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Sample preparation for scanning electron microscopy

Reinhard Wagner, Daniel Rettenwander, Günther J Redhammer, Gerold Tippelt, Gebhard Sabathi, Maurizio E Musso, Bernhard Stanje, Martin Wilkening, Emmanuelle Suard, Georg Amthauer
Li oxide garnets are among the most promising candidates for solid-state electrolytes in novel Li ion and Li metal based battery concepts. Cubic Li7La3Zr2O12 stabilized by a partial substitution of Zr(4+) by Bi(5+) has not been the focus of research yet, despite the fact that Bi(5+) would be a cost-effective alternative to other stabilizing cations such as Nb(5+) and Ta(5+). In this study, Li7-xLa3Zr2-xBixO12 (x = 0.10, 0.20, ..., 1.00) was prepared by a low-temperature solid-state synthesis route. The samples have been characterized by a rich portfolio of techniques, including scanning electron microscopy, X-ray powder diffraction, neutron powder diffraction, Raman spectroscopy, and (7)Li NMR spectroscopy...
December 5, 2016: Inorganic Chemistry
Ying Cai, Zhihong Yan, Ming Yang, Xiaoying Huang, Weiping Min, Lijia Wang, Qingyun Cai
In this work, polydopamine coated 3D nickel foam (NF-PDA) was prepared and applied as sorbent for the solid phase extraction (SPE) of 16 polycyclic aromatic hydrocarbons (PAHs) from water samples. NF-PDA were synthesized by situ oxidative self-polymerization procedure and characterized by using the techniques of scanning electron microscopy (SEM), energy dispersive spectrum analysis (EDS) and X-ray photoelectron spectroscopy (XPS). Its performance was evaluated by the SPE of 16 PAHs from water samples, followed by gas chromatography-mass spectrometrical (GC-MS) analysis...
November 21, 2016: Journal of Chromatography. A
Sakine Tuncay Tanrıverdi, Catalina Natalia Cheaburu-Yilmaz, Sonia Carbone, Özgen Özer
Melatonin loaded hyaluronic acid and poly(vinyl alcohol) gels were prepared by using freeze-thaw technique and an emulsion method followed by freeze-thaw technique to produce a new synergistic system for topical application. Freeze-thaw hydrogels and emulgels were characterized by means of Fourier Transform Infrared Spectroscopy, rheology and swelling tests. The porous structure of the hydrogels was shown by scanning electron microscopy observations and thermal properties were tested by Differential Scanning Calorimetry measurements...
December 5, 2016: Pharmaceutical Development and Technology
Youwei Yu, Zhefeng Fan
An efficient magnetic sorbent consisting of benzofuran-2-carboxylic acid-loaded magnetic nanocomposite was successfully synthesized for preconcentration of patulin from apple juice. The prepared magnetic nanocomposite was characterized by scanning electron microscopy, transmission electron microscopy, and Fourier transform-infrared spectroscopy. Determination of enriched patulin was performed by HPLC. The best adsorption conditions were 40 mg of sorbent, 50 mL of apple juice sample, pH 5, ambient temperature and 25 min; the elution conditions were 500 μL methanol, pH 5, ambient temperature, and 4 min...
November 30, 2016: Food Additives & Contaminants. Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment
Hasan Bagheri, Ali Hajian, Mosayeb Rezaei, Ali Shirzadmehr
In the present research, we aimed to fabricate a novel electrochemical sensor based on Cu metal nanoparticles on the multiwall carbon nanotubes-reduced graphene oxide nanosheets (Cu/MWCNT/RGO) for individual and simultaneous determination of nitrite and nitrate ions. The morphology of the prepared nanocomposite on the surface of glassy carbon electrode (GCE) was characterized using various methods including scanning electron microscopy (SEM), atomic force microscopy (AFM), and electrochemical impedance spectroscopy...
November 21, 2016: Journal of Hazardous Materials
J Ofner, J Kirschner, E Eitenberger, G Friedbacher, A Kasper-Giebl, H Lohninger, C Eisenmenger-Sittner, B Lendl
The quality of chemical imaging, especially multisensor hyperspectral imaging, strongly depends on sample preparation techniques and instrumental infrastructure but also on the choice of an appropriate imaging substrate. To optimize the combined imaging of Raman microspectroscopy, scanning-electron microscopy and energy-dispersive X-ray spectroscopy, a novel substrate was developed based on sputtering of highly purified aluminium onto classical microscope slides. The novel aluminium substrate overcomes several disadvantages of classical substrates like impurities of the substrate material and contamination of the surface as well as surface roughness and homogeneity...
