Leica Science Lab - Tag : Ion Beam Milling https://www.leica-microsystems.com//science-lab/tag/tags/ion-beam-milling/show/Tag/ Article tagged with Ion Beam Milling en-US https://www.leica-microsystems.com/20352 EM Sample Preparation Macroscale to Nanoscale Pore Analysis of Shale and Carbonate Rocks Physical porosity in rocks, like shale and carbonate, has a large effect on the their storage capacity. The pore geometries also affect their permeability. Imaging the visible pore space provides insights into the physical pore space, pore geometries, and the associated mineral and organic matter phases relevant for storage and transport. For example, organic-matter porosity is an important property of mature organic-rich shales providing storage capacity for liquids and gases, like hydrocarbons. Imaging the microstructure is the only technique which delivers data giving direct insight into the organic matter porosity. However, imaging porosity in fine-grained shale as well as carbonate rocks in a representative way at high resolution is challenging. https://www.leica-microsystems.com//science-lab/macroscale-to-nanoscale-pore-analysis-of-shale-and-carbonate-rocks/ Tue, 04 Sep 2018 22:00:00 +0000 PhD Jop Klaver, PhD Joyce Schmatz, MSc Mingze Jiang, PhD James DeRose https://www.leica-microsystems.com/18221 EM Sample Preparation Contrast Enhancement of Polycrystalline Metals - Sample Preparation for SEM Application Note - Ion milling is a perfect alternative for chemical etching, especially for polycrystalline metals, such as copper. Ion milling can be used to increase the contrast of the grain structure and their interfaces. In contrast to chemical etching the milling process is clean, safe and easy to operate. Ion energy and milling time depend on the milling rate of the metal. https://www.leica-microsystems.com//science-lab/contrast-enhancement-of-polycrystalline-metals-sample-preparation-for-sem/ Wed, 01 Feb 2017 10:33:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18156 EM Sample Preparation Cross Sectioning of Cadmiumsulphide (CdS) for Cathodoluminescence Cathodoluminescence can be used to achieve spectra and high resolution images of impurity and structural defects in semicondoctors, minerals and insulating materials. This application note explains how to prepare a perfect sample surface for carhodoluminescence and how to use ion beam slope cutting to prepare the sample surface free of any preparation artefacts. https://www.leica-microsystems.com//science-lab/cross-sectioning-of-cadmiumsulphide-cds-for-cathodoluminescence/ Tue, 24 Jan 2017 18:12:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18196 EM Sample Preparation Cross Sectioning of Copper for Electron Backscattered Diffraction (EBSD) Application Note for Leica EM TIC 3X - Electron Backscattered Diffraction (EBSD) is a surface technique creating diffraction patterns (Kikuchi-bands). It can be used for crystal orientation mapping, defect studies, phase identification, grain boundary studies and morphological studies. The information depth is just a few nm, therefore good sample preparation is very important to avoid damages. https://www.leica-microsystems.com//science-lab/cross-sectioning-of-copper-for-electron-backscattered-diffraction-ebsd/ Thu, 19 Jan 2017 16:37:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18249 EM Sample Preparation Removal of Surface Layers - Sample Preparation for SEM and TEM Application Note for Leica EM RES102 - Sometimes it is necessary to remove surface layers to gain access to the real surface structure. That can be a native oxide, or layers coming from the preparation process itself, like re-deposition. Depending on the layers thickness and the energy used for the cleaning process, it takes between a few seconds and half an hour. The energy depends on the milling rate of the material. https://www.leica-microsystems.com//science-lab/removal-of-surface-layers-sample-preparation-for-sem-and-tem/ Wed, 11 Jan 2017 10:10:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18243 EM Sample Preparation Multilayer Systems with Widely Different Sputter Rates - Sample Preparation for TEM Application Note for Leica EM RES102 - The multi-layer system to be prepared in cross-section consists of a Si substrate, a TiN layer with a thickness of a few nm and a 500 nm W layer. All these components have extreme differences in their hardness, their atomic weight and in their sputter rates. A preparation of this kind of samples with sample rotation would lead to a wall overlying the area of the layers. https://www.leica-microsystems.com//science-lab/multilayer-systems-with-widely-different-sputter-rates-sample-preparation-for-tem/ Fri, 16 Dec 2016 16:57:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18225 EM Sample Preparation In-Containing Compound Semiconductors - Sample Preparation for TEM Application Note for Leica EM RES102 - Previous studies showed that surface accumulation of In occurs when InP was milled in a conventional way with Ar ions. The consequence is In islands on the sample surface. This leads to low quality of TEM samples. To remove these islands, reactive ion milling with iodine ions (RIBE / CAIBE) can be used. This method has the disadvantage of polluting the ion guns and the vacuum system of the ion milling device and leads to chemical reactions with the sample material. To avoid these problems we prepared these samples very gently with low energy Ar ions. https://www.leica-microsystems.com//science-lab/in-containing-compound-semiconductors-sample-preparation-for-tem/ Mon, 12 Dec 2016 10:13:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18255 EM Sample Preparation "Shallow Trench Isolation" Structures - Sample Preparation for TEM Application Note for Leica EM RES102 - The cross-sectional preparation of structured semiconductor materials requires a very thorough mechanical pre-preparation. In doing this, it must be ensured that the structure of interest should be located as close to the centre of the sample as possible. As the sample will be ion milled from both sides, a specific preparation of the structure is necessary in most cases, which means that you must thin these structures from both sides. https://www.leica-microsystems.com//science-lab/shallow-trench-isolation-structures-sample-preparation-for-tem/ Fri, 18 Nov 2016 16:50:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18241 EM Sample Preparation Metal Films and Sheets - Sample Preparation for TEM Application Note for Leica EM RES102 - Most metal films already have a thickness that requires no further mechanical pre-preparation. Frequently, however, they are also domed, which can lead to undefined milling angles. This is a disadvantage, particularly for films that contain inclusions, and that therefore mostly require very flat milling angles. Metal sheets are thicker than 100 µm. Mechanical pre-preparation is necessary to obtain an acceptable initial thickness and a good surface quality for ion milling. https://www.leica-microsystems.com//science-lab/metal-films-and-sheets-sample-preparation-for-tem/ Wed, 16 Nov 2016 13:32:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18213 EM Sample Preparation Cross-Sectional Preparation of Structured Semiconductor Materials for TEM Application Note for Leica EM RES102 - The vertical layer construction of a semiconductor structure should be examined as a TEM cross-sectional sample. In addition to the specific preparation of the desired structure, the widely different sputter rates and atomic weights of the individual components represent the level of difficulty involved with this preparation problem. https://www.leica-microsystems.com//science-lab/cross-sectional-preparation-of-structured-semiconductor-materials-for-tem/ Mon, 31 Oct 2016 08:15:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18235 EM Sample Preparation Contrast Enhancement of Polished Cross Sections of Semiconductor Structures - Sample Preparation for SEM Application Note for Leica EM RES102 - The surfaces of polished cross sections often show fine scratches and residues of the removed material or of the abrasive material. The artefacts are strongly material-dependent, and are mostly only detectable at higher resolutions in the scanning electron microscope. A further problem arises from the fact that the ground section mostly only has low contrast, i.e., in the structures of the semiconductor materials are very difficult to discern. With the use of ion beam milling, the ground sections of semiconductor structures can be "contrasted". https://www.leica-microsystems.com//science-lab/contrast-enhancement-of-polished-cross-sections-of-semiconductor-structures-sample-preparation-for-sem/ Fri, 28 Oct 2016 12:08:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18257 EM Sample Preparation Surface Modification of ZnAg Sample - Sample Preparation for SEM Application Note for Leica EM RES102 - By means of cleaning, polishing and contrast enhancement a soft ZnAg sample should be prepared to obtain information concerning the grain structure and interfaces of the sample. The sample is contaminated after mechanical polishing. There are still some scratches on the surface. Grain structure is almost invisible. https://www.leica-microsystems.com//science-lab/surface-modification-of-znag-sample-sample-preparation-for-sem/ Mon, 17 Oct 2016 08:16:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18364 EM Sample Preparation Cross Sectioning of Ni/Cu on Steel for EBSD Application Note for Leica EM TIC 3X - Electron Backscattered Diffraction (EBSD) is a surface technique creating a diffraction pattern (Kikuchi-bands). It can be used for crystal orientation mapping, defect studies, phase identification, grain boundary studies and morphology studies. The information depth is just a few nm. Therefore a good sample preparation is very important. https://www.leica-microsystems.com//science-lab/cross-sectioning-of-nicu-on-steel-for-ebsd/ Fri, 14 Oct 2016 09:45:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18259 EM Sample Preparation Thin Metal Foils with Coatings - Sample Preparation for SEM Application Note for Leica EM RES102 - Thin foils are mostly unstable because of their thickness of a few microns. This makes it difficult to do slope cutting without any protection of the sample. A common realisation to protect the sample surface is by sticking a cover glass on top of the sample. Another issue is cutting the foils before ion milling. The sample edge should be flat and sharp without any broken areas. A razor blade is mostly the best solution. A protected sample can salso be sawed with a wire saw. https://www.leica-microsystems.com//science-lab/thin-metal-foils-with-coatings-sample-preparation-for-sem/ Wed, 05 Oct 2016 07:16:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18344 EM Sample Preparation Cross Section of an Aluminium Sample for Electron Backscattered Diffraction (EBSD) Application Note for Leica EM TIC020, Leica EM TIC 3X - Electron backscattered diffraction (EBSD) is for example used to examine the crystallographic orientation of material. The sample preparation for such samples is sometimes very tricky as the depth of information is just few nm (~20nm or less). That means the sample surface must be flat and free of preparation artefacts. Mechanical polishing leads mostly to sample surfaces damages. https://www.leica-microsystems.com//science-lab/cross-section-of-an-aluminium-sample-for-electron-backscattered-diffraction-ebsd/ Thu, 15 Sep 2016 07:54:00 +0000 Robert Ranner https://www.leica-microsystems.com/18239 EM Sample Preparation Ion Beam Polishing of Sample Surfaces - Sample Preparation for SEM Application Note for Leica EM RES102 - Ion milling can be used to reduce the roughness of sample surfaces. Small angles less than 6° with respect to the sample surface are necessary. The high voltage depends on the material to be prepared. The reason for the levelling effect is the different milling angle of flat and rough surface areas. The milling rate is lower for small angles. The rough surface area will be faster milled. Ion polishing is often the final step of sample preparation. The prerequisite is a perfect mechanical prepreparation as samples with deep surface scratches cannot be ion polished. Soft materials usually have a smeared sample surface after mechanical polishing. It is necessary to remove this smeared material before ion polishing. Otherwise the above mentioned polishing effect does not work. https://www.leica-microsystems.com//science-lab/ion-beam-polishing-of-sample-surfaces-sample-preparation-for-sem/ Tue, 06 Sep 2016 11:11:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18215 EM Sample Preparation Cleaning of Smeared Sample Surfaces - Sample Preparation for SEM Application Note for Leica EM RES102 - Mechanical polishing of soft materials or hard / soft material combinations is tricky. The mechanical polishing process leads very often to smearing of the soft material. The smeared material covers the surface and fills small pores or holes. Grain structures, interfaces and other structural details can be masked. An additional ion milling step with milling angles between 10° C and 15° C with respect to the sample surface can remove or reduce the contamination. https://www.leica-microsystems.com//science-lab/cleaning-of-smeared-sample-surfaces-sample-preparation-for-sem/ Fri, 02 Sep 2016 06:49:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18209 EM Sample Preparation Ceramics - Sample Preparation for TEM Application Note for Leica EM RES102 - Ceramic samples are mostly very brittle, and are therefore very difficult to thin mechanically to a low starting thickness for ion beam milling. The ion beam milling of insulators often leads to static charging of the surface of the sample. This, in turn, reduces the sputter rate. When using the Ti standard holder (standard TEM holder), however, sufficient secondary electrons are created by the ion beam also falling on the sample holder to