Calcium sulfoaluminate (CSA) cements are being developed using a novel processing method having as its objective lowering specific CO2 emissions by ∼50% relative to a Portland cement benchmark. We need to be able to measure the properties of the products. Porosity and permeability measurements help define the engineering properties but their quantification is influenced by the choice of experimental protocols. In the present study we used ordinary Portland cement (PC) paste as a benchmark and hydrated ye’elimite, which is a main component of CSA cements, to understand its pore structure. We report on the use of synchrotron-sourced radiation for µCT (Computerized Tomography) and 3D image re-construction of the internal micro-pore structure of PC and ye’elimite-gypsum pastes. As a comparison, porosity and permeability measurements were traditionally obtained using Mercury Intrusion Porosimetry (MIP). The Mori-Tanaka method and the polynomial statistical model were used to analyze the effects of different 3-D micro-pore structures on mechanical properties. The results show that e micro-pore structures differ considerably between PC and ye’elimite pastes and their bulk modulus is significantly affected by the shapes of their micro-pore structures.

In our earlier work [1] microstructural evolution in tungsten under self-ion irradiation was investigated as a function of temperature and dose by in-situ 150 keV W+ ion irradiations on the IVEM-Tandem facility at Argonne National Laboratory (ANL). The present work focuses on the thermal stability of this damage. Thin foils of tungsten were irradiated at room temperature (R.T.) to fluences up to 1018 W+m-2 (∼ 1.0 dpa) and were then annealed in-situ for up to 120 min at temperatures between 300 and 800°C.

We found that: (1) loops with Burgers vectors ½ <111> and <100> coexist during annealing; (2) <100> is not a stable loop configuration above 300°C and the fraction of such loops decreased with increasing temperature and/or time; (3) changes in loop populations during annealing were very sensitive to temperature, but less sensitive to time. The majority of changes occurred within 15 min, and were associated with the loss of small (1-2 nm) dislocation loops. The origin of these trends is discussed by considering defect mobility and the energetics of defect configurations predicted by previous DFT calculations [2].

The focused ion beam (FIB) has the necessary precision, spatial resolution and control over ion delivery for potential nano-scale doping of nanostructures such as semiconductor quantum dots (QDs). The ion current density in a FIB is 0.1-10 A/cm2, which is at least three orders of magnitude higher than that in a commercial broad beam ion implanter. Therefore an understanding of FIB implantation damage and recovery is of substantial interest. In this work we employ Raman probes of wavelengths 514 nm and 405 nm for quantifying ion implantation damage—both before and after annealing—in 30 kV Si2+, Ge2+ and Ga+ implants (fluences: 1x1012-5x1015 ions/cm2) into Si(100), for the purpose of understanding the effect of ion species on damage recovery.

Herein, we detail the fabrication of atomic force microscope (AFM) probes that have two and three coaxial electrodes at their tips. This fabrication strategy leverages the availability of conductive AFM probes and encompasses a general method for processing their complex and delicate structure through the deposition of insulating and conductive layers by shadow masked chemical and physical vapor deposition, respectively. Focused ion beam milling is used to expose the two electrode (coaxial) or three electrode (triaxial) structures at the tip of the AFM probe. Finally, we discuss new imaging modalities enabled by these probes including electrically-driven contact resonance imaging for nanoscale mechanical characterization, imaging the local dielectric constant by quantifying the dielectrophoretic force, and trapping functional particles at the tip of a probe using dielectrophoresis. These imaging techniques illustrate the generality and utility of this fabrication approach and suggest that such probes could be widely applied to image many nanoscale materials.

Spherical submicrometer-sized silica particles were prepared by the sol-gel method and deposited as a monolayer onto silicon wafers, in order to use them as a mask to create regular arrays of nanoscale surface features. Thus, by e-gun evaporation of a 50 nm thick Ag film through the silica mask, Ag nanostructures were obtained after removal of the silica monolayer. In order to tailor the mask characteristics (size and interparticle spacing), the silica masks were irradiated at room temperature with 4 and 6 MeV Si ions at different fluences up to 5×1015 ion/cm2, perpendicularly to the sample surface. After the irradiation the silica particles turned into oblate particles, as a result of the increase of the particle dimension perpendicular to the ion beam and the decrease in the parallel direction. By this way, the mask openings of the silica particle monolayer were modified as a function of the irradiation parameters, and the subsequent Ag e-gun evaporation allowed the formation of ordered arrays of Ag features. The size, shape and interparticle spacing of both the silica particles and the Ag deposits were determined by scanning electron microscopy.

Molecules such as dithiols are of significant interest for potential molecular electronics applications. To investigate their properties, an efficient method for measuring their electrical conductance is crucial. This research focuses on the time domain measurement, a novel technique capable of measuring hundreds of molecules within a matter of seconds. Measurements were conducted using STM with the tip positioned within tunneling distance over a SAM of 1,8-octanedithiol on Au(111)-mica substrate submerged in toluene. Bonding/debonding events between the tops of molecules and the tip were observed through jumps in the time domain current waveform. A new time-spent histogram data analysis technique was developed to extract conductance values from complex waveforms. Conductance of 2.6 nS was obtained for a single 1,8-octanedithiol molecule, consistent with results obtained from wellestablished but time consuming break junction technique, validating the new STM based time domain technique for fast measurement of molecular conductance.

