G. Denbeaux

High resolution protein localization using soft X-ray microscopy.

Soft X‐ray microscopes can be used to examine whole, hydrated cells up to 10 µm thick and produce images approaching 30 nm resolution. Since cells are imaged in the X‐ray transmissive ‘water window’, where organic material absorbs approximately an order of magnitude more strongly than water, chemical contrast enhancement agents are not required to view the distribution of cellular structures. Although living specimens cannot be examined, cells can be rapidly frozen at a precise moment in time and examined in a cryostage, revealing information that most closely approximates that in live cells. In this study, we used a transmission X‐ray microscope at photon energies just below the oxygen edge (λ = 2.4 nm) to examine rapidly frozen mouse 3T3 cells and obtained excellent cellular morphology at better than 50 nm lateral resolution. These specimens are extremely stable, enabling multiple exposures with virtually no detectable damage to cell structures. We also show that silver‐enhanced, immunogold labelling can be used to localize both cytoplasmic and nuclear proteins in whole, hydrated mammary epithelial cells at better than 50 nm resolution. The future use of X‐ray tomography, along with improved zone plate lenses, will enable collection of better resolution (approaching 30 nm), three‐dimensional information on the distribution of proteins in cells.

Nanofabrication and diffractive optics for high-resolution x-ray applications

Short wavelength x-ray radiation microscopy is well suited for a number of material and life science studies. The x-ray microscope (XM1) at the Advanced Light Source Synchrotron in Berkeley, California uses two diffractive Fresnel zone plate lenses. The first is a large condenser lens, which collects soft x-ray radiation from a bending magnet, focuses it, and serves as a linear monochromator. The second is the objective zone plate lens, which magnifies the image of the specimen onto a high-efficiency charge coupled device detector. The objective lens determines the numerical aperture and ultimate resolution. New objective lens zone plates with a minimum linewidth of 25 nm and excellent linewidth control have been fabricated using Berkeley Lab’s 100 keV Nanowriter electron beam lithography tool, a calixarene high-resolution negative resist, and gold electroplating. Although the condenser zone plate is less critical to the resolution of the instrument, its efficiency determines the flux on the sample and ul...

High-resolution imaging of fast magnetization dynamics in magnetic nanostructures

By combining magnetic transmission x-ray microscopy with a stroboscopic pump and probe technique using synchrotron radiation we are able to image the magnetization dynamics in micron sized magnetic particles on a sub-100 ps time scale with a lateral spatial resolution down to 21 nm. We report first observations in squared elements indicating locally varying precessional frequencies which are in agreement with micromagnetic simulations. The experiment opens a route towards a high spatiotemporal resolution of spin patterns which is needed to understand the microscopic origin of magnetization reversal of micron sized and nano-sized magnetic particles.

Element-specific imaging of magnetic domains at 25 nm spatial resolution using soft x-ray microscopy

The combination of magnetic circular dichroism as a magnetic contrast mechanism and a transmission x-ray microscope allows imaging of magnetic structures with lateral resolutions down to 25 nm. Results on magneto-optical Tb25(Fe75Co25)75 layers system with thermomagnetically written bits of various sizes were obtained at the x-ray microscope XM-1 at the Advanced Light Source in Berkeley, CA. The results prove the thermal stability of the bits in the recording process. Furthermore the capability of soft x-ray microscopy with respect to the achievable lateral resolution, element specificity and sensitivity to thin magnetic layers is demonstrated. The potential of imaging in applied magnetic fields for both out-of-plane and in-plane magnetized thin magnetic films is outlined.

X-ray studies of aligned magnetic stripe domains in perpendicular multilayers

We have investigated the stripe domain structure and the magnetic reversal of perpendicular Co/Pt based multilayers at room temperature using magnetometry, magnetic imaging and magnetic x-ray scattering. In-plane field cycling aligns the stripe domains along the field direction. In magnetic x-ray scattering the parallel stripe domains act as a magnetic grating resulting in observed Bragg reflections up to 5th order. We model the scattering profile to extract and quantify the domain as well as domain wall widths. Applying fields up to {approx}1.2 kOe perpendicular to the film reversibly changes the relative width of up versus down domains while maintaining the overall stripe periodicity. Fields above 1.2 kOe introduce irreversible changes into the domain structure by contracting and finally annihilating individual stripe domains. We compare the current results with modeling and previous measurements of films with perpendicular anisotropy.

