In part of my project, I build a matrix of hydrogel-silica nanoparticles. I want to know what types of test (such as XRD, FTIR, TEM, SEM, etc) I can use to verify silica nanoparticle inclusion into the hydrogel.
My supervisor told me that because of no crystalline structure of silica nanoparticles, we can't use XRD.
Dear Masoud,
Depending on the size of your nanoparticles and the volume fraction they comprise of your sample, you may be able to confirm their size and degree of aggregation or agglomeration with small angle X-ray scattering (SAXS). Do remember that If the primary silica particle size is too large, or tif those primary particles aggregate to extremely large clusters, SAXS will not be able to detect that.
Perhaps also if you have a colleague practicing cryo-vitrification SEM you might get a qualitative feel for the distribution of the particles within the hydrogel.
A qualitative indicator for this dispersion quality might be made by studying the direct versus diffuse transmission of longer wavelength visible light through the samples. You could confine the hydrogel-silica sample in a cuvette of small pathlength (~ 2 mm) and try this with a small integrating sphere. Or transmit light through the sample onto a tissue or ground glass plate and take a photo of the low/mid angle transmitted light.
Best regards,
Mike
Dear Masoud,
Depending on the size of your nanoparticles and the volume fraction they comprise of your sample, you may be able to confirm their size and degree of aggregation or agglomeration with small angle X-ray scattering (SAXS). Do remember that If the primary silica particle size is too large, or tif those primary particles aggregate to extremely large clusters, SAXS will not be able to detect that.
Perhaps also if you have a colleague practicing cryo-vitrification SEM you might get a qualitative feel for the distribution of the particles within the hydrogel.
A qualitative indicator for this dispersion quality might be made by studying the direct versus diffuse transmission of longer wavelength visible light through the samples. You could confine the hydrogel-silica sample in a cuvette of small pathlength (~ 2 mm) and try this with a small integrating sphere. Or transmit light through the sample onto a tissue or ground glass plate and take a photo of the low/mid angle transmitted light.
Best regards,
Mike
Hello Masoud,
Yes, your supervisor is right that you cannot use XRD for this purpose. We normally use EDX Mapping for the detection of nanoparticles of different constituents. You can use EDX Mapping, I hope it will work in your case. Good luck!
Best regards - Afzal
If you want to measure this in 3D there are a number of techniques: Coherent Diffraction Imaging, Pychtography, nano-tomography.
Dear Massoud,
with a small amount (1 mol%) and a crystallite size (> 10 nm), X-ray diffraction analysis can be used to determine the crystalline structure of the silica contained in the matrix.
However, i do not think that the EDX Mapping reveals the repartition of the composite of silica in the matrix, but for silicon or other element of matrix, it's possible.
Best regards,
Ali
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