Corrosion is a degradation process by which materials react with their environment. Corrosion causes the formation of oxide scale which can reduce the mechanical, thermal, or electrical properties of materials, especially metallic materials. Ebatco’s NAT Lab can analyze the surface and cross section of oxides formed on samples along with determining their microstructure. We can identify the function and distribution of alloying elements within materials and determine the effectiveness of protective coatings. Our expertise enables us to measure coating properties such as thickness, wear resistance, hardness, etc. and analyze the interactions that occur at coating and substrate interfaces.
Typical Experimental Results
SEM image of a failed Ti-6Al-4V rod possessing a Titanium-Vanadium coating.
Optical microscopy image of a case hardened metal fastener.
SEM/EDS image of a corroded Ti-6Al-4V dental implant’s surface.
Applications
Alloys | Chemical Etching | Case Hardening | Carburization | Corrosion Analysis |
Cross-Section Analysis | Crystal Structures | Element Identification | Failure Analysis | Foreign Material Identification |
Forensic Analysis | Fractography | Fracture Study | Grains | Grain Boundaries |
Grain Growth | Grain Orientation | Grain Size | Grain Structure | IC Failure Analysis |
Materials | Metals | Metallography | Metallurgy | Microscopy |
Microstructure | Phase Diagram | Penetration Depth | Spectroscopy | Steels |
For more information please read our application notes:
Compression Fracture of a Pellet Press Shaft, PDF
Identify Unknown Materials and Coating by Energy Dispersive Spectrum
Tensile Fracture Failure Mechanisms of 316L Stainless Steel
Instruments: JEOL 6610 LV Scanning Electron Microscope
Key Specifications
Filament | W hairpin filament |
Resolution | High Vacuum: 3nm (30kV), 8nm (3kV), 15nm (1kV) Low Vacuum: 4 nm (30kV) |
Accelerating Voltage | 300 V to 30 kV |
Magnification | 5x to 300,000x |
LV Detector | Multi-segment BSED |
LV Pressure | 10 to 270 Pa |
Sample Sizes | Height: 80mm; Width: 178 mm |
Stage | Eucentric 5 axis motor control, asynchronous movement, x-y: 125mm-110mm, z: 5mm-8mm, tilt:-10 to 90 degrees, rotation: 360 degrees |
Resolution | 5120 x 3840 pixels |
Condenser Lens | Zoom condenser lens |
Objective Lens | Conical objective lens |
Compression Fracture of a Pellet Press Shaft
When parts break unexpectedly, determining the root cause is an important step in avoiding future problems. SEM fractography and composition mapping are excellent ways to determine the reasons behind part failures. In this study, a shaft from a pellet press was examined after breaing during routine use. Figure 1 shows the broken shaft compared to an intact shaft. The shaft broke into seven fragments and there was a small black hole at the top center of the shaft. The head of the shaft had a small protrusion which fit into the hole. The shaft was likely connected to the head by a welding or brazing process.
Figure 1. Intact (left) and fractured (right) pellet press shafts.
The composition of the shaft was analyzed by X-ray energy dispersive spectroscopy (EDS), the results of which are shown in Figure 2. The EDS spectrum indicates that the shaft was primarily composed of Fe, Cr, W, Mo and V, which are the most common elements used to create tool steels. The bright particles in the SEM image are W, Mo and V carbide particles added to limit the growth of cracks in the alloy and increase the mechanical strength of the material.
Figure 2. EDS spectrum of the fracture surface of the shaft. Inset: SEM image of the corresponding area.
The microstructure of the compression fracture surface was investigated further using SEM (Figure 3). Figure 3a is the SEM image of fragment 5 from Figure 1. In fragment 5, chevron marks, or small lines which converge at the crack origination site. Chevron marks were not only observed in fragment 5, but also in fragments 1, 3, and 4. By tracing the chevron marks back, the fracture on fragment 5 originated from the bottom of the hole (red circle, Figure 3a). This location corresponds to the joint area between the shaft and the head, which is an area of high stress concentration. For this shaft fragment, several cracks initiated at the joint area, and the top part of the shaft broke into five pieces. After the crack initiated, the crack propagated downward at approximately 45º, which is the direction of highest shear stress. This also explains why fragment 2 had two slopes at about 45º angles (not shown).