20-nm-resolution Soft x-ray microscopy demonstrated by use of multilayer test structures

A spatial resolution of 20 nm is demonstrated at 2.07-nm wavelength by use of a soft x-ray microscope based on Fresnel zone plate lenses and partially coherent illumination. Nanostructural test patterns, formed by sputtered multilayer coatings and transmission electron microscopy thinning techniques, provide clear experimental results.

Dynamical x-ray microscopy investigation of electromigration in passivated inlaid Cu interconnect structures

Quantitative time-resolved x-ray microscopy mass transport studies of the early stages of electromigration in an inlaid Cu line/via structure were performed with about 40 nm lateral resolution. The image sequences show that void formation is a highly dynamic process, with voids being observed to nucleate and grow within the Cu via and migrate towards the via sidewall. Correlation of the real time x-ray microscopy images with postmortem high voltage electron micrographs of the sample indicates that the void nucleation occurs at the site of grain boundaries in Cu, and that the voids migrate along these grain boundaries during electromigration.

Soft x-ray microscopy to 25 nm with applications to biology and magnetic materials

We report both technical advances in soft X-ray microscopy (XRM) and applications furthered by these advances. With new zone plate lenses we record test pattern features with good modulation to 25 nm and smaller. In combination with fast cryofixation, sub-cellular images show very fine detail previously seen only in electron microscopy, but seen here in thick, hydrated, and unstained samples. The magnetic domain structure is studied at high spatial resolution with X-ray magnetic circular dichroism (X-MCD) as a huge element-specific magnetic contrast mechanism, occurring e.g. at the L2,3 edges of transition metals. It can be used to distinguish between in-plane and out-of-plane contributions by tilting the sample. As XRM is a photon based technique, the magnetic images can be obtained in unlimited varying external magnetic fields. The images discussed have been obtained at the XM-1 soft X-ray microscope on beamline 6.1 at the Advanced Light Source in Berkeley. # 2001 Elsevier Science B.V. All rights reserved.

Study of in-plane magnetic domains with magnetic transmission x-ray microscopy

Magnetic transmission x-ray microscopy is a novel technique to image element specifically magnetic domain structures. A lateral resolution down to 25 nm is provided by the Fresnel zone plates used as optical elements in soft x-ray microscopy. The magnetic contrast is given by x-ray magnetic circular dichroism, i.e., large magnetic contributions up to 25% to the absorption cross section of circularly polarized x rays that occur in the vicinity of, e.g., the Fe L3,2 edges (706 and 719 eV) and depend on the relative orientation of the projection of the magnetization of the sample onto the photon propagation direction. Thus, both in-plane and out-of-plane contributions to the magnetization are accessible. Here we present images of the magnetic domain structure of a (3 nm Cr/50 nm Fe/6 nm Cr) thin film system with a preferentially in-plane magnetization recorded at the Fe L edges. The samples have been prepared by thermal evaporation onto a 100 nm thin Si3N4 membrane and were mounted under a tilt of 30° with r...

Magnetic imaging of ion-irradiation patterned Co/Pt multilayers using complementary electron and photon probes

The three-dimensional magnetic structure and reversal mechanism of patterned Co/Pt multilayers, were imaged using complementary Lorentz transmission electron microscopy (LTEM) (in-plane component) and magnetic transmission x-ray microscopy (M-TXM) (perpendicular magnetization). The Co/Pt films with perpendicular anisotropy were patterned by ion irradiation through a stencil mask to produce in-plane magnetization in the irradiated regions. The boundaries of the patterns, defined by the transition from out-of-plane to in-plane magnetization, were found to be determined by the stencil mask, whilst the scale of the magnetic reversal by the physical microstructure. The nucleation fields were substantially reduced to 50 Oe for the in-plane regions and 1 kOe for the perpendicular regions, comparing to 4.5 kOe for the as-grown film. The perpendicular reversals were found to always originate at the pattern boundaries.