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Signal enhancement in laser diode thermal desorption-triple quadrupole mass spectrometry analysis using microwell surface coatings
摘要: Laser diode thermal desorption (LDTD) is an ionization source usually coupled to triple quadrupole mass spectrometry (QqQMS) and specifically designed for laboratories requiring high-throughput analysis. It has been observed that surface coatings on LDTD microwell plates can improve the sensitivity of the analysis of small polar molecules. The objective of the present study is to understand and quantify the effect of microwell surface coatings on signal intensity of small organic molecules of clinical, environmental and forensic interest. Experiments showed that the peak areas of diclofenac, chloramphenicol, salicylic acid and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol obtained by LDTD-QqQMS increased by up to 3 orders of magnitude when using microwells coated with ethylenediaminetetraacetic acid (EDTA). Tests with different chelating agents and polytetrafluoroethylene as microwell surface coatings showed that nitrilotriacetic acid gave significantly higher peak areas for five out of the nine compounds that showed signal enhancement using chelating agents as coatings. Scanning electron microscopy studies of EDTA-coated and uncoated microwells showed that analytes deposited in the former formed more uniform and thinner films than in the latter. The enhancement effect of surface coatings in LDTD-QqQMS was explained mainly by the formation of homogenous and thinner layers of nanocrystals of analytes that are easier to desorb thermally than the layers formed when the analytes dry in direct contact with the bare stainless steel surface. Chemisorption of some analytes to the stainless steel surface of the microwell plate appeared to be a minor factor. Surface coatings widen the number of compounds analyzable by LDTD-QqQMS and can also improve sensitivity and limits of detection.
关键词: pharmaceuticals,high-throughput,hormones,pesticides,x-ray photoelectron spectroscopy,scanning electron microscopy,stainless steel,small organic molecules,chelating agents
更新于2025-09-23 15:23:52
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RGB color coded images in scanning electron microscopy of biological surfaces
摘要: We present here a methodological approach for the creation of color images in scanning electron microscopy by processing grayscale images taken simultaneously from at least three different detectors in a scanning electron microscope. The final color images are then produced by merging together those grayscale images in RGB color space. We show the images from non-conductive standard sample together with those obtained from real microbiological samples. The first one represents a microbial biofilm naturally grown on fiber glass filter. The other shows individual Bacillus subtilis cells from batch culture. All the image handling was done in open source image processing software ImageJ or GNU Image Manipulation Program (Gimp) or, alternatively, in proprietary AnalySis 3.2 Pro software processing suite.
关键词: high resolution,color images,scanning electron microscopy,biological surfaces
更新于2025-09-23 15:22:29
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A comparison of the morphological and electrical properties of sol-gel dip coating and atomic layer deposition of ZnO on 3D nanospring mats
摘要: We report on the morphological and electrical properties, with (light) and without (dark) UV illumination, of conformal coatings of ZnO on silica nanosprings deposited by sol-gel and atomic layer deposition (ALD) for the first time. Field Emission Scanning Electron Microscopy (FESEM) imaging showed that both methods produce conformal coatings of ZnO on the nanosprings. The surface of the sol-gel coatings exhibited cracks at higher numbers of dipping/sintering cycles, while the morphology of ALD ZnO films were always smooth and devoid of cracks. The effective photoconductivity of the sol-gel ZnO coated nanospring mats increased nonlinearly with increasing coating thickness. The corresponding dark effective conductivity of the sol-gel ZnO coated nanospring mats also increased within the same thickness range. Alternatively, the effective photoconductivity of the ALD ZnO coated nanospring mats increased linearly with increasing coating thickness. The corresponding dark effective conductivity also increased within the same thickness range. The superior effective conductivity and photoconductivity of the ALD ZnO coated nanospring mats is attributed to the uniformity of the coating and the absence of cracks, which are observed for the thicker sol-gel ZnO coatings.
关键词: atomic layer deposition (ALD),semiconductors,sol-gel,nanosprings,field emission scanning electron microscopy,conductivity,ZnO
更新于2025-09-23 15:22:29
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Role of microstructure and structural disorder on tribological properties of polycrystalline diamond films
摘要: Polycrystalline diamond films with systematic change in microstructure that varies from microcrystalline to nanocrystalline structure are synthesized on Si by hot filament chemical vapor deposition. The morphology and structural properties of the grown diamond films are analyzed using field emission scanning electron microscope (FESEM), atomic force microscope (AFM), X-ray diffraction and Raman spectroscopy. The average roughness and grain size of the diamond films decrease with increase in CH4 to H2 ratio from 0.5 to 3%. Also, structural disorder in these diamond films increases with decrease in grain size as evidenced from Raman spectroscopy. The coefficient of friction (CoF) is found to be very low for all the films. However, the average CoF is found to increase from 0.011 ± 0.005 to 0.03 ± 0.015 as the grain size decrease from ~1 μm down to ~20 nm. Post analysis of wear track by FESEM, AFM based nanoscale friction and Raman spectroscopy reveal that microcrystalline diamond undergoes shear induced amorphization with negligible wear rate while nanocrystalline diamond films undergo shear induced plastic deformation without amorphization. A comprehensive mechanism for the observed CoF is discussed in the framework of microstructure, structural disorder and shear induced tribo-chemical reactions at the sliding interface.