A typical microstructure of the fracture surface at 2000X magnification is shown in Figure 3b. Pieces 1 through 5 and the lower shaft had similar uneven and dimpled fracture surfaces, characteristic of ductile fracture. Some carbide particles were also found at the base of these dimples. The top view of the lower shafts’ fracture surface is shown in Figure 3c. Three unique areas were identified and labeled as zones 1, 2, and 3. Zone 1’s fracture surface has a cliff shape (Figure 3d). As shown in Figures 3c and 3d, cleavage lines formed on the fracture surface, demonstrating the growth direction of the cracks. Reassembling the fragments, fragment 2 fitted into zone 1, fragments 1 and 3 fitted into zone 2, and fragments 4 and 5 fitted into zone 3. The slopes on the fragments demonstrated that the cracks grew due to shear stress.
Figure 3. Fracture surface microstructures. a) SEM image of fragment 5, b) Typical microstructure of the fracture surface at 2000x, c) Top view of the fracture surface on the lower shaft, d) Zone 1 fracture surface.
Based on morphological analysis, the fracture was identified as a ductile compression fracture. The cracks initiated at the joint area between the shaft and the head, and grew along the highest shear stress direction. The size and distribution of the carbide particles were homogenous. No large carbide segregation was observed at the critical areas. The failure of the shaft was due to an overload of compressive force.
ASTM Number | Title | Website Link |
A262 – 15 | Standard Practices for Detecting Susceptibility to Intergranular Attack in Austenitic Stainless Steels | Link |
A763 – 93(2009) | Standard Practices for Detecting Susceptibility to Intergranular Attack in Ferritic Stainless Steels | Link |
A802 – 95(2015) | Standard Practice for Steel Castings, Surface Acceptance Standards, Visual Examination | Link |
B487 – 85(2013) | Standard Test Method for Measurement of Metal and Oxide Coating Thickness by Microscopical Examination of Cross Section | Link |
B578 – 87(2015) | Standard Test Method for Microhardness of Electroplated Coatings | Link |
B748 – 90(2016) | Standard Test Method for Measurement of Thickness of Metallic Coatings by Measurement of Cross Section with a Scanning Electron Microscope | Link |
E1077 – 01(2005) | Standard Test Methods for Estimating the Depth of Decarburization of Steel Specimens | Link |
E1508 – 98(2008) | Standard Guide for Quantitative Analysis by Energy-Dispersive Spectroscopy | Link |
E3 – 01(2007)e1 | Standard Guide for Preparation of Metallographic Specimens | Link |
E340 – 00(2006) | Standard Test Method for Macroetching Metals and Alloys | Link |
E381 – 01(2012) | Standard Method of Macroetch Testing Steel Bars, Billets, Blooms, and Forgings | Link |
E384 – 09 | Standard Test Method for Microindentation Hardness of Materials | Link |
E384 – 10e2 | Standard Test Method for Knoop and Vickers Hardness of Materials | Link |
E407 – 07(2015)e1 | Standard Practice for Microetching Metals and Alloys | Link |
E407 – 07(2015)e1 | Standard Practice for Microetching Metals and Alloys | Link |
E7 – 03(2009) | Standard Terminology Relating to Metallography | Link |
F2328 – 17 | Standard Test Method for Determining Decarburization and Carburization in Hardened and Tempered Threaded Steel Bolts, Screws, Studs, and Nuts | Link |
ISO |
Title | Link |
9220:1988 |
Metallic coatings — Measurement of coating thickness — Scanning electron microscope method | |
5949:1983 |
Tool steels and bearing steels — Micrographic method for assessing the distribution of carbides using reference photomicrographs | |
4499-4:2016 |
Hardmetals — Metallographic determination of microstructure — Part 4: Characterisation of porosity, carbon defects and eta-phase content | |
4499-1:2008 |
Hardmetals — Metallographic determination of microstructure — Part 1: Photomicrographs and description | |
3887:2017 |
Steels — Determination of the depth of decarburization | |
26146:2012 |
Corrosion of metals and alloys — Method for metallographic examination of samples after exposure to high-temperature corrosive environments | |
18203:2016 |
Steel — Determination of the thickness of surface-hardened layers | |
11845:1995 |
Corrosion of metals and alloys — General principles for corrosion testing | |
11463:1995 |
Corrosion of metals and alloys — Evaluation of pitting corrosion | |
10271:2011 | Dentistry — Corrosion test methods for metallic materials |