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1.
《Advanced Powder Technology》2020,31(5):2072-2078
This work is aimed to identify the structure of the graphene-based particles (GPs) from old coconut shell as the raw material after the mechanical exfoliation processes. The burnt coconut shell was at first heated at 400 °C for 5 h in ambient air. The sample was then stirred in an acid solution (HCl) and then continued by ultrasonication and centrifugation. The exfoliated GPs were characterized by x-ray diffraction (XRD), particle size analyzer (PSA), Fourier-transform infrared spectroscopy (FTIR), scanning and transmission electron microscopy (SEM and TEM, respectively), atomic force microscopy (AFM), Raman spectroscopy, and synchrotron wide and small angle x-ray scattering (WAXS and SAXS, respectively). The XRD and WAXS analyses show Bragg peaks corresponding to a pure phase of reduced graphene oxide (rGO). PSA, SEM/TEM, AFM, and Raman analyses show that the use of HCl-assist in the solution during the exfoliation process has successfully reduced particle size of the obtained GPs. SAXS pattern of the exfoliated GPs using the assist of HCl, confirmed by TEM and AFM images, results in the specific particle sizes of between 1.42 and 4.99 nm. The present mechanical exfoliation technique has successfully been applied to obtain several nanometers of GPs and provides an alternative of simple synthesis of biomass – based graphene products.  相似文献   

2.
Water-processable nanoparticle dispersions of semiconducting polymers offer an attractive approach to the fabrication of organic electronic devices since they offer: (1) control of nanoscale morphology and (2) environmentally friendly fabrication. Although the nature of phase segregation in these polymer nanoparticles is critical to device performance, to date there have been no techniques available to directly determine their intra-particle structure, which consequently has been poorly understood. Here, we present scanning transmission x-ray microscopy (STXM) compositional maps for nanoparticles fabricated from poly(9,9-dioctyl-fluorene-2,7-diyl-co-bis-N, N'-(4-butylphenyl)-bis-N, N'-phenyl-1,4-phenylenedi-amine) (PFB) and poly(9,9-dioctylfluorene-2,7-diyl-co-benzothiadiazole) (F8BT) 1:1 blend mixtures. The images show distinct phase segregation within the nanoparticles. The compositional data reveals that, within these nanoparticles, PFB and F8BT segregate into a core-shell morphology, with an F8BT-rich core and a PFB-rich shell. Structural modelling demonstrates that the STXM technique is capable of quantifying morphological features on a sub-10 nm length scale; below the spot size of the incident focused x-ray beam. These results have important implications for the development of water-based 'solar paints' fabricated from microemulsions of semiconducting polymers.  相似文献   

3.
Photonic crystals consisting of nano- to micrometer-sized building blocks, such as multiple sorts of colloids, have recently received widespread attention. It remains a challenge, however, to adequately probe the internal crystal structure and the corresponding deformations that inhibit the proper functioning of such materials. It is shown that scanning transmission X-ray microscopy (STXM) can directly reveal the local structure, orientations, and even deformations in polystyrene and silica colloidal crystals with 30-nm spatial resolution. Moreover, STXM is capable of imaging a diverse range of crystals, including those that are dry and inverted, and provides novel insights complementary to information obtained by benchmark confocal fluorescence and scanning electron microscopy techniques.  相似文献   

