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At least 37 records · Page 2

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DOE OSTI2013

Surface sampling concentration and reaction probe

A method of analyzing a chemical composition of a specimen is described. The method can include providing a probe comprising an outer capillary tube and an inner capillary tube disposed co-axially within the outer capillary tube, where the inner and outer capillary tubes define a solvent capillary and a sampling capillary in fluid communication with one another at a distal end of the probe; contacting a target site on a surface of a specimen with a solvent in fluid communication with the probe; maintaining a plug volume proximate a solvent-specimen interface, wherein the plug volume is in fluid communication with the probe; draining plug sampling fluid from the plug volume through the sampling capillary; and analyzing a chemical composition of the plug sampling fluid with an analytical instrument. A system for performing the method is also described.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Surface sampling concentration and reaction probe with controller to adjust sampling position

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2011

Molecular Surface Sampling and Chemical Imaging using Proximal Probe Thermal Desorption/Secondary Ionization Mass Spectrometry

Proximal probe thermal desorption/secondary ionization mass spectrometry was studied and applied to molecular surface sampling and chemical imaging using printed patterns on photopaper as test substrates. With the use of a circular cross section proximal probe with a tip diameter of 50 m and fixed temperature (350 C), the influence of probe-to-surface distance, lane scan spacing, and surface scan speed on signal quality and spatial resolution were studied and optimized. As a compromise between signal amplitude, signal reproducibility, and data acquisition time, a surface scan speed of 100 m/s, probe-to-paper surface distance of 5 m, and lane spacing of 10 m were used for imaging. Under those conditions the proximal probe thermal desorption/secondary ionization mass spectrometry method was able to achieve a spatial resolution of about 50 m as determined by the ability to distinguish surface patterns of known dimensions that were printed on the paper substrate. It is expected that spatial resolution and chemical image quality could be further improved by using probes of smaller cross section size and by incorporating a means to maintain a fixed optimal probe-to-surface distance real time, continuously adapting to the changing topography of the surface during a lane scan.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Sampling probe

A system for sampling a surface includes a sampling probe including a housing with a probe end having a sampling fluid opening, a sampling fluid supply conduit and a sampling fluid exhaust conduit. The sampling fluid supply conduit supplies sampling fluid to the sampling fluid opening. The sampling fluid exhaust conduit includes a wall, a sampling fluid exhaust conduit inlet opening for removing sampling fluid from the sampling fluid opening, and a sampling fluid exhaust conduit outlet opening for removing fluid from the sampling fluid exhaust conduit. A sampling fluid analytic conduit is also provided in the sampling probe and has a sampling fluid analytic conduit inlet opening spaced upstream from the sampling fluid exhaust conduit outlet opening, downstream from the sampling fluid exhaust conduit inlet opening, and from the wall of the sampling fluid exhaust conduit. A wash conduit can also be provided. Methods for sampling are also disclosed.

Van Berkel, Gary↗

DOE OSTI2011

Near-field examination of perovskite-based superlenses and superlens-enhanced probe-object coupling

A planar slab of negative-index material works as a superlens with sub-diffraction-limited resolution, as propagating waves are focused and, moreover, evanescent waves are reconstructed in the image plane. Here we demonstrate a superlens for electric evanescent fields with low losses using perovskites in the mid-infrared regime. The combination of nearfield microscopy with a tunable free-electron laser allows us to address precisely the polariton modes, which are critical for super-resolution imaging. We spectrally study the lateral and vertical distributions of evanescent waves around the image plane of such a lens, and achieve imaging resolution of λ/14 at the superlensing wavelength. Interestingly, at certain distances between the probe and sample surface, we observe a maximum of these evanescent fields. Comparisons with numerical simulations indicate that this maximum originates from an enhanced coupling between probe and object, which might be applicable for multifunctional circuits, infrared spectroscopy and thermal sensors.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Super resolution for magneto-optical microscopy

Sub-diffraction limited magneto-optical microscopy, such as Kerr or Faraday effect microscopy, provide many advantages to fields of science and technology for measuring, or imaging, the magnetization structures and magnetization domains of materials. Disclosed is a method and system for performing sub-diffraction limited magneto-optic microscopy. The method includes positioning a microlens or microlens layer relative to a surface of a sample to image the surface of the sample, forming a photonic nanojet to probe the surface of the sample, and receiving light reflected by the surface of the sample or transmitted through the sample at an imaging sensor. The methods and associated systems and devices enable sub-diffraction limited imaging of magnetic domains at resolutions 2 to 8 times the classical diffraction limit.

