it is depicted that by electrostatic and optical doping, even at temperatures far above liquid helium cryogenic temperature (80 K) and under off‐resonance laser excitation, a competitive valley polarization degree of monolayer WS₂ can be achieved (more than threefold enhancement). The enhanced polarization is understood by a general doping dependent valley relaxation mechanism, which agrees well with the unified theory of carrier screening effects on intervalley scattering process. These results demonstrate that the tunability corresponds to an effective magnet field of ≈10 T at 4.2 K. This work not only serves as a reference to future valleytronic studies based on monolayer TMDs with various external or native carrier densities, but also provides an alternative approach toward enhanced polarization degree, which denotes an essential step toward practical valleytronic applications.     

Nitrogen-doped tungsten oxide nanowires: low-temperature synthesis on Si, and electrical, optical, and field-emission properties

Very dense and uniformly distributed nitrogen-doped tungsten oxide (WO(3)) nanowires were synthesized successfully on a 4-inch Si(100) wafer at low temperature. The nanowires were of lengths extending up to 5 mum and diameters ranging from 25 to 35 nm. The highest aspect ratio was estimated to be about 200. An emission peak at 470 nm was found by photoluminescence measurement at room temperature. The suggested growth mechanism of the nanowires is vapor-solid growth, in which gaseous ammonia plays a significant role to reduce the formation temperature. The approach has proved to be a reliable way to produce nitrogen-doped WO(3) nanowires on Si in large quantities. The direct fabrication of WO(3)-based nanodevices on Si has been demonstrated.     

氧化钨纳米线敏感膜对CO气体的气敏性能

采用丝网印刷法制备了氧化钨纳米线敏感膜,系统研究了不同热处理温度下敏感膜的结构、形貌以及对CO气体的气敏性能.结果表明,氧化钨纳米线敏感膜具有较高的结构稳定性,经450℃热处理后其结晶取向和结构均未发生变化;热处理温度的升高有助于提高敏感膜的晶化程度,同时导致其表面的氧化钨纳米棒逐渐变短、变粗直至消失,并最终形成较大的纳米颗粒;经300℃热处理的敏感膜在300℃时对1×10 叫CO气体具有最佳的气敏性能,其灵敏度为17.64,响应时间为8s,恢复时间为16s.     

氨化Ga2O3/Nb薄膜制备GaN纳米线

采用射频磁控溅射技术先在硅衬底上制备Ga2O3/ Nb薄膜,然后在900℃时于流动的氨气中进行氨化制备GaN纳米线.用X射线衍射(XRD)、傅立叶红外吸收光谱(FTIR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)详细分析了GaN纳米线的结构和形貌.结果表明:采用此方法得到的GaN纳米线为六方纤锌矿结构,其纳米线的直径大约在50～100nm之间,纳米线的长约几个微米.室温下以325nm波长的光激发样品表面,只显示出一个位于364.4nm的很强的紫外发光峰.最后,简单讨论了GaN纳米线的生长机制.     

Monolayer Tungsten Disulfide (WS2) via Chlorine‐Driven Chemical Vapor Transport

Large‐scale production of high‐quality tungsten disulfide (WS₂) monolayers is a prerequisite for potential device applications using this promising transition metal dichalcogenide semiconductor. The most researched technique is chemical vapor deposition, typically involving the reaction of sulfur vapors with tungsten oxide. Other techniques such as physical vapor deposition have been explored with some success, but low vapor pressures make growth difficult. This study demonstrates a growth process that relies on halide‐driven vapor transport commonly utilized in bulk crystal growth. Using a small amount of sodium chloride salt as a source of chlorine, nonvolatile WS₂ can react to form gaseous tungsten chloride and sulfur. With an open tube system, a controlled reaction generates mono and few‐layer WS₂ crystals. Optical and physical characterization of the monolayer material shows good uniformity and triangular domains over 50 µm in length. Photoluminescence transient measurements show similar nonlinear exciton dynamics as exfoliated flakes, attributed to multiparticle physics. Requiring only the powder of the desired crystal and appropriate halide salt as precursors, the technique has the potential to realize other layered materials that are challenging to grow with current processes.     

