Time-lapse lab-based x-ray nano-CT study of corrosion damage.

An experimental protocol (workflow) has been developed for time-lapse x-ray nanotomography (nano-CT) imaging of environmentally driven morphological changes to materials. Two case studies are presented. First, the leaching of nanoparticle corrosion inhibitor pigment from a polymer coating was followed over 14 days, while in the second case the corrosion damage to an AA2099 aluminium alloy was imaged over 12 hours. The protocol includes several novel aspects relevant to nano-CT with the use of a combination of x-ray absorption and phase contrast data to provide enhanced morphological and composition information, and hence reveal the best information to provide new insights into the changes of different phases over time. For the pigmented polymer coating containing nominally strontium aluminium polyphosphate, the strontium-rich components within the materials are observed to leach extensively whereas the aluminium-rich components are more resistant to dissolution. In the case of AA2099 it is found that the initial grain boundary corrosion is driven by the presence of copper-rich phases and is then followed by the corrosion of grains of specific orientation.

The Bionanoprobe: hard X-ray fluorescence nanoprobe with cryogenic capabilities.

Hard X-ray fluorescence microscopy is one of the most sensitive techniques for performing trace elemental analysis of biological samples such as whole cells and tissues. Conventional sample preparation methods usually involve dehydration, which removes cellular water and may consequently cause structural collapse, or invasive processes such as embedding. Radiation-induced artifacts may also become an issue, particularly as the spatial resolution increases beyond the sub-micrometer scale. To allow imaging under hydrated conditions, close to the `natural state', as well as to reduce structural radiation damage, the Bionanoprobe (BNP) has been developed, a hard X-ray fluorescence nanoprobe with cryogenic sample environment and cryo transfer capabilities, dedicated to studying trace elements in frozen-hydrated biological systems. The BNP is installed at an undulator beamline at sector 21 of the Advanced Photon Source. It provides a spatial resolution of 30 nm for two-dimensional fluorescence imaging. In this first demonstration the instrument design and motion control principles are described, the instrument performance is quantified, and the first results obtained with the BNP on frozen-hydrated whole cells are reported.

An in-vacuum x-ray diffraction microscope for use in the 0.7-2.9 keV range.

A dedicated in-vacuum coherent x-ray diffraction microscope was installed at the 2-ID-B beamline of the Advanced Photon Source for use with 0.7-2.9 keV x-rays. The instrument can accommodate three common implementations of diffractive imaging; plane wave illumination; defocused-probe (Fresnel diffractive imaging) and scanning (ptychography) using either a pinhole, focused or defocused probe. The microscope design includes active feedback to limit motion of the optics with respect to the sample. Upper bounds on the relative optics-to-sample displacement have been measured to be 5.8 nm(v) and 4.4 nm(h) rms/h using capacitance micrometry and 27 nm/h using x-ray point projection imaging. The stability of the measurement platform and in-vacuum operation allows for long exposure times, high signal-to-noise and large dynamic range two-dimensional intensity measurements to be acquired. Finally, we illustrate the microscope's stability with a recent experimental result.

Differential phase contrast with a segmented detector in a scanning X-ray microprobe.

Scanning X-ray microprobes are unique tools for the nanoscale investigation of specimens from the life, environmental, materials and other fields of sciences. Typically they utilize absorption and fluorescence as contrast mechanisms. Phase contrast is a complementary technique that can provide strong contrast with reduced radiation dose for weakly absorbing structures in the multi-keV range. In this paper the development of a segmented charge-integrating silicon detector which provides simultaneous absorption and differential phase contrast is reported. The detector can be used together with a fluorescence detector for the simultaneous acquisition of transmission and fluorescence data. It can be used over a wide range of photon energies, photon rates and exposure times at third-generation synchrotron radiation sources, and is currently operating at two beamlines at the Advanced Photon Source. Images obtained at around 2 keV and 10 keV demonstrate the superiority of phase contrast over absorption for specimens composed of light elements.

Quantitative phase imaging with a scanning transmission x-ray microscope.

We obtain quantitative phase reconstructions from differential phase contrast images obtained with a scanning transmission x-ray microscope and 2.5 keV x rays. The theoretical basis of the technique is presented along with measurements and their interpretation.

Storage effects on dentin permeability and shear bond strengths.

The effects of duration of storage and selection of storage solution upon dentin permeability and bond strength were studied over a period of 8 days to 6 mon. Teeth were stored immediately after extraction in one of five commonly used solutions: 70% ethanol (E); 10% formalin (F); distilled water (W); distilled water with thymol (WT); or phosphate-buffered saline with thymol (ST). Permeability and lap shear bond strength measurements were evaluated in a repeated measures design (n = 20) after 8 days, 15 days and 6 mon. Dentin permeability varied with solution type and duration of storage as demonstrated by ANOVA, increasing F, E and the water-based solutions, respectively. Saline storage resulted in large significant decreases in permeability after prolonged storage, suggesting changes in dentin. Bond strengths were unaffected by duration of storage or by solution type, except for saline. Thus, permeability and bond strength values may be affected by storage conditions. The results of this study indicate that saline, the most commonly used solution in dental materials research, may be unsuitable for use as a result of its effect on dentin permeability and bond strength.

Influence of tissue heterogeneity on the determination of steroid receptors in breast cancer.

Biochemical determination of hormone receptors in carcinomas is influenced by the potential heterogeneity of the tissue samples. In order to check this, samples of 16 breast cancers were divided into 6 segments. These segments were alternately examined for their ratio of tumor tissue to connective tissue ("percentage of carcinoma") or for the content of estrogen and progesterone receptors. Only 3 of the tumors were homogeneous, and 9 of the heterogeneous tissues had hormone receptors. The segment with the maximum "percentage of carcinoma" was adjacent to that with the peak value of hormone receptors in all but 1 tissue. The same applied to the minima. The maximum and minimum values of estrogen and progesterone receptors were located within the same segment in all but one tissue sample. The results demonstrated that biochemical assay of hormone receptors is reliable. A reduction of the sample volume does not enhance the precision of the receptor assay, since it increases the possibility of a false negative result.