November 28, 2016: Journal of Microscopy
Márcia Helena Wagner, Ricardo Abreu da Rosa, José Antonio Poli de Figueiredo, Marco Antonio Húngaro Duarte, Jefferson Ricardo Pereira, Marcus Vinicius Reis Só
OBJECTIVES: The aim of this study was to evaluate the effect of different irrigation protocols on the root dentin structure using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). MATERIALS AND METHODS: Thirty-nine lower bovine incisors were hemisected longitudinally and randomly divided into 13 groups (n = 3). After the root halves were reassembled, it was applied a specific irrigation protocol for each group, as following: G1, distilled water (control); G2, 0...
November 25, 2016: Clinical Oral Investigations
Louise Helene Søgaard Jensen, Lars Michael Skjolding, Amalie Thit, Sara Nørgaard Sørensen, Carsten Købler, Kristian Mølhave, Anders Baun
Increasing use of engineered nanoparticles has led to extensive research into their potential hazards to the environment and human health. Cellular uptake from the gut is sparsely investigated and microscopy techniques applied for uptake studies can result in misinterpretations. Various microscopy techniques are used to investigate internalization of 10 nm gold nanoparticles in Daphnia magna gut lumen and gut epithelial cells upon 24h exposure and outline potential artefacts, i.e. high contract precipitates from sample preparation related to these techniques...
November 25, 2016: Environmental Toxicology and Chemistry
N Vyas, R L Sammons, Z Pikramenou, W M Palin, H Dehghani, A D Walmsley
OBJECTIVES: Functionalised silica sub-micron particles are being investigated as a method of delivering antimicrobials and remineralisation agents into dentinal tubules. However, their methods of application are not optimised, resulting in shallow penetration and aggregation. The aim of this study is to investigate the impact of cavitation occurring around ultrasonic scalers for enhancing particle penetration into dentinal tubules. METHODS: Dentine slices were prepared from premolar teeth...
November 21, 2016: Journal of Dentistry
Anupam Srivastav, Anuradha Verma, Anamika Banerjee, Saif A Khan, Mukul Gupta, Vibha Rani Satsangi, Rohit Shrivastav, Sahab Dass
The present study investigates the effect of gradient doping on modifying the photoelectrochemical response of Ti-doped Fe2O3 photoanodes for their use in sunlight based water splitting for hydrogen evolution. The deposition of a thin film over the ITO (tin doped indium oxide) substrate was carried out using a spray pyrolysis method. The concentration of dopant was varied from 0.5-8.0 at% and two sets of samples were also prepared with low to high (0.5-8%) and high to low (8-0.5%) dopant concentrations in the direction towards the substrate...
November 23, 2016: Physical Chemistry Chemical Physics: PCCP
Maria T Fabbro, Carla Saliby, Larissa R Rios, Felipe A La Porta, Lourdes Gracia, Máximo S Li, Juan Andrés, Luís P S Santos, Elson Longo
We present a combined theoretical and experimental study on the morphological, structural, and optical properties of β-Ag2MoO4 microcrystals. β-Ag2MoO4 samples were prepared by a co-precipitation method. The nucleation and formation of Ag nanoparticles on β-Ag2MoO4 during electron beam irradiation were also analyzed as a function of electron beam dose. These events were directly monitored in real-time using in situ field emission scanning electron microscopy (FE-SEM). The thermodynamic equilibrium shape of the β-Ag2MoO4 crystals was built with low-index surfaces (001), (011), and (111) through a Wulff construction...
December 2015: Science and Technology of Advanced Materials
K Ogawa, H Miyaji, A Kato, Y Kosen, T Momose, T Yoshida, E Nishida, S Miyata, S Murakami, H Takita, B Fugetsu, T Sugaya, M Kawanami
BACKGROUND AND OBJECTIVE: Nanoparticle bioceramics are being investigated for biomedical applications. We fabricated a regenerative scaffold comprising type I collagen and beta-tricalcium phosphate (β-TCP) nanoparticles. Fibroblast growth factor-2 (FGF-2) is a bioeffective signaling molecule that stimulates cell proliferation and wound healing. This study examined the effects, on bioactivity, of a nano-β-TCP/collagen scaffold loaded with FGF-2, particularly on periodontal tissue wound healing...
December 2016: Journal of Periodontal Research
Michael J Zachman, Emily Asenath-Smith, Lara A Estroff, Lena F Kourkoutis
Scanning transmission electron microscopy (STEM) allows atomic scale characterization of solid-solid interfaces, but has seen limited applications to solid-liquid interfaces due to the volatility of liquids in the microscope vacuum. Although cryo-electron microscopy is routinely used to characterize hydrated samples stabilized by rapid freezing, sample thinning is required to access the internal interfaces of thicker specimens. Here, we adapt cryo-focused ion beam (FIB) "lift-out," a technique recently developed for biological specimens, to prepare intact internal solid-liquid interfaces for high-resolution structural and chemical analysis by cryo-STEM...