4.
Magnetic nanoparticles (NPs) were functionalised with soy protein isolate (SPI) and bovine serum albumin (BSA) for inulinase immobilisation. The results revealed the nanomagnetite size of about 50 nm with a polydispersity index (PDI) of 0.242. The average size of the SPI NPs prepared by using acetone was 80–90 nm (PDI, 0.277), and SPI–BSA NPs was 80–90 nm (PDI, 0.233), and their zeta potential was around −34 mV. The mean diameter of fabricated Fe3 O4 @SPI–BSA NPs was <120 nm (PDI, 0.187). Inulinase was covalently immobilised successfully through glutaraldehyde on Fe3 O4 @SPI–BSA NPs with 80% enzyme loading. Fourier transform infrared spectra, field emission scanning electron microscopy, and transmission electron microscopy images provided sufficient proof for enzyme immobilisation on the NPs. The immobilised inulinase showed maximal activity at 45°C, which was 5°C higher than the optimum temperature of the free enzyme. Also, the optimum pH of the immobilised enzyme was shifted from 6 to 5.5. Thermal stability of the enzyme was considerably increased to about 43% at 75°C, and K m value was reduced to 25.4% after immobilisation. The half‐life of the enzyme increased about 5.13‐fold at 75°C as compared with the free form. Immobilised inulinase retained over 80% of its activity after ten cycles.Inspec keywords: magnetic particles, nanoparticles, proteins, molecular biophysics, nanofabrication, enzymes, Fourier transform spectra, infrared spectra, scanning electron microscopy, field emission ion microscopy, transmission electron microscopy, pH, biochemistry, nanobiotechnology, biomagnetism, electrokinetic effects, iron compoundsOther keywords: magnetic nanoparticles, soy protein isolate, bovine serum albumin, inulinase immobilisation, nanomagnetite, polydispersity index, SPI‐BSA NP, zeta potential, inulinase, glutaraldehyde, enzyme loading, Fourier transform infrared spectra, field emission scanning electron microscopy, transmission electron microscopy images, enzyme immobilisation, pH, size 80 nm to 90 nm, temperature 45 degC, temperature 75 degC, Fe3 O4   相似文献   

5.
Scanning transmission x-ray microscopy (STXM) and magnetoresistance (MR) measurements are used to investigate the magnetic behavior of a nanoconstriction joining two micrometric electrodes (a pad and a wire). The reversal of the magnetization under variable external static magnetic fields is imaged. By means of a detailed analysis of the STXM images at the nanocontact area, the MR is calculated, based on diffusive anisotropic-MR. This MR agrees well with that obtained from electrical transport measurements, allowing a direct correlation between the MR signal and the magnetic reversal of the system. The magnetization behavior depends on the sample thickness and constriction dimensions. In 40 nm-thick samples, with 20 × 175 nm(2) contact areas, the magnetization at the two sides of the constriction forms a net angle of 90°, with a progressive evolution of the magnetization structure between the electrodes during switching. The MR in those cases has a more peaked shape than with 20 nm-thick electrodes and 10 × 80 nm(2) contact areas, where the magnetization forms 180° between them, with a wide domain wall pinned at the constriction. As a consequence of this configuration, a plateau in the MR is observed for about 20 Oe.  相似文献   

6.
Bronnikov AV  Duifhuis G 《Applied optics》1998,37(20):4437-4448
We consider an application of the wavelet transform to image processing in x-ray imaging and three-dimensional (3-D) tomography aimed at industrial inspection. Our experimental setup works in two operational modes-digital radiography and 3-D cone-beam tomographic data acquisition. Although the x-ray images measured have a large dynamic range and good spatial resolution, their noise properties and contrast are often not optimal. To enhance the images, we suggest applying digital image processing by using wavelet-based algorithms and consider the wavelet-based multiscale edge representation in the framework of the Mallat and Zhong approach [IEEE Trans. Pattern Anal. Mach. Intell. 14, 710 (1992)]. A contrast-enhancement method by use of equalization of the multiscale edges is suggested. Several denoising algorithms based on modifying the modulus and the phase of the multiscale gradients and several contrast-enhancement techniques applying linear and nonlinear multiscale edge stretching are described and compared by use of experimental data. We propose the use of a filter bank of wavelet-based reconstruction filters for the filtered-backprojection reconstruction algorithm. Experimental results show a considerable increase in the performance of the whole x-ray imaging system for both radiographic and tomographic modes in the case of the application of the wavelet-based image-processing algorithms.  相似文献   

