XRD/XRR v. AFM for Film Thickness

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SUMMARY

The discussion evaluates the effectiveness of X-ray Reflectometry (XRR), Atomic Force Microscopy (AFM), and Scanning Electron Microscopy (SEM) for measuring the thickness of a wedge-shaped PZT sample layered with LSMO. The wedge varies from 50nm to 0nm across its length, and the AFM is recommended as the simplest method for obtaining thickness measurements, with a z-resolution of up to 0.5nm. XRR can provide reliable thickness and roughness values using the Parratt formalism, but requires careful beam constriction due to the sample's non-standard shape. SEM can also be utilized for cross-sectional analysis but involves more complex sample preparation.

PREREQUISITES
  • Understanding of X-ray Reflectometry (XRR) and its application in thin film analysis.
  • Familiarity with Atomic Force Microscopy (AFM) techniques and their resolution capabilities.
  • Knowledge of Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) for material characterization.
  • Basic principles of film thickness measurement and material layering.
NEXT STEPS
  • Research the Parratt formalism and its application in XRR for thin film analysis.
  • Learn about the operational principles and setup of Atomic Force Microscopes (AFM).
  • Explore the sample preparation techniques required for Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM).
  • Investigate methods for measuring film thickness in non-standard geometries using XRR and AFM.
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Researchers, material scientists, and engineers involved in thin film characterization, particularly those working with complex geometries and layered materials.

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Currently in our lab we have a WEDGE shaped sample that we would like to be able to know the thickness at various points along it. Our sample is about 5mm x 5mm. The wedge SHOULD extend from one side to the other. At the highest point, the wedge is 50nm, and then drops down, hopefully at a constant rate, to 0nm at the other side.

**Special Note**
The wedge is made of PZT and is between two layers of LSMO, with the layer on top of the wedge measuring a constant 5nm.

We were thinking about using the XRR/XRD to find the thickness, but I've recently been told to try the Atomic Force Microscope because of our unique shape, and even perhaps the Scanning Electron Microscope.

I have no personal experience using either the AFM or the SEM and have no idea how they would compare to using the XRR

Thoughts/ Concerns from the forum please.
 
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Hi,

I think all three of the techniques you mention could answer your question:

XRR: thickness interference fringes in XRR can be modeled with the Parratt formalism (e.g. using Parratt32.exe), and give very reliable thickness and roughness values (~0.1 nm precision for good data and fits). As your sample shape is non-standard, you would have to constrict your x-ray beam to ~0.1 mm sideways, so as to not sample the whole wedge but just a part of it. This is doable on a good reflectometer, but you sacrifice a lot of flux, which makes it challenging

AFM: I do not know what the abbreviations of your materials stand for, but if you can make a scratch down to the substrate you can scan the scratch then and (taking care to look beyond the bulge) extract film thickness. z-resolution should be up to 0.5 nm.

SEM / TEM: You could break your sample an look at the cross section. IN SEM one would expect a resolution of 10nm, TEM where sample preparation would be much more involved can get much more precise.

I would try AFM first (simplest), then XRR.
 

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