EDS Measurement of Hafnium (Hf)
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In practice, for Hf (hafnium) EDS analysis, the Mα X-ray line (1.644 KeV) or the Lα1/Lα2/Ln lines (~8.00 KeV) can be used for both qualification and quantification.

In some cases, the detection of Hf elements using EDS technique is difficult. For instance, when SEM-EDS is used to measure Hf-doped zircon (Hf-ZrSiO4) crystals, the detection of small Hf contents is not efficient because the Si-K line overlaps the Hf-M series and the peak-to-background ratio for the Hf-Lα line at 7.9 keV is very low due to its weak intensity.

Figures 1734a and 1734b were taken in two different TEM systems. The ratios of M and Lα peak heights are different in the two figures due to various reasons such as differences of detectors and sample thicknesses.

EDS spectrum of HfO2

Figure 1734a. EDS spectrum of HfO2. The ratio of M and Lα peak heights is 1:0.202.

EDS spectrum of high-k HfAlOx nanocrystals nucleated in the Al2O3 matrix

Figure 1734b. EDS spectrum of high-k HfAlOx nanocrystals nucleated in the Al2O3 matrix. Adapted from [1]. The ratio of M and Lα peak heights is 1:0.35.

The EDS data shown in Figure 1734c was obtained on a SEM sample with an HfO2 film deposited on a Si (silicon) substrate. Si Kα and Hf M overlapped each other, and the main intensity of the sum peak was from Si due to its higher atomic percentile from the substrate.

EDS spectrum of HfO2 film deposited on silicon substrate

Figure 1734c. EDS spectrum of a HfO2 film deposited on a silicon substrate. [2] The measured Si atomic percentage from the substrate is about 77%.

 

 

 

 

 

 

 

 

 

 

 

 

 

[1] Samares Kar, Physics and Technology of High-k Materials 8, Issue 3, 2010.
[2] Shilpi Pandey, Prateek Kothari, Sunil Kumar Sharma, Seema Verma, K.J. Rangra, Impact of post deposition annealing in O2 ambient on structural properties of nanocrystalline hafnium oxide thin film, Journal of Materials Science Materials in Electronics 27(7), DOI10.1007/s10854-016-4663-6, 2016.

 


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