7.
Optical systems capable of three-dimensional transmission imaging are considered; these systems employ a conventional tomographic setup with an added linear shift-invariant optical system between the sample and the detector. A theoretical analysis is presented of image formation and sample reconstruction in such systems, examples of which include diffraction tomography and phase-contrast tomography with the use of analyzer crystals. An example is introduced in which the image is obtained by scanning the beam along the line orthogonal to the optic axis and to the axis of rotation with a one-dimensional slit or grating parallel to the rotation axis. We show that under certain conditions the proposed system may allow quantitative local (region-of-interest) tomography.  相似文献   

8.
We describe the distinction between the operation of a short focal length x-ray microscope forming a real image with a laboratory source (convergent illumination) and with a highly collimated intense beam from a synchrotron light source (Köhler illumination). We demonstrate the distinction with a Kirkpatrick-Baez microscope consisting of short focal length multilayer mirrors operating at an energy of 8 keV. In addition to realizing improvements in the resolution of the optics, the synchrotron radiation microscope is not limited to the usual single magnification at a fixed image plane. Higher magnification images are produced by projection in the limit of geometrical optics with a collimated beam. However, in distinction to the common method of placing the sample behind the optical source of a diverging beam, we describe the situation in which the sample is located in the collimated beam before the optical element. The ultimate limits of this magnification result from diffraction by the specimen and are determined by the sample position relative to the focal point of the optic. We present criteria by which the diffraction is minimized.  相似文献   

9.
Silica nanoparticles are imaged in solution with scanning transmission electron microscopy (STEM) using a liquid cell with silicon nitride (SiN) membrane windows. The STEM images reveal that silica structures are deposited in well‐defined patches on the upper SiN membranes upon electron beam irradiation. The thickness of the deposits is linear with the applied electron dose. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) demonstrate that the deposited patches are a result of the merging of the original 20 nm‐diameter nanoparticles, and that the related surface roughness depends on the electron dose rate used. Using this approach, sub‐micrometer scale structures are written on the SiN in liquid by controlling the electron exposure as function of the lateral position.  相似文献   

10.
We investigate the influence of annealing on the morphology of intimately mixed blends of the conjugated polymers poly(9,9'-dioctylfluorene-co-bis-N,N'-(4-butylphenyl)-bis-N,N'-phenyl-1,4-phenylene-diamine) (PFB) and poly(9,9'-dioctylfluorene-co-benzothiadiazole) (F8BT) with scanning transmission x-ray microscopy (STXM). Through the use of a zone plate with theoretical Rayleigh resolution of 30?nm, we are able to resolve sub-100?nm bulk structure in these films. Surprisingly, for unannealed films spin-coated from chloroform we observe features with an average diameter of 85?nm. The high degree of photoluminescence quenching in these as-spun films (>95%) implies that there is significant intermixing within the 85?nm structures, indicating that a hierarchy of phase separation exists even on the length scale of less than 100?nm. With annealing up to 160?°C, close to the T(g) of the components, there is little change in the feature sizes observed by STXM, although an increase in variation of the composition is observed. With annealing above 160?°C the imaged features begin to evolve in size, increasing to 225?nm in extent, alongside large changes in composition with annealing to 200?°C. Comparing the evolution of morphology imaged by STXM with the change in photoluminescence quenching with annealing, we propose that phase separation first evolves via the evolution of relatively pure phases on the length scale of a few to tens of nanometres within the larger 85?nm structures. Once the length scale of compositional fluctuations exceeds 85?nm (for anneal temperatures above 160?°C) the hierarchy of phase separation is lost and the subsequent morphological evolution is readily imaged by STXM. Applying the results of an exciton diffusion and quenching model, we find good agreement between the size of the domains measured by STXM (above 180?°C) and the results of the model for an exciton diffusion length of 15?nm. The growth in domain size and towards purer structures has also been observed with resonant soft x-ray scattering.  相似文献   