te Velthuis, Suzanne Gabriëlle Everdine↗

DOE OSTI2013

Laser Ablation Sampling of Materials Directly into the Formed Liquid Microjunction of a Continuous Flow Surface Sampling Probe/Electrospray Ionization Emitter for Mass Spectral Analysis and Imaging

Transmission geometry laser ablation directly into a formed liquid microjunction of a continuous flow liquid microjunction surface sampling probe/electrospray ionization emitter was utilized for molecular and elemental detection and mass spectrometry imaging. The ability to efficiently capture and ionize ablated material was demonstrated by the detection of various small soluble n-mers of polyaniline and silver ion solvent clusters formed from laser ablation of electropolymerized polyaniline and silver thin films, respectively. In addition, analysis of surfaces that contain soluble components was accomplished by coating or laminating the sample with an insoluble film to enable liquid junction formation without directly extracting material from the surface. The ability to perform mass spectrometry imaging at a spatial resolution of about 50 m was illustrated by using laminated inked patterns on a microscope slide. In general, these data demonstrate at least an order of magnitude signal enhancement compared to the non-contact, laser ablation droplet capture-based surface sampling/ionization approaches that have been previously presented.

electrospray ionization (ESI)↗

DOE OSTI2022

Porous membrane enabled mass spectrometry characterization of microfluidic devices

A system for sampling a liquid includes a sample fluid conduit including a membrane having pores. The membrane prevents the passage of the sample liquid through the pores at a first pressure of the sample liquid in the sample fluid conduit. A surface sampling capture probe has a distal end. The capture probe includes a solvent supply conduit and a solvent exhaust conduit. A solvent composition flowing at the distal end of the capture probe establishes a liquid junction with the membrane and establishes a second pressure within the liquid junction at the membrane. The second pressure is lower than the first pressure. Sample liquid will be drawn through the pores of the membrane by the second pressure at the liquid junction. A method for sampling a liquid and for performing chemical analysis on a liquid are also disclosed.

Cahill, John F.↗

DOE OSTI2024

Porous membrane enabled mass spectrometry characterization of microfluidic devices

Cahill, John F.↗

DOE OSTI2014

Direct determination of the local Hamaker constant of inorganic surfaces based on scanning force microscopy

The energetics involved in the bonding fluctuations between nanometer-sized silicon dioxide (SiO{sub 2}) probes and highly oriented pyrolytic graphite (HOPG) and molybdenum disulfide (MoS{sub 2}) could be quantified directly and locally on the submicron scale via a time-temperature superposition analysis of the lateral forces between scanning force microscopy silicon dioxide probes and inorganic sample surfaces. The so-called “intrinsic friction analysis” (IFA) provided direct access to the Hamaker constants for HOPG and MoS{sub 2}, as well as the control sample, calcium fluoride (CaF{sub 2}). The use of scanning probe enables nanoscopic analysis of bonding fluctuations, thereby overcoming challenges associated with larger scale inhomogeneity and surface roughness common to conventional techniques used to determine surface free energies and dielectric properties. A complementary numerical analysis based on optical and electron energy loss spectroscopy and the Lifshitz quantum electrodynamic theory of van der Waals interactions is provided and confirms quantitatively the IFA results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Applications of Subsurface Microscopy

Exploring the interior of a cell is of tremendous importance in order to assess the effects of nanomaterials on biological systems. Outside of a controlled laboratory environment, nanomaterials will most likely not be conveniently labeled or tagged so that their translocation within a biological system cannot be easily identified and quantified. Ideally, the characterization of nanomaterials within a cell requires a nondestructive, label-free, and subsurface approach. Subsurface nanoscale imaging represents a real challenge for instrumentation. Indeed the tools available for high resolution characterization, including optical, electron or scanning probe microscopies, mainly provide topography images or require tagants that fluoresce. Although the intercellular environment holds a great deal of information, subsurface visualization remains a poorly explored area. Recently, it was discovered that by mechanically perturbing a sample, it was possible to observe its response in time with nanoscale resolution by probing the surface with a micro-resonator such as a microcantilever probe (Figure 1). Microcantilevers are used as the force-sensing probes in Atomic Force Microscopy (AFM), where the nanometer-scale probe tip on the microcantilever interacts with the sample in a highly controlled manner to produce high-resolution raster-scanned information of the sample surface. Taking advantage of the existing capabilities of AFM, we present a novel technique, Mode Synthesizing Atomic Force Microscopy (MSAFM) (Figure 1), which has the ability to probe subsurface structures such as non-labeled nanoparticles embedded in a cell. In MSAFM mechanical actuators (PZTs) excite the probe and the sample at different frequencies as depicted in Figure 1. The nonlinear nature of the tip-sample interaction, at the point of contact of the probe and the surface of the sample, in the contact mode AFM configuration permits the mixing of the elastic waves. The new dynamic system comprises new synthesized imaging modes, resulting from sum- and difference-frequency generation of the driving frequencies. The specific electronics of MSAFM allows the selection of individual modes and the monitoring of their amplitude and phase. From these quantities of various synthesized modes a series of images can be acquired. The new images contain subsurface information, thus revealing the presence of nanoparticles inside the cells.

