Metals and Alloys

Building the future with stronger, tougher, lighter and sustainable metals and alloys

Metals and alloys is a key research topic around most academic materials science programs. Imagine being able to engineer microstructure and thus enhance mechanical, thermal and electrical properties. You will be able to use precise control of the grain size, engineer grain boundaries and precipitates, control the presence of defects such as inclusions or voids. You will achieve remarkable improvements in the properties of traditional metals and alloys and thus create more useful materials.

Create understanding from macro- to nano

That is why detailed knowledge over multiple length scales is a prerequisite for metals researchers. Metals and alloys are characterized by features ranging from a macro- over micro- to nanoscales. Think of surface roughness, pits, cracks; grains with their different sizes, crystallographic orientations and morphologies; metals’ and alloys’ texture, twinning, voids, inclusions and precipitates at the 10 – 100 micrometer range; and ultimately nanoscale features such as dislocations, nano-precipitates, lattice defects, crack initiation sites or nano-crystalline grain features. All of them are important to understand – and this requires microscopic characterization techniques which cover all those length scales and seamlessly integrate multi-modal, multi-scale techniques.

Combine information from different modalities and scales

With ZEISS Research Microscopy Solutions you are enabled to capture all crucial details that are necessary to understanding metals and alloys and all mechanisms that contribute to strength, toughness and other properties. Take advantage of using light, X-ray and electron microscopes together with software tailored to multi-modal experiments. Make the most of correlative approaches. Combine information gathered from various modalities at different length scales and acquire comprehensive information for a given material system.

Schematic Overview

In the image below, click on the blue dots to enlarge each application image.

Surface Roughness
Surface Roughness

Laser polished surface of stainless steel test piece. 3D view of color-coded height map shows surface texture of areas with different process parameter.  Area imaged: 2x2 tiles, objective: C Epiplan-APOCHROMAT 10x/0.4. Acquired with ZEISS LSM 900 for materials.

Weld Characterization
Weld Characterization

Laser weld, coaxial brightfield illumination, objective: 1.6x, magnification: 32x acquired with ZEISS Smartzoom 5 digital microscope.

Failure Inspection
Failure Inspection
Grains and Phases
Grains and Phases

Cross-section of extruded aluminium alloy component, showing grain structure transverse to the extrusion direction. Dark field light micrograph taken using ZEISS Axio Imager Z2.

Non-metallic Inclusions
Non-metallic Inclusions
3D Void Mapping
3D Void Mapping
Particle Chemistry
Particle Chemistry
Diffraction Contrast Tomography
Diffraction Contrast Tomography

3D grain map of an armco iron sample with dimension of (diameter) 1.0 mm and (height) 3 mm. Sample scanned using helical phyllotaxis raster scheme. Sample courtesy of Prof. Burton R. Patterson, University of Florida, USA.

Nanotomography
Nanotomography

Macroscale Features

Understanding the interdependencies of macro-, micro- and nanostructure

Effectively characterize material at the macroscale and gain insights related to geometric defects, surface roughness, cracks, voids and inclusions. Use a combination of ZEISS light and X-ray microscopes (XRM). While light microscopy provides rapid information from the surface over a wide area, X-ray methods enable peering into the sub-surface non-destructively and deliver three-dimensional information on complex microstructural features. Generate a deep understanding of metals samples using light microscopy contrasts including brightfield, darkfield and polarization.

Capture the microstructural information in 3D in a single snapshot with ZEISS XRMs. 

  • Investigate new-age manufacturing methods, more precisely 3D printing materials, where structural parts with an ever-increasing structural complexity are being produced.  
  • Characterize specimens in 3D at the nanoscale and benefit from XRMs providing you with information on nanoprecipitates or eutectic microstructures. 
  • Unlock crystallographic secrets. Non-destructive 3D crystallographic grain characterization is possible with advances in diffraction contrast tomography delivering information on grain size, crystallographic orientation and morphology.

Investigate macroscale surface features

Light microscopy image of a pure magnesium sample using polarization contrast shows the structural anisotropy.

Polarization contrast light microscopy image from a Barker etched anodized AlNi3.5 sample.

Ferrite and pearlte phase in steel imaged using light microsopy and quantitatively analyzed.

Location of a single profile across root of autogenous TIG weld in corrosion-resistant nickel alloy (Hastelloy® C-276).

Laser polished surface of stainless steel test piece. 3D view of color-coded height map shows surface texture of areas with different process parameter.

Gain deeper insights non-destructively and in 3D on micro- and nanoscale features

Non-destructive 3D rendering of crack networks formed due to corrosion fatigue in the shank section of a load bearing steel bolt.

3D grain map of an Al-Cu sample with gauge section dimension of (length) 1.25 mm, (width) 1.0 mm and (thickness) 0.5 mm. Sample scanned using helical phyllotaxis HART. Sample courtesy of Prof. Masakazu Kobayashi, Toyohashi University of Technology, Japan.

3D volumetric rendering of sintered CoCr particles. The consolidated bulk after sintering and portions of unsintered powder can be observed.

3D rendering of a reconstructed nanoscale X-ray tomography dataset obtained from a Zn-Mg spiral eutectic sample.

From Micro- to Nanoscale

Comprehensive characterization with a scanning electron microscope

Think of the possibilities it would open if you found a solution to characterize materials from micro- to nanometer with one instrument. You would be able to set up a workflow for root cause analysis enabling you to study the relationship between microstructure and fracture resistance or understand structural failures of critical parts. You could determine fracture modes and analyze crack propagation. What if you could analyze the chemical composition of precipitates and inclusions in detail over multiple length scales; describe grain characteristics including size, crystal orientation, shape, boundaries, and phase distribution; understand deformation behavior of metals and alloys? And, finally, modify the materials processing route and chemistries and fine tune their properties and performance? In fact, scanning electron microscopes (SEM) and their accessories have become an integral part of the materials characterization workflow. To many researchers the SEM is the go-to instrument, the “Swiss-knife“. 

