Sample preparation is often required before scanning electron microscope measurements can be performed. Cutting and polishing are common preparation techniques to remove surface roughness and to obtain a flat surface. Such traditional mechanical techniques apply shear forces to the sample, which result in surface artifacts like scratches, smearing, delamination and other damages at soft materials. All these issues are circumvented with the latest ion milling techniques developed by Hitachi High-Tech. These systems apply a broad low-energy Ar+ ion beam to sputter sample material from the sample and can be used both as cross section polisher and surface polisher. No mechanical stress is applied, which leaves extremely flat surfaces and cross sections without any artifacts.
♦ Dual milling configuration in a single instrument
♦ Cross-section milling rate of 1 mm/hour
♦ Cross-section widths up to 8 mm
The ion milling systems manufactured by Hitachi High-Tech apply a broad low-energy Ar+ ion beam to sputter sample material. Cryogenic ion milling (https://www.stinstruments.com/energy/cryogenic-ion-milling-of-a-fuel-cell-membrane-electrode-assembly-mea/) is even possible for heat sensitive samples to reduce damage by beam irradiation. Both systems, the IM4000Plus and the ArBlade5000 are hybrid models suitable for two different milling configurations: cross section milling and flat milling.
A mask is placed directly on top of the sample. This protects the top surface and provides a sharp edge to create a polished cross section by sputtering material away that is exposed beyond the edge of the mask.
The argon ion beam has a Gaussian-shaped current profile and material removal rate is therefore higher at the center of the beam than at the surrounding area. For this reason, the ion beam center is eccentric from the sample rotation center. As the sample rotation and swing center are varied with respect to the ion beam center, a wide area can be sputtered uniformly.
Conventional grinding and polishing techniques often generate flaws and artifacts such distorted structures, superficial scratching or smearing. Cross sections prepared by cleaving or mechanical methods often induce damage and result in distorted internal structures. The cross section polishers from Hitachi create cross sections without applying mechanical stress to the sample and enable analysis of sub-surface structures. Flat ion milling removes the upper most sample surface layer and can be utilized as a final process finishing to expose microstructures and crystal grain arrangements.
Relief ion milling VS. flat ion milling
Because of the Gaussian-shaped argon beam, it is possible to emphasize topographical information of composite materials (relief ion milling) or to reduce surface topography for enhanced crystal orientation visualization (flat ion milling) by adjusting the beam irradiation angle.
Flat ion milling at an oblique angle minimizes the dependence between sputtering rate and crystal orientation, yielding reduced surface topography and a flat sample surface. If the topography of composite materials is of interest, relief ion milling is applied. By sputtering perpendicular to the sample surface, convex and concave surfaces appear caused by compositional differences or grain orientations.
Electron backscatter diffraction (EBSD)
EBSD is a characterization technique used to study the crystal orientation and material phases within the sample. Within a SEM, the primary electron beam interacts with a tilted crystalline sample. Electron diffraction occurs and these electrons interact with a phosphor screen to become fluorescent. These signals are detected and a characteristic diffraction pattern is obtained. Slight variations in surface height change the angle of incidence of the electrons, thereby effecting diffraction patterns. For that reason, flat ion milling is typically utilized as sample preparation technique to obtain flat surfaces for EBSD measurements.
Even the inside from individual powder particles are revealed with cross section polishing. If a sufficient amount of powder is mixed with epoxy and cured, the new block can be cut and processed with the ion miller. In battery research, powder analysis is common practice. Catalysts and cathodes are analyzed to improve their performance. The following image shows hollow zirconium shells containing one active nanoparticle.
Hitachi High-Tech Europe GmbH, created in 2001 and part of the worldwide conglomerate Hitachi Group, provides a wide variety of scientific instruments. Their innovative R&D approach enables them to provide world-class solutions in the fields of materials sciences, life sciences and semiconductor.
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