Tetard, Laurene↗

DOE OSTI2014

Atomic Force Microscope Controlled Topographical Imaging and Proximal Probe Thermal Desorption/Ionization Mass Spectrometry Imaging

This paper reports on the development of a hybrid atmospheric pressure atomic force microscopy/mass spectrometry imaging system utilizing nano-thermal analysis probes for thermal desorption surface sampling with subsequent atmospheric pressure chemical ionization and mass analysis. The basic instrumental setup and the general operation of the system were discussed and optimized performance metrics were presented. The ability to correlate topographic images of a surface with atomic force microscopy and a mass spectral chemical image of the same surface, utilizing the same probe without moving the sample from the system, was demonstrated. Co-registered mass spectral chemical images and atomic force microscopy topographical images were obtained from inked patterns on paper as well as from a living bacterial colony on an agar gel. Spatial resolution of the topography images based on pixel size (0.2 m x 0.8 m) was better than the resolution of the mass spectral images (2.5 m x 2.0 m), which were limited by current mass spectral data acquisition rate and system detection levels.

Ovchinnikova, Olga S↗

DOE OSTI2014

Combining low-energy electron microscopy and scanning probe microscopy techniques for surface science: Development of a novel sample-holder

We introduce an experimental facility dedicated to surface science that combines Low-Energy Electron Microscopy/Photo-Electron Emission Microscopy (LEEM/PEEM) and variable-temperature Scanning Probe Microscopy techniques. A technical challenge has been to design a sample-holder that allows to exploit the complementary specifications of both microscopes and to preserve their optimal functionality. Experimental demonstration is reported by characterizing under ultrahigh vacuum with both techniques: Au(111) surface reconstruction and a two-layer thick graphene on 6H-SiC(0001). A set of macros to analyze LEEM/PEEM data extends the capabilities of the setup.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2017

Quantification of in-contact probe-sample electrostatic forces with dynamic atomic force microscopy

Here, atomic force microscopy (AFM) methods utilizing resonant mechanical vibrations of cantilevers in contact with a sample surface have shown sensitivities as high as few picometers for detecting surface displacements. Such a high sensitivity is harnessed in several AFM imaging modes. Here, we demonstrate a cantilever-resonance-based method to quantify electrostatic forces on a probe in the probe-sample junction in the presence of a surface potential or when a bias voltage is applied to the AFM probe. We find that the electrostatic forces acting on the probe tip apex can produce signals equivalent to a few pm of surface displacement. In combination with modeling, the measurements of the force were used to access the strength of the electrical field at the probe tip apex in contact with a sample. We find an evidence that the electric field strength in the junction can reach ca. 1 V nm –1 at a bias voltage of a few volts and is limited by non-ideality of the tip-sample contact. This field is sufficiently strong to significantly influence material states and kinetic processes through charge injection, Maxwell stress, shifts of phase equilibria, and reduction of energy barriers for activated processes. Besides, the results provide a baseline for accounting for the effects of local electrostatic forces in electromechanical AFM measurements as well as offer additional means to probe ionic mobility and field-induced phenomena in solids.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Formation of a memristor matrix based on titanium oxide and investigation by probe-nanotechnology methods

The results of investigation of a memristor-matrix model on the basis of titanium-oxide nanoscale structures (ONSs) fabricated by methods of focused ion beams and atomic-force microscopy (AFM) are presented. The effect of the intensity of interaction between the AFM probe and the sample surface on the memristor effect in the titanium ONS is shown. The memristor effect in the titanium ONS is investigated by an AFM in the mode of spreading-resistance map. The possibility of the recording and erasure of information in the submicron cells is shown on the basis of using the memristor effect in the titanium ONS, which is most promising for developing the technological processes of the formation of resistive operation memory cells.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Constant-Distance Mode Nanospray Desorption Electrospray Ionization Mass Spectrometry Imaging of Biological Samples with Complex Topography

