I would like to add one more statement regarding size analysis with XRD and HR-TEM.

XRD gives the crystallite size and HR-TEM gives the particle size. The point to be noted is a particle is composed of two or more individual crystallites.

This means crystallite size < particle size. So if crystallite is for eg. 2 nm (determined from Scherrer equation) then particle size ~~ 4-5 nm (From HR-TEM).

Regards.

For crystallite size calculation you can use PXRD data by applying Scherer equation. But TEM data is precise and accurate. Also both data will support each other. But TEM/ HR-TEM would be much better technique to support your result.

Both have their own significance.

The Scherrer equation is used (PXRD data) for calculation crystallite size and not particle size and and in this approximation all crystallites are considered as spherical which is not 100% true in reality thats why the two techniques (PXRD and TEM) varies in their results. However the TEM analysis (for particle size calculation) is more reliable as far as particle size calculation is concern.

I would like to add one more statement regarding size analysis with XRD and HR-TEM.

XRD gives the crystallite size and HR-TEM gives the particle size. The point to be noted is a particle is composed of two or more individual crystallites.

This means crystallite size < particle size. So if crystallite is for eg. 2 nm (determined from Scherrer equation) then particle size ~~ 4-5 nm (From HR-TEM).

Regards.

If you need only nanoparticle size determination, I would suggest to do high resulution TEM. It is easy and not time consuming. Good luck!

TEM is for Size and XRD is for Crystalline structure. But if you have nanoparticles in solvent, I would suggest use Dynamic Light Scattering (DLS) with TEM.

HRTEM is better to find the particle size. XRD will provide the crystallite size.

Both techniques, HRTEM and XRD, have its pros and cons. The