Graduation Year

2016

Document Type

Thesis

Degree

Ph.D.

Degree Name

Doctor of Philosophy (Ph.D.)

Degree Granting Department

Mechanical Engineering

Major Professor

Wenjun Cai, Ph.D.

Committee Member

Alex A. Volinsky, Ph.D.

Committee Member

Delcie Durham, Ph.D.

Committee Member

Jing Wang, Ph.D.

Committee Member

Andreas Muller, Ph.D.

Keywords

Nanotechnology, Nanoindentation, Residual stress, Wear, TEM

Abstract

Nanostructured metallic multilayers (NMMs) are well-known for their high strength in smaller bilayer thicknesses. Six Al/Ti (NMM) with different individual layer thickness were tested for their mechanical hardness using a nanoindentation tool. Individual layer thicknesses were chosen carefully to cover the whole confined layer slip (CLS) model. Nano-hardness had a reverse relation with the square root of individual layer thickness and reached a steady state at ~ 5 nm bilayer thickness. Decreasing the layer bilayer thickness from ~ 104 nm to ~ 5 nm, improved the mechanical hardness up to ~ 101%. Residual stresses were measured using grazing incident X-ray diffraction (GIXRD). Effect of residual stress on atomic structure and dislocation propagation was then investigated by comparing the amount and type of stresses in both aluminum and titanium phases. Based on the gathered data from GIXRD scans tensile stress in Ti phases, and compressive stress in Al would increase the overall coherency of structure.

Wear rate in coatings is highly dependent on design and architect of the structure. NMM coatings are known to have much better wear resistance compare to their monolithic constituent phases by introducing a reciprocal architect. In current study wear rate of two Al/Ti NMMs with individual layer thicknesses of ~ 2.5 nm and ~ 30 nm were examined under normal loads of 30 µN, 60 µN, and 93 µN. Wears strokes were performed in various cycles of 1, 2, 3, 4 5 and 10. Wear rates were then calculated by comparing the 3D imaging of sample topology before and after tests. Nano-hardness of samples was measured pre and post each cycle of wear using a nanoindentation tool. The microstructure of samples below the worn surface was then characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), focus ion beam (FIB) and an optical profilometer. Orientation mapping was performed to analyze the microstructure of layers beneath the nano indents. TEM imaging from the cross section of worn samples indicated severely plastically deformed layer (SPDL) below the worn surface. Shear bands and twins are visible after wear and below the worn surface. Decreasing the layer thickness from 30 nm to 2.5 nm resulted in ~ 5 time’s better wear resistance. Nanowear caused surface hardening which consequently increased nano hardness up to ~ 30% in the sample with 2.5 nm individual layer thickness.

Increasing the interfaces density of NMMs will significantly improve the corrosion resistance of coating. Reciprocal layers and consequently interfaces will block the path of aggressive content toward the substrate. Corrosion rate evolution of Al/Ti multilayers was investigated through DC corrosion potentiodynamic test. Results seem to be very promising and demonstrate up to 30 times better corrosion resistance compared to conventional sputtered monolithic aluminum. Corrosion started in the form of pitting and then transformed to the localized galvanic corrosion. Decreasing the bilayer thickness from ~ 10.4 nm to ~ 5 nm will decrease the corrosion current density (icorr) of ~ 5.42 × 10-7 (A/cm2) to ~ 6.11 × 10-10 (A/cm2). No sign of corrosion has been seen in the sample with ~ 2.5 nm individual layer thickness. Further AFM and TEM analysis from surface and cross section of NMMs indicate that a more coherent layer by layer structure improves the corrosion rate. Interfaces have a significant role in blocking the pores and imperfections inside coating.

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