November 21, 2016: Microscopy and Microanalysis
Li Cui, E Sune, Jie Song, Jing Wang, Xiao-Bin Jia, Zhen-Hai Zhang
BACKGROUND: Baicalin is the main bioactive constitute of the dried roots of Scutellaria baicalensis and possesses various biological activities. However, the poor water solubility and low oral bioavailability limit its efficacy. OBJECTIVE: The present study was conducted to enhance the dissolution and oral bioavailability of baicalin (BA) through a novel mesoporous carbon nanopowder (MCN) drug carrier. MATERIALS AND METHODS: Solid dispersions (SDs) of BA with MCN were prepared using a solvent evaporation method...
October 2016: Pharmacognosy Magazine
Thomas Später, Florian S Frueh, Wolfgang Metzger, Michael D Menger, Matthias W Laschke
Integra(®) matrix wound dressing (MWD) is used for the reconstruction of full-thickness skin defects. For the treatment of complex wounds, this dermal substitute is available as a flowable wound matrix (FWM) of identical composition. To clarify whether variations in sample preparation and consistency affect the biocompatibility and tissue incorporation, we herein compared MWD and FWM. The matrices were characterized using scanning electron microscopy and histology. Moreover, they were implanted in mouse dorsal skinfold chambers to analyze their in vivo performance over 2 weeks...
November 14, 2016: Journal of Biomedical Materials Research. Part B, Applied Biomaterials
Qurrat-Ul-Ain Baloach, Aneela Tahira, Arfana Begum Mallah, Muhammad Ishaq Abro, Siraj Uddin, Magnus Willander, Zafar Hussain Ibupoto
The production of a nanomaterial with enhanced and desirable electrocatalytic properties is of prime importance, and the commercialization of devices containing these materials is a challenging task. In this study, unique cupric oxide (CuO) nanostructures were synthesized using lysine as a soft template for the evolution of morphology via a rapid and boiled hydrothermal method. The morphology and structure of the synthesized CuO nanomaterial were characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively...
November 14, 2016: Sensors
Muhammad Sajid, Chanbasha Basheer, Muhammad Mansha
In this work, zinc oxide nanoparticles incorporated carbon foam was utilized as sorbent for extraction and preconcentration of fifteen organochlorine pesticides in milk samples. The sorbent was prepared by a fast and single step reaction between the sucrose and zinc nitrate that was accomplished by heating the mixture for 10min. The resulting sorbent was characterized by scanning electron microscopy and X-ray diffraction. The sorbent was then employed in membrane protected micro-solid-phase extraction (μ-SPE) of OCPs in milk samples...
December 2, 2016: Journal of Chromatography. A
Ali Maleki, Hamed Movahed, Parisa Ravaghi
In this work, design, preparation and performance of magnetic cellulose/Ag nanobiocomposite as a recyclable and highly efficient heterogeneous nanocatalyst is described. Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) pattern, vibrating sample magnetometer (VSM) curve, field-emission scanning electron microscopy (FE-SEM) image, energy dispersive X-ray (EDX) analysis and thermogravimetric analysis/differential thermal analysis (TGA/DTA) were used for the characterization. Then, its activity was investigated in the synthesis of 2-amino-6-(2-oxo-2H-chromen-3-yl)-4-phenylnicotinonitrile derivatives...
January 20, 2017: Carbohydrate Polymers
Yvonne Perrie, Habib Ali, Daniel J Kirby, Afzal U R Mohammed, Sarah E McNeil, Anil Vangala
The structural characteristics of liposomes have been widely investigated and there is certainly a strong understanding of their morphological characteristics. Imaging of these systems, using techniques such as freeze-fracturing methods, transmission electron microscopy, and cryo-electron imaging, has allowed us to appreciate their bilayer structures and factors which can influence this. However, there are few methods which all us to study these systems in their natural hydrated state; commonly the liposomes are visualized after drying, staining, and/or fixation of the vesicles...
2017: Methods in Molecular Biology
Na Li, Fenglian Fu, Jianwei Lu, Zecong Ding, Bing Tang, Jiabin Pang
Chromium-contaminated water is regarded as one of the biggest threats to human health. In this study, a novel magnetic mesoporous MnFe2O4@SiO2-CTAB composite was prepared by a facile one-step modification method and applied to remove Cr(VI). X-ray diffraction, scanning electron microscopy, transmission electron microscopy, specific surface area, and vibrating sample magnetometer were used to characterize MnFe2O4@SiO2-CTAB composites. The morphology analysis showed that the composites displayed a core-shell structure...
January 2017: Environmental Pollution
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