11.
The first in situ measurements with scanning transmission X-ray microscopy (STXM) of an active electrochemical cell are reported. An electrochemical wet cell, consisting of an electrodeposited polyaniline thin film on a thin Au film covered by an overlayer of 1 M HCl solution sitting between two X-ray transparent silicon nitride windows, was assembled. X-ray absorption images and spatial and time-resolved spectra of this system under potential control were examined using the beamline 5.3.2 STXM at the Advanced Light Source. The chemical state of the polyaniline film was reversibly converted between reduced (leucoemeraldine) and oxidized (emeraldine chloride) states by changing the applied potential. The electrochemical changes were monitored by spatially resolved C 1s and N 1s X-ray absorption spectroscopy and chemical-state selective imaging. Comparison of differences between images at two energies at different potentials provided electrochemical contrast with a resolution better than 50 nm, thereby monitoring that component of the polyaniline film that was electrochemically active. Kinematic studies in the subsecond regime are demonstrated.  相似文献   

12.
Digital tomosynthesis (DTS) has been widely used in both industrial nondestructive testing and medical x-ray imaging as a popular multiplanar imaging modality. However, although it provides some of the tomographic benefits of computed tomography (CT) at reduced dose and imaging time, the image characteristics are relatively poor due to blur artifacts originated from incomplete data sampling for a limited angular range and also aspects inherent to imaging system, including finite focal spot size of the x-ray source, detector resolution, etc. In this work, in order to overcome these difficulties, we propose an intuitive method in which a compressed-sensing (CS)-based deblurring scheme is applied to the projection images before common DTS reconstruction. We implemented the proposed deblurring algorithm and performed a systematic experiment to demonstrate its viability for improving the image characteristics in DTS. According to our results, the proposed method appears to be effective for the blurring problems in DTS and seems to be promising to our ongoing application to x-ray nondestructive testing.  相似文献   

13.
陈旖旎  白文坤  胡兵 《声学技术》2014,33(6):508-511
原子力声显微镜结合了超声检测技术的三维成像能力与原子力显微镜的纳米尺度成像的近场显微技术。它在商用的原子力显微镜设备的基础上加以压电超声传感器产生声激励,并使用锁相放大器对数据进行收集分析,既可得到三维的纳米级的清晰形貌图,又能通过建模分析样品表面的接触刚度及样品的弹性模量。目前,原子力显微镜被广泛应用于材料领域,用于检测样品的机械性能,比如样品的接触刚度、薄膜高分子材料的弹性模量,同时还运用于医学生物领域,用于观察细胞的超微结构及其表面和亚表面的弹性模量等。  相似文献   

14.
X-ray imaging in differential interference contrast (DIC) with submicrometer optical resolution was performed by using a twin zone plate (TZP) setup generating focal spots closely spaced within the TZP spatial resolution of 160 nm. Optical path differences introduced by the sample are recorded by a CCD camera in a standard full-field imaging and by an aperture photodiode in a standard scanning transmission x-ray microscope. Applying this x-ray DIC technique, we demonstrate for both the full-field imaging and scanning x-ray microscope methods a drastic increase in image contrast (approximately 20x) for a low-absorbing specimen, similar to the Nomarski DIC method for visible-light microscopy.  相似文献   

15.
Biosynthesis of novel therapeutic nano‐scale materials for biomedical and pharmaceutical applications has been enormously developed, since last decade. Herein, the authors report an ecological way of synthesising the platinum nanoparticles (PtNPs) using Streptomyces sp. for the first time. The produced PtNPs exhibited the face centred cubic system. The fourier transform infrared spectrum revealed the existence of amino acids in proteins which serves as an essential reductant for the formation of PtNPs. The spherical morphology of the PtNPs with an average size of 20–50 nm was observed from topographical images of atomic force microscopy and field emission scanning electron microscopy. The X‐ray fluorescence spectrum confirms the presence of PtNPs with higher purity. The PtNPs size was further confirmed with transmission electron microscopy analysis and the particles were found to exist in the same size regime. Additionally, PtNPs showed the characteristic surface plasmon resonance peak at 262 nm. Dynamic light scattering studies report that 97.2% of particles were <100 nm, with an average particle diameter of about 45 nm. Furthermore, 3‐(4, 5‐dimethyl‐2‐thiazolyl)‐2, 5‐diphenyl‐tetrazolium assay based in vitro cytotoxicity analysis was conducted for the PtNPs, which showed the inhibitory concentration (IC50) at 31.2 µg/ml against Michigan Cancer Foundation‐7 breast cancer cells.Inspec keywords: biomedical materials, materials preparation, nanoparticles, nanomedicine, nanofabrication, cellular biophysics, microorganisms, cancer, platinum, Fourier transform infrared spectra, proteins, atomic force microscopy, scanning electron microscopy, fluorescence, transmission electron microscopy, surface plasmon resonance, light scatteringOther keywords: cytotoxic potentials, biologically fabricated platinum nanoparticles, Streptomyces sp, MCF‐7 breast cancer cells, biosynthesis, therapeutic nanoscale materials, biomedical applications, pharmaceutical applications, Fourier transform infrared spectrum, amino acids, spherical morphology, topographical images, atomic force microscopy, field emission scanning electron microscopy, X‐ray fluorescence spectrum, transmission electron microscopy analysis, surface plasmon resonance, dynamic light scattering, 3‐(4, 5‐dimethyl‐2‐thiazolyl)‐2, 5‐diphenyl‐tetrazolium assay, cytotoxicity analysis, Pt  相似文献   

