XRD/XRR v. AFM for Film Thickness

In summary, the lab has a WEDGE shaped sample that measures 5mm x 5mm and is made of PZT with two layers of LSMO on top. The thickness of the wedge ranges from 50nm at the highest point to 0nm at the other side. The forum suggests using either XRR/XRD, Atomic Force Microscope, or Scanning Electron Microscope to find the thickness. XRR can give precise thickness and roughness values, but it requires constricting the x-ray beam. AFM can also provide thickness measurements with a resolution of 0.5 nm, while SEM offers a resolution of 10nm but requires breaking the sample. The recommendation is to try AFM first and then
  • #1
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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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  • #2
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.
 

What is the difference between XRD/XRR and AFM for film thickness measurement?

XRD/XRR (X-ray diffraction/reflectivity) is a technique that uses X-rays to measure the thickness of thin films on a substrate. It provides information on both the thickness and crystal structure of the film. On the other hand, AFM (atomic force microscopy) uses a small probe to scan the surface of a film to measure its thickness and topography. While XRD/XRR is a non-destructive technique, AFM requires contact with the film surface and can potentially damage it.

Which technique is more accurate for film thickness measurement?

The accuracy of both XRD/XRR and AFM depends on various factors such as sample preparation, instrument calibration, and operator skill. However, in general, XRD/XRR has a higher accuracy for thin films in the range of a few nanometers to micrometers. AFM, on the other hand, can provide higher resolution for very thin films (less than 10 nanometers).

Can XRD/XRR and AFM be used together for film thickness measurement?

Yes, XRD/XRR and AFM can be complementary techniques for film thickness measurement. XRD/XRR provides information on the overall film thickness and structure, while AFM can provide local variations in thickness and topography. Using both techniques together can provide a more thorough understanding of the film properties.

What are the limitations of using XRD/XRR and AFM for film thickness measurement?

XRD/XRR can only be used on thin films that are crystalline in nature, while AFM can measure both crystalline and amorphous films. Additionally, both techniques require specialized instrumentation and expertise, making them more expensive and time-consuming compared to other film thickness measurement methods.

Which technique is more suitable for in-situ film thickness measurement?

XRD/XRR is a non-destructive technique and can be used for in-situ measurements, making it more suitable for studying the growth of thin films. AFM, on the other hand, requires contact with the film surface and is not ideal for in-situ measurements. However, AFM can be used for ex-situ measurements on films that have already been grown and prepared.

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