关键词: Raman spectroscopy,Tribology,Diamond,Scanning electron microscopy,Hot filament CVD,Atomic force microscopy
更新于2025-09-23 15:21:01
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Thulium fiber laser: ready to dust all urinary stone composition types?
摘要: Purpose To evaluate whether stone dust can be obtained from all prevailing stone composition types using the thulium fiber laser (TFL) for lithotripsy. Where applicable, stone dust was further characterized by morpho-constitutional analysis. Methods Human urinary stones were submitted to in vitro lithotripsy using a FiberLase U2 TFL generator with 150 μm silica core fibers (IPG Photonics?, IPG Medical?, Marlborough, MA, USA). Laser settings were 0.05 J, 320 Hz and 200 μs. A total of 2400 J were delivered to each stone composition type. All evaluated stones had a > 90% degree of purity (calcium oxalate monohydrate, calcium oxalate dihydrate, uric acid, carbapatite, struvite, brushite and cystine). Spontaneously floating stone particles were considered as stone dust and collected for analysis by scanning electron microscopy and Fourier transform infrared spectroscopy. Results Stone dust could be retrieved from all evaluated urinary stones after TFL lithotripsy. Most stone dust samples revealed changes in crystalline organization, except for calcium oxalate monohydrate and carbapatite, which conserved their initial characteristics. Mean maximal width of stone dust particles did not exceed 254 μm. Conclusions The TFL is capable to produce stone dust from all prevailing stone types. Morpho-constitutional changes found in stone dust suggest a photothermal interaction of laser energy with the stone matrix during TFL lithotripsy.
关键词: Urolithiasis,Stone dust,Fourier transform infrared spectroscopy,Lithotripsy,Scanning electron microscopy,Thulium fiber laser
更新于2025-09-23 15:21:01
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Spectroscopic Studies of M??ssbauer, Infrared, and Laser-Induced Luminescence for Classifying Rare-Earth Minerals Enriched in Iron-Rich Deposits
摘要: Rare-earth (RE) phosphates often appear as an accessory phase in igneous or metamorphic rocks; however, these rocks are composed of myriad chemical elements and nuclides that interfere with the qualitative or quantitative analyses of the RE phosphates over a range of concentrations in the absence of a pretreatment. In addition, the limit of each analytical methodology constrains the approach as well as the usefulness of the results in geoscience applications. Here, we report the specific mineral characterization of RE-containing ores from Yen Phu mine, Vietnam, using a range of state-of-the-art spectroscopic techniques in conjunction with microscopy: M?ssbauer spectroscopy, infrared microspectroscopy, time-resolved laser-induced fluorescence spectroscopy (TRLFS), and scanning electron microscopy with energy-dispersive X-ray spectroscopy. Because the distribution of each element in the deposit differs, such combinatorial works are necessary and could lead to more plausible answers to questions surrounding the point of origin of RE elements. The results of our M?ssbauer spectroscopic analysis indicate that the three ores sampled at different locations all contain magnetite-like, hematite-like, and iron(III) salts other than hematite. In addition, we confirmed the presence of phosphate around the grain boundary in the magnetite-like mineral phase by infrared microspectroscopic analysis. The present analytical findings of trace amounts of europium(III) using TRLFS suggest that the europium ions generate identical luminescence spectra despite being embedded in three different matrices of iron minerals. This demonstration highlights the benefits of combinatorial spectroscopic analyses to gain insights into the effects of the environment of REs on their solid-state chemistry and shows the potential utility of TRLFS as a resource mining tool. Further applications of this approach in the analytical screening of rocks and minerals are feasible.