16.
Ideally, scanning probe microscopy (SPM) should generate a three-dimensional map of a sample surface such that the result is an exact replication of the actual sample. Any measurement data that result in an image differing from the actual sample surface are artifacts. The chief sources of SPM artifacts are mechanical systems, piezoelectric crystals, electronic scanners, tip-sample interaction, and image processing. For example, choosing the proper SPM probe for a specific sample is only the first step in minimizing probe-related artifacts. In fact, geometrical effects cause the largest number of artifacts. Good quality atomic SPM images can be clearly seen in raw data and should respond appropriately when the scan range or rotation is changed. Because SPM images are often periodic, it is possible for heavily filtered “data” to sometimes be misinterpreted as “atomic resolution images”. This paper presents SPM image studies using a range of materials from hard rough diamond films to soft nanometer smooth polyimide films. The investigation brings out the hidden sources of SPM artifacts for samples with different geometries and physical properties. Ten suggestions are presented which, if implemented/followed, should minimize the number of SPM image artifacts thereby assuring high quality images.  相似文献   

17.
Wright CA  Solares SD 《Nano letters》2011,11(11):5026-5033
In 2004 Hembacher et al. (Science 2004, 305, 380-383) reported simultaneous higher-harmonics atomic force mocroscopy (AFM)/scanning tunneling microscopy (STM) images acquired while scanning a graphite surface with a tungsten tip. They interpreted the observed subatomic features in the AFM images as the signature of lobes of increased electron density at the tungsten tip apex. Although these intriguing images have stirred controversy, an in-depth theoretical feasibility study has not yet been produced. Here we report on the development of a method for simulating higher harmonics AFM images and its application to the same system. Our calculations suggest that four lobes of increased electron density are expected to be present at a W(001) tip apex atom and that the corresponding higher harmonics AFM images of graphite can exhibit 4-fold symmetry features. Despite these promising results, open questions remain since the calculated amplitudes of the higher harmonics generated by the short-range forces are on the order of hundredths of picometers, leading to very small corrugations in the theoretical images. Additionally, the complex, intermittent nature of the tip-sample interaction, which causes constant readjustment of the tip and sample orbitals as the tip approaches and retracts from the surface, prevents a direct quantitative connection between the electron density and the AFM image features.  相似文献   

18.
Blind tip reconstruction(BTR) method is one of the favorable methods to estimate the atomic force microscopy(AFM) probe shape. The exact shape of the characterizer is not required for BTR, while the geometry of the sample may affect the reconstruction significantly. A cone-shaped array sample was chosen as a characterizer to be evaluated. The target AFM probe to be reconstructed was a diamond triangular pyramid probe with two feature angles, namely front angle(FA) and back angle(BA). Four conical structures with different semi-angles were dilated by the pyramid probe. Simulation of scanning process demonstrates that it is easy to judge from the images of the isolated rotary structure, cone-shaped, the suitability of the sample to be a tip characterizer for a pyramid probe. The cone-shaped array sample was repeatedly scanned 50 times by the diamond probe using an AFM. The series of scanning images shrank gradually and more information of the probe was exhibited in the images, indicating that the characterizer has been more suitable for BTR. The feature angle FA of the characterizer increasingly reduces during the scanning process. A self-adaptive grinding between the probe and the characterizer contributes to BTR of the diamond pyramid probe.  相似文献   