Assess Grain Characteristics and Deformation Behavior

Investigate grains, inclusions or precipitates, gain essential information on morphology and qualitative and quantitative chemical composition of metals and alloys, and understand their fracture properties. 

  • Energy dispersive X-ray spectroscopes (EDS) enable you to understand chemical makeup and elemental distributions. 
  • Measure grain size and shape, crystallographic orientation, texture, and grain boundary character distribution over scales from a few micrometers down to 10 nm using electron backscattered diffraction (EBSD). 
  • Use electron channeling along crystal planes and apply electron channeling contrast imaging (ECCI) letting you observe and quantify lattice defects directly. 
  • Identify dislocations and stacking faults within grains and describe their location with respect to grain boundaries and orientations. 
  • Combine ECCI with in situ deformation or heating experiments of metal samples to observe the formation of dislocation networks under the influence of mechanical loads. 
EDS mapping of a conspicuous mixed inclusion. The core of the mixed inclusion consists of the "typical" inclusion types MnS (red) and Al2O3 (blue) whereas the surrounding bright phase contains the elements Bi (yellow) and P (green).

Combine a variety of imaging modalities with analytical capabilities using an SEM. Readily obtain critical information on the topography and morphology, on micro- and nanostructure, on the chemical makeup, crystallographic and phase identification. Easily discern crystal defects, orientations, and sub-grain information such as twinning and slip band formations. Use a highly sophisticated electron optical column designed for high resolution, surface sensitive imaging and capable of performing powerful analytics.

  • For the characterization of surface fractures at micro- and nanoscales take advantage of gaining unique information from secondary and backscatter electron detectors that deliver exceptional topographical and compositional contrasts.  
  • Expand the imaging capabilities of your SEM with an in situ lab: link microstructure to performance and observe metals during deformation and heating. 

High-resolution, high-contrast imaging aids microstructural observations

Scanning electron microscopy (SEM) delivers extremely high contrasts of crystal orientations and defects in the high temperature alloy TiAl₂.

Advanced alloy material 3kV HV mode. This advanced alloy material reveals a tungsten core material surrounded by a steel matrix when imaged with Inlens SE detector at low voltage.

Metal fracture acquired with ZEISS Sigma, Inlens SE detector, field of view 125µm.

Tensile testing of irradiation effects on the mechanical behavior of pure nickel. A. Reichardt et al. / Acta Materialia 100 (2015) 147–154.

High resolution surface characterization of metal powders. Scanning electron microscopy image of stellite powder for additive manufacturing. 

Broaden opportunities at the Mesoscale

Machine nano-, micro- or meso-scale structures and enhance high-resolution sub-surface microstructural characterization

Investigating metals and alloys down to the level of individual atomic arrangements while keeping the full context over a scale of millimeters is critical. Only the combination of both, overview over millimeter- and detailed insight into micro- or nanometer-scaled areas, enables you to understand the linkage between structure and properties. This is the point where it becomes necessary to add the meso-scale to your workflow. When you seek to understand properties at the nanoscale, when you want to prepare minute devices like atom probe tips or ultra-thin TEM lamellae, when it is your objective to precisely target a unique void, a precipitate located along a certain grain boundary, or the region around a crack tip you will need a precision tool that is tailored for advanced imaging and sample manipulation. Site-specific characterization below the surface plus fast and precise material removal combined with high resolution imaging and a seamless workflow is what you need. 
 
ZEISS FIB-SEMs (focused ion beam scanning electron microscopes) unite the high resolution imaging ability of an SEM with the ability to prepare samples.  

  • Perform precise serial milling or sectioning to reveal the sub-surface features or produce 3D nanotomography datasets.  
  • Access the meso-scale regime by equipping your ZEISS FIB-SEM with a device tailored for massive material ablation or for the preparation of extremely large sections, a femto-second laser.  
  • Combining this LaserFIB from ZEISS with EDS or EBSD, allows for 3D multi-modal nanotomography, giving you the best of sample preparation at high throughput, and advanced imaging and analytics – an extremely powerful combination for the investigation of grains, precipitates, fractures, corrosion, or thermal and electrical properties. 

Rapidly produce samples to characterize metals and alloys from meso- to nano scale

Laser prepared cube in a tungsten carbide cobalt hard metal sample (WCoC). The cube has side walls of 180 µm length and is 120 µm tall. Laser machining time 85 s. FOV 696 µm. ZEISS Crossbeam 350 laser, SESI detector, 5 kV. 

Laser polished sample surfaces produce satisfactory EBSD grain maps without the need for Ga-FIB polishing steps in cases where a quick overview of a large area of the sample is sufficient. 

Multi-site lamella preparation of a 3 x 2 array of laser- machined chunks followed by FIB millingfor precise thinning to produce a < 2 µm TEM lamella.

High resolution serial section FIB-SEM tomography (8 nm/voxel) from a correlative microscopy experiment to study the process of intergranular corrosion observed in a magnesium alloy. Sample courtesy of the University of Manchester.

3D FIB-SEM tomography data on the precipitate distribution in aluminum 7075 alloy. The 3D data provides quantitative information on the spatial distribution of precipitates with respect to the grain boundaries. Sample courtesy of Prof. N. Chawla, Purdue University.

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