Template-free synthesis of nickel nanowires by magnetic field

Nickel nanowires were prepared by a template free method combined with chemical reduction and magnetic field. The application of an external magnetic field resulted in the formation of self-aligned metallic nickel nanowires of about 50 nm in diameter. Nickel particles were prepared in the absence of a magnetic field to better illustrate the structure directing role of the magnetic field. Physical properties of the nickel nanochains were examined by scanning electron microscopy (SEM), transmission electron microscope (TEM), X-Ray diffraction (XRD), and thermogravimetric analysis (TGA) methods. This study provides a simple method to prepare Ni nanowires in large scale which broads their practical applications.     

One-pot synthesis of ultranarrow single crystal ZnSe nanowires

High-quality wurtzite-type ultranarrow single crystal ZnSe nanowires were synthesized via a one-pot, solution-based method for the first time. The as-prepared nanowires have diameters ranging from 1.0 nm to 3.5 nm and lengths up to 300 nm. The optical characterizations indicate that the as-synthesized ZnSe nanowires have a band gap of 3.31 eV, whose absorbance spectra are different from recent literatures. Both the quantum confinement and the vacancies of Zn in ZnSe or impurities were accounted for the phenomenon. The solvent employed in the synthesis is also playing a dominant role in the size and morphology control of the ZnSe nanowires. A reasonable mechanism was proposed to describe the function of solvent. The excellent properties of the ZnSe nanowires would render it a promising alternative functional material which might be widely used in short-wavelength lasers and other photoelectronic devices.     

Synthesis and characterisation of selenium nanowires using template synthesis

Selenium (Se) nanowires were grown in the pores of anodic alumina membrane as template. Facile electrodeposition technique was used for the synthesis of Se nanowires. Scanning electron microscopy was used for the morphological study of the nanowires. X-ray diffraction and Energy dispersive X-ray fluorescence were utilised for the structural characterisation. The optical properties of Se nanowires were investigated using optical absorption spectroscopy.     

Improved Photo-Excited Carriers Transportation of WS2-O-Doped-Graphene Heterostructures for Solar Steam Generation (Small 19/2023)

Two-dimensional (2D) transition metal dichalcogenides and graphene have revealed promising applications in optoelectronic and energy storage and conversion. However, there are rare reports of modifying the light-to-heat transformation via preparing their heterostructures for solar steam generation. In this work, commercial WS₂ and sucrose are utilized as precursors to produce 2D WS₂-O-doped-graphene heterostructures (WS₂-O-graphene) for solar water evaporation. The WS₂-O-graphene evaporators demonstrate excellent average water evaporation rate (2.11 kg m⁻² h⁻¹) and energy efficiency (82.2%), which are 1.3- and 1.2-fold higher than WS₂ and O-doped graphene-based evaporators, respectively. Furthermore, for the real seawater with different pH values (pH 1 and 12) and rhodamine B pollutants, the WS₂-O-graphene evaporators show great average evaporation rates (≈2.08 and 2.09 kg m⁻² h⁻¹, respectively) for producing freshwater with an extremely low-grade of dye residual and nearly neutral pH values. More interestingly, due to the self-storage water ability of WS₂-O-graphene evaporators, water evaporation can be implemented without the presence of bulk water. As a result, the evaporation rate reaches 3.23 kg m⁻² h⁻¹, which is ≈1.5 times higher than the regular solar water evaporation system. This work provides a new approach for preparing 2D transition metal dichalcogenides and graphene heterostructures for efficient solar water evaporation.     

二氧化锡纳米线的生长机理研究

使用水平石英管式电炉，以二氧化锡和石墨的混合物为原材料、高纯氮气为载气，在850℃温度下用直接热蒸发法制备二氧化锡纳米线．衬底硅片的直径为10mm，其上覆盖一层5nm厚的金催化剂．原材料放在石英舟中，离原材料30mm的下风口处放置硅衬底，原材料和硅衬底都放置在石英管的中部电炉的恒温区内．用扫描电子显微镜（SEM）和透射电子显微镜（TEM）观察到二氧化锡的纳米线结构；X射线衍射（XRD）表明二氧化锡纳米线具有四方金红石结构；选区电子衍射（SAED）照片表明二氧化锡纳米线具有完善的晶体结构．不同生长时间下制备样品的扫描电子显微镜和透射电子显微镜照片再现了二氧化锡纳米线的生长过程，该纳米线的生长符合传统的VLS生长机制．