Scanning probe microscopy, having the capability of nano-positioning and nanomanipulation, enables the characterization of material properties at a very small scale. In our previous work, the investigation of localized electrochemical reactions in Si3N4-TiC ceramic nanocomposites had been demonstrated using a single conductive scanning probe in a scanning impedance microscope (SIM). The results have provided experimental evidence that links the relations among microstructural heterogeneity, electrochemical property, and sintering behavior of spark plasma sintered ceramics. This single-probe SIM measurement gave through-body electrochemical information of specific surface feature of interest; however, the characterization of across-surface material properties in nanoscale is still much desired and unavailable.

To further investigate the heterogeneity of materials, we have designed and developed a dual-electrode scanning probe (DESP), which is capable of localized electrochemical characterization across the surface of a material. These probes were designed based on computer simulation and iterations, and fabricated using common semiconductor processing techniques. The span of two probes (electrodes) in our first prototypes was 10∼15 microns, which can be further reduced with optimized parameters. The DESP probes have been evaluated on Si3N4-TiC nanocomposites to demonstrate their functionality in topography scanning and in-situ impedance measurement. The impedance spectroscopy revealed two distinct impedance patterns for measurements across TiC-rich and Si3N4-rich surface regions. The design, fabrication, and evaluation of DESP were discussed in addition to the analysis of Si3N4-TiC nanocomposites.

Platinum particles supported in zeolites are used as catalysts for hydrogenation/ dehydrogenation reactions. In this study in situ high energy synchrotron X-ray diffraction was used to study the Pt particle formation under calcination and reduction conditions using time resolved pair distribution function (PDF). Because these particles grow inside the pores of zeolite X, PDF is able to give insight to unique information at the short and medium interatomic distance range that cannot be readily obtained with other techniques. Among the information obtained are the Pt atom interactions during calcination and the evolvement of the Pt particle sizes and average Pt-Pt distances during reduction.

We employ intense and short pulses of energetic lithium (Li+) ions to investigate the relaxation dynamics of radiation induced defects in single crystal silicon samples. Ions both create damage and track damage evolution simultaneously at short time scales when we use the channeling effect as a diagnostic tool. Ion pulses, ∼20 to 600 ns long and with peak currents of up to ∼1 A are formed in an induction type linear accelerator, the Neutralized Drift Compression eXperiment at Lawrence Berkeley National Laboratory. By rotating silicon (<100>) membranes of different thicknesses and changing the incident ion energy, the fraction of channeled ions in the transmitted beam could be varied. In preliminary experiments we find that the Li ion intensity is not high enough to generate overlapping cascades (in time and space) that would be necessary to measure a change in the shape of the current waveform of the transmitted ion beam. We discuss the concept of pump-probe type experiments with short ion beam pulses to access defect dynamics in materials and outline a path to increasing damage rates with heavier ions and by the application of longitudinal and lateral pulse compression techniques.

A statistically sound procedure for the unambiguous identification of the underlying Bravais lattice of an image of a 2D periodic array of objects is described. Our Bravais lattice detection procedure is independent of which type of microscope has been utilized for the recording of the image data. It is particularly useful for the correction of Scanning Tunneling Microscope (STM) images that suffer from a blunt scanning probe tip artifact, i.e. simultaneously recording multiple mini-tips. The unambiguous detection of the type of translation symmetry presents a first step towards making objective decisions about which plane symmetry a 2D periodic image is best modeled by. Such decisions are important for the application of Crystallographic Image Processing (CIP) techniques to images from Scanning Probe Microscopes (SPMs).

A scanning force microscope for in situ nanofocused X-ray studies (SFINX) has been developed which can be installed on diffractometers at synchrotron beamlines allowing for the combination with various techniques such as coherent X-ray diffraction and fluorescence. The capabilities of this device are demonstrated on Cu nanowires and on Au islands grown on sapphire (0001). The sample topography, crystallinity, and elemental distribution of the same area are investigated by recording simultaneously an AFM image, a scanning X-ray diffraction map, and a fluorescence map. Additionally, the mechanical response of Au islands is studied by in situ indentation tests employing the AFM-tip and recording 2D X-ray diffraction patterns during mechanical loading.

As the conventional atomic force microscopy (AFM) uses a Cartesian coordinate system to scan sample and the probe has different characteristics in each direction, it is impossible to scan in arbitrary direction. Therefore, we present the AFM which is able to rotate its probe. The deflection of cantilever was measured using optical pickup head of DVD drive. For verifying the system feasibility, the multidirectional scanning of the standard sample was carried out. Also we presented the modified structure which includes aligner and mirror to enhance the performance.