关键词: energy-dispersive X-ray spectroscopy,spectroscopic techniques,rare-earth phosphates,Yen Phu mine,infrared microspectroscopy,scanning electron microscopy,time-resolved laser-induced fluorescence spectroscopy,M?ssbauer spectroscopy,Vietnam
更新于2025-09-23 15:21:01
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Morphology and magnetic properties of grain-oriented steel scribed using different picosecond lasers
摘要: Micro-scribing experiments were conducted to investigate the characteristics of the associated ablative behavior and the improvements to the magnetic properties of grain-oriented steel using both a 532 nm and a 1064 nm wavelength ultra-fast picosecond laser. Ablative morphological characteristic analysis and elemental analysis were carried out using a 3D confocal microscope, a scanning electron microscope, and energy-dispersive spectroscopy. The damage mechanisms were analyzed by comparing the ablation morphologies. Furthermore, an iron loss tester and magnetic domain observation instrument were used to analyze the dynamic hysteresis loop, macroscopic magnetic property parameters, and to observe the microscopic structure of the magnetic domains. The magnetization behavior, loop characteristics, and magnetic domain refinement mechanisms were discussed. The results indicated that the magnetic domains were clearly refined and that the magnetic properties were significantly improved after picosecond laser scribing of the grain-oriented steel. The sample scribed using an ultra-fast wavelength 532 nm laser was more effectively scribed: the magnetic domain was slightly more refined, the iron loss was reduced by 15.73%, the coercivity was reduced by 24.42%, the residual magnetism was reduced by 20.8%, and the relative permeability was increased by 10.3%. The surface was of a high quality, but there were traces of stress damage caused by high-pressure steam in the scribed area. The 1064 nm wavelength ultra-fast laser clearly showed the effects of heat accumulation in the scribed area. Defects due to thermal damage were more common. The improvement to the macroscopic magnetic properties depended largely on the surface quality of the scribing and the penetration depth of the residual stress in the sample.
关键词: Magnetic domains,Laser surface treatment,Scanning electron microscopy,Iron core loss,Magnetic properties,Grain-oriented silicon steel
更新于2025-09-23 15:21:01
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Application of Nanostructured Tungsten Fabricated by Helium Plasma Irradiation for Photoinduced Decolorization of Methylene Blue
摘要: The dendritic nanostructure was fabricated on a surface of tungsten plate by helium plasma irradiation. The nanostructure consisting of W metal was partially oxidized to form WO3 on exposure to air, and the resulting surface exhibited a broad photoabsorption in the range from 1 to 5 eV. We examined photoinduced reaction of methylene blue (MB) on the material. It was found that the partially and fully oxidized surface nanostructures were able to promote a decolorization of MB under photoirradiation even with the near-infrared light (< 1:55 eV), whose energy is lower than the band gap of WO3. The reaction rate was varied with the fraction of W and WO3 on the surface layers, that is, the partially oxidized sample promoted the reaction at a higher rate than the fully oxidized one. It is also found that the reaction rate decreased with time, which would be caused by the products accumulation on the surface and the surface oxidation.
关键词: Scanning electron microscopy (SEM),Tungsten oxide,Surface photochemistry,Plasma processing,Nano-wires, quantum wires, and nanotubes,Visible/ultraviolet absorption spectroscopy, X-ray photoelectron spectroscopy
更新于2025-09-23 15:21:01
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Applying Fast Scanning Method Coupled with Digital Image Processing Technology as Standard Acquisition Mode for Scanning Electron Microscopy
摘要: This study proposes an e?cient and fast method of scanning (e.g., television (TV) scan) coupled with digital image processing technology to replace the conventional slow-scan mode as a standard model of acquisition for general-purpose scanning electron microscopy (SEM). SEM images obtained using the proposed method had the same quality in terms of sharpness and noise as slow-scan images, and it was able to suppress the adverse e?ects of charging in a full-vacuum condition, which is a challenging problem in this area. Two problems needed to be solved in designing the proposed method. One was suitable compensation in image quality using the inverse ?lter based on characteristics of the frequency of a TV-scan image, and the other to devise an accurate technique of image integration (noise suppression), the position alignment of which is robust against noise. This involved using the image montage technique and estimating the number of images needed for the integration. The ?nal result of our TV-scan mode was compared with the slow-scan image as well as the conventional TV-scan image.
关键词: image integration,inverse filter,TV scan,charging effects,scanning electron microscopy,fast scanning method,digital image processing,slow-scan mode
更新于2025-09-23 15:19:57
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Controlled deposition of size-selected metal nanoclusters on prepatterned substrate
摘要: An endeavor of organizing Cu nano-particles of controlled size in ordered arrays at room temperature is reported. This involves the guided deposition of size-selected nanoparticles otherwise known as nanoclusters via periodic modulation of the substrate surface. Ultra-high vacuum compatible magnetron-based gas-aggregation type source combined with a quadrupole mass filter has been employed to produce the size-selected nanoclusters whereas the surface modulations (ripples) in the nanoscale are induced by low energy oblique angle ion beam irradiation. Morphological aspects of deposited nanoclusters and the substrates were characterized by high-resolution scanning electron microscopy (HRSEM) and atomic force microscopy (AFM). The chemical composition of the deposited nanoclusters was characterized by x-ray photoelectron spectroscopy. The alignment of size-selected metal nanoclusters along the substrate-patterns is observed. Depending upon deposition conditions quality of the organization varies. The optimum angle of deposition for the improved alignment depends on the pattern parameters of the substrate.
关键词: Ion sputtering,Room-temperature organization,Metal nanocluster,Patterned substrate,Supported clusters,Scanning Electron Microscopy
更新于2025-09-23 15:19:57