largely compensate for the static charging. https://www.leica-microsystems.com//science-lab/ceramics-sample-preparation-for-tem/ Mon, 15 Aug 2016 18:46:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/18368 EM Sample Preparation Cross Sectioning of Oil Shale Rock Application Note for Leica TIC 3X - High quality sample preparation of large area to investigate the sample in the SEM. For the mechanical preparation step diamond lapping foils of 9μm subsequently 2μm and finally 0.5μm grain size were used. It took about 1.5 hours. The sample was removed from the stub with a razor blade after TXP processing and fixed onto the holder of the rotary stage of the Leica EM TIC 3X. https://www.leica-microsystems.com//science-lab/cross-sectioning-of-oil-shale-rock/ Tue, 28 Jun 2016 13:04:00 +0000 Robert Ranner https://www.leica-microsystems.com/17971 EM Sample Preparation Cross Sectioning of Basalt Fibres Application Note for Leica EM TIC 3X - Material Research. Purpose: The fibres are embedded in a soft matrix. That makes it difficult to prepare a cross section. Goal: Cross section of the basalt fibres. https://www.leica-microsystems.com//science-lab/cross-sectioning-of-basalt-fibres/ Fri, 20 May 2016 15:31:00 +0000 PhD Wolfgang Grünewald https://www.leica-microsystems.com/17377 EM Sample Preparation Triple-beam Ar-Ion-Milling with a Rotary Stage to Decorate Grain Boundaries and Substructures in Rock Salt Decoration of grain boundaries in polycrystalline rocks has a long tradition in Structural Geology as in a monomineralic rock the recrystallized grain size is a good indicator for the paleostress conditions. Understanding the mechanical properties of rock salt and its deformation behavior is of major importance for the prediction of long-term stability of nuclear waste repositories, and our understanding of the dynamics of salt-related sedimentary basins which host the majority of oil and gas accumulations on Earth. https://www.leica-microsystems.com//science-lab/triple-beam-ar-ion-milling-with-a-rotary-stage-to-decorate-grain-boundaries-and-substructures-in-rock-salt/ Thu, 03 Mar 2016 11:01:00 +0000 PhD Joyce Schmatz, PhD Oliver Schenk, PhD Jop Klaver, PhD Janos Urai, PhD Wolfgang Grünewald https://www.leica-microsystems.com/16804 EM Sample Preparation Electron Microscopy Sample Preparation: “The Future is Cold, Dynamic and Hybrid” In 2014, the renowned Electron Microscopy for Materials Science (EMAT) research lab at the University Antwerp, Belgium, and Leica Microsystems started a fruitful collaboration to establish a Leica Reference Site in Antwerp. This site, officially opened in July 2014, is dedicated to specimen preparation for electron microscopy in materials science with a special focus on ion beam milling and recently also on carbon coating. In this interview Prof Gustaf van Tendeloo, Director of EMAT, and Frédéric Leroux, TEM specimen preparation specialist, talk about research topics at EMAT, how the Leica reference site has evolved, and future trends for EM sample preparation. https://www.leica-microsystems.com//science-lab/electron-microscopy-sample-preparation-the-future-is-cold-dynamic-and-hybrid/ Thu, 22 Oct 2015 19:22:00 +0000 Prof. Gustaaf (Staf) Van Tendeloo, PhD Frédéric Leroux, Florence Hauger https://www.leica-microsystems.com/15930 EM Sample Preparation High Quality Sample Preparation for EBSD Analysis by Broad Ion Beam Milling Electron Backscatter Diffraction technique (EBSD) is known as a "surface" technique because electron diffraction is generated within a few tens of nanometers of the sample surface. Therefore, the specimen surface should be exempt of any damages in order to produce EBSD patterns. Here, we present a successful and efficient EBSD sample polishing of two very challenging specimens prepared by broad ion beam milling. https://www.leica-microsystems.com//science-lab/high-quality-sample-preparation-for-ebsd-analysis-by-broad-ion-beam-milling/ Fri, 12 Jun 2015 20:30:00 +0000 PhD Laurie Palasse, PhD Wolfgang Grünewald https://www.leica-microsystems.com/11027 EM Sample Preparation Neuroscience Focussed Ion Beam Milling and Scanning Electron Microscopy of Brain Tissue This protocol describes how biological samples, like brain tissue, can be imaged in three dimensions using the focussed ion beam/scanning electron microscope (FIB/SEM). The samples are fixed with aldehydes, heavy metal stained using osmium tetroxide and uranyl acetate. They are then dehydrated with alcohol and infiltrated with resin, which is then hardened. https://www.leica-microsystems.com//science-lab/focussed-ion-beam-milling-and-scanning-electron-microscopy-of-brain-tissue/ Wed, 06 Jul 2011 16:17:00 +0000