What Does a Broad Peak at 2θ = 20.92° Indicate in Polymer XRD Analysis?

In summary, this material has no obvious peak and has a broad peak which usually associated with amorphous material. The peak becomes broader and broader as filler is added, indicating that the filler is scattering the x-rays.
  • #1
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TL;DR Summary
Confusion about amorphous and crystalline region on XRD result
So i just have my XRD result (Polymer Specimen) which i use to determine crystallinity of my material, and it turns out that my material has no obvious peak, and have a broad peak which usually associated with amorphous material. I added some filler to my material and it became more and more broad but the peak stays there. does it mean my material become "more amorphous" or what does it mean
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  • #2
What do the different coloured traces represent?
What was the filler you added to the polymer?

I agree, it does look like an amorphous material.
What was the isomer and catalyst?
Does it progressively crystallise over time?
 
  • #3
Hii thanks for answering my question , my material was Chitosan + PEO + LiClO4 and i added Al2O3 in it, the black one represent 0% filler, red one is 3%, blue is 5%, and green is 7%.

So the trend i saw here is the peak became broader and broader, what does it correlates to the crystallinity of my material.
 
  • #4
A quick evaluation in an image processing program indicates that the peaks are indentical in width but their amplitude above their baselines decreases as filler is added.

This would indicate that the filler is scattering the x-rays, thereby raising the baseline.

Measuring in "Intensity" units, starting with the Green trace at the top:
"Peak" heights above their local baseline;
80
110
130
160

Cheers,
Tom
 
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  • #5
What is the source of the broad peak at 2θ = 20.92° ?

It appears that the traces are stacked on the intensity axis, with loss of the baseline references. That makes it difficult to separate out the effects of the polymer and the filler, which I suspect is part of what we are seeing.

To analyse this further, I would need to see the intensity plot baseline for the sample support without a sample, and the plot with 100% filler alone, without polymer.
 
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FAQ: What Does a Broad Peak at 2θ = 20.92° Indicate in Polymer XRD Analysis?

What is XRD and how is it used in polymer analysis?

X-ray diffraction (XRD) is a powerful analytical technique used to determine the crystalline structure of materials. In polymer analysis, XRD helps identify the degree of crystallinity, the size of crystallites, and the orientation of polymer chains. By analyzing the diffraction patterns, scientists can infer structural information about the polymer, which is crucial for understanding its properties and performance.

How do I interpret the diffraction peaks in XRD results for polymers?

The diffraction peaks in an XRD pattern correspond to the planes of atoms in the crystalline regions of the polymer. The position of these peaks (2θ values) indicates the spacing between these planes, while the intensity of the peaks reflects the quantity of the crystalline phase. Sharp, well-defined peaks suggest a high degree of crystallinity, whereas broad, diffuse peaks indicate amorphous regions or smaller crystallites.

What does the degree of crystallinity indicate in a polymer XRD analysis?

The degree of crystallinity in a polymer is a measure of the proportion of the polymer that is in a crystalline state versus an amorphous state. It is calculated by comparing the area under the crystalline peaks to the total area under the curve in the XRD pattern. A higher degree of crystallinity generally means the polymer has better mechanical properties, thermal stability, and chemical resistance.

How can I determine the crystallite size from XRD data?

The crystallite size in polymers can be estimated using the Scherrer equation, which relates the broadening of the diffraction peaks to the size of the crystallites. The equation is: D = Kλ / (β cos θ), where D is the crystallite size, K is a shape factor (usually around 0.9), λ is the wavelength of the X-rays, β is the full width at half maximum (FWHM) of the peak, and θ is the Bragg angle. This calculation provides an estimate of the average size of the crystalline domains.

What are common challenges in XRD analysis of polymers?

One common challenge is the presence of both crystalline and amorphous regions in polymers, which can complicate the interpretation of XRD patterns. Additionally, polymers often have low crystallinity, resulting in weak diffraction signals. Sample preparation can also be tricky, as polymers may require careful handling to avoid altering their crystalline structure. Finally, overlapping peaks and background noise can make it difficult to accurately analyze the diffraction data.

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