A new approach for constant distance mode mass spectrometry imaging of biological samples using nanospray desorption electrospray ionization (nano-DESI MSI) was developed by integrating a shear-force probe with nano-DESI probe. The technical concept and basic instrumental setup as well as general operation of the system are described. Mechanical dampening of resonant oscillations due to the presence of shear forces between the probe and the sample surface enables constant-distance imaging mode via a computer controlled closed feedback loop. The capability of simultaneous chemical and topographic imaging of complex biological samples is demonstrated using living Bacillus Subtilis ATCC 49760 colonies on agar plates. The constant-distance mode nano-DESI MSI enabled imaging of many metabolites including non-ribosomal peptides (surfactin, plipastatin and iturin) and iron-bound heme on the surface of living bacterial colonies ranging in diameter from 10 mm to 13 mm with height variations of up to 0.8 mm above the agar plate. Co-registration of ion images to topographic images provided higher-contrast images. Constant-mode nano-DESI MSI is ideally suited for imaging biological samples of complex topography in their native state.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Co-registered Topographical, Band Excitation Nanomechanical, and Mass Spectral Imaging Using a Combined Atomic Force Microscopy/Mass Spectrometry Platform

The advancement of a hybrid atomic force microscopy/mass spectrometry imaging platform demonstrating for the first time co-registered topographical, band excitation nanomechanical, and mass spectral imaging of a surface using a single instrument is reported. The mass spectrometry-based chemical imaging component of the system utilized nanothermal analysis probes for pyrolytic surface sampling followed by atmospheric pressure chemical ionization of the gas phase species produced with subsequent mass analysis. We discuss the basic instrumental setup and operation and the multimodal imaging capability and utility are demonstrated using a phase separated polystyrene/poly(2-vinylpyridine) polymer blend thin film. The topography and band excitation images showed that the valley and plateau regions of the thin film surface were comprised primarily of one of the two polymers in the blend with the mass spectral chemical image used to definitively identify the polymers at the different locations. Data point pixel size for the topography (390 nm x 390 nm), band excitation (781 nm x 781 nm), mass spectrometry (690 nm x 500 nm) images was comparable and submicrometer in all three cases, but the data voxel size for each of the three images was dramatically different. The topography image was uniquely a surface measurement, whereas the band excitation image included information from an estimated 10 nm deep into the sample and the mass spectral image from 110-140 nm in depth. Moreover, because of this dramatic sampling depth variance, some differences in the band excitation and mass spectrometry chemical images were observed and were interpreted to indicate the presence of a buried interface in the sample. The spatial resolution of the mass spectral image was estimated to be between 1.5 m 2.6 m, based on the ability to distinguish surface features in that image that were also observed in the other images.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Neutron and X-Ray Studies of Advanced Materials V: CENTENNIAL Symposium

In 2012 the diffraction community will celebrate 100 years since the prediction of X-ray diffraction by M. Laue, and following his suggestion the first beautiful diffraction experiment by W. Friedrich and P. Knipping. The significance of techniques based on the analysis of the diffraction of X-rays, neutrons, electrons and Mossbauer photons discovered later, has continued to increase in the past 100 years. The aim of this symposium is to provide a forum for discussion of using state-of-the-art neutron and X-ray scattering techniques for probing advanced materials. These techniques have been widely used to characterize materials structures across all length scales, from atomic to nano, meso, and macroscopic scales. With the development of sample environments, in-situ experiments, e.g., at temperatures and applied mechanical load, are becoming routine. The development of ultra-brilliant third-generation synchrotron X-ray sources, together with advances in X-ray optics, has created intense X-ray microbeams, which provide the best opportunities for in-depth understanding of mechanical behavior in a broad spectrum of materials. Important applications include ultra-sensitive elemental detection by X-ray fluorescence/absorption and microdiffraction to identify phase and strain with submicrometer spatial resolution. X-ray microdiffraction is a particularly exciting application compared with alternative probes of crystalline structure, orientation and strain. X-ray microdiffraction is non-destructive with good strain resolution, competitive or superior spatial resolution in thick samples, and with the ability to probe below the sample surface. Advances in neutron sources and instrumentation also bring new opportunities in neutron scattering research. In addition to characterizing the structures, neutrons are also a great tool for elucidating the dynamics of materials. Because neutrons are highly penetrating, neutrons have been used to map stress in engineering systems. Neutrons have also played a vital role in our understanding of the magnetism and magnetic properties. Specialized instruments have been built to gain physical insights of the fundamental mechanisms governing phase transformation and mechanical behaviors of materials. The application of those techniques, in combination with theoretical simulations and numerical modeling, will lead to major breakthroughs in materials science in the foreseeable future that will contribute to the development of materials technology and industrial innovation.

36 MATERIALS SCIENCE↗