19.
The authors report the comparative antibacterial activity of silver nanoparticles synthesised by biological (using Fusarium oxysporum) and chemical routes in the presence and absence of pluronic F68 as a stabilising agent. The production of silver nanoparticles was evidenced by UV–visible spectra, with absorbance at about 420 nm in the case of both biological and chemical synthesis. X‐ray diffraction pattern confirmed the presence of face‐centred cubic structure (FCC plane). The nanoparticles characterised by transmission and scanning electron microscopy showed spherical silver nanoparticles with size range of 5–40 and 10–70 nm in the case of biologically and chemically synthesised nanoparticles, respectively. Addition of pluronic F68 showed the stabilisation of silver nanoparticles. Antibacterial efficacy of silver nanoparticles demonstrated different inhibitory activity against Escherichia coli, Pseudomonas aeruginosa and Staphylococcus aureus. Overall, biologically synthesised silver nanoparticles showed higher activity as compared with chemically synthesised nanoparticles. Silver nanoparticles synthesised in the presence of pluronic F68 by the chemical route exhibited synergism in antibacterial activity as compared with those synthesised without pluronic F68. On the contrary, biogenic silver nanoparticles without pluronic F68 showed higher antibacterial potential.Inspec keywords: antibacterial activity, nanofabrication, silver, X‐ray diffraction, biomedical materials, nanomedicine, transmission electron microscopy, scanning electron microscopy, ultraviolet spectra, visible spectra, materials preparation, nanoparticlesOther keywords: pluronic F68, stabilising agent, comparative antibacterial activity, Fusarium oxysporum, UV‐visible spectra, biological synthesis, chemical synthesis, X‐ray diffraction pattern, face‐centred cubic structure, FCC plane, transmission electron microscopy, scanning electron microscopy, spherical silver nanoparticles, antibacterial efficacy, Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, synergism, biogenic silver nanoparticles, wavelength 420 nm, size 10 nm to 70 nm, size 5 nm to 40 nm, Ag  相似文献   

20.
Green synthesis of silver nanoparticles (AgNPs) using Shivlingi (Bryonia laciniosa) seed extract was carried out. Characterisation of synthesised nanoparticles was accomplished through the optical absorption and photoluminescence spectrum, X‐ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. The XRD analysis further confirmed the size of nanoparticles ∼15 nm. TEM images revealed homogeneous spherical ∼10 nm Bryonia extract capped AgNPs. The biological studies indicated that both Bryonia seed extract and the nanoparticles lack anti‐microbial activity; however, the nanoparticles had better cytotoxicity and total antioxidant activity. The Lethal concentration (LC)50 value of water extract and the nanoparticles were found to be 1091 and 592 μg/ml, respectively. The lower LC50 of nanoparticles indicates that it is more cytotoxic than the crude extract. The results indicate that the Bryonia seed is safe to be used as a medicine and the formation of their nanoparticle has further enriched the chemical reactivity, energy absorption and biological mobility.Inspec keywords: silver, nanoparticles, nanomedicine, particle size, microorganisms, cellular biophysics, nanofabrication, photoluminescence, X‐ray diffraction, transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectra, Raman spectra, antibacterial activity, biochemistryOther keywords: green synthesis, biological studies, Shivlingi seed extraction, Bryonia laciniosa, silver nanoparticles, optical absorption, photoluminescence spectrum, X‐ray diffraction, transmission electron microscopy, scanning electron microscopy, SEM, Fourier transform infrared spectroscopy, Raman spectroscopy, XRD analysis, nanoparticle size, TEM images, homogeneous spherical images, antioxidant activity, water extraction, chemical reactivity, energy absorption, biological mobility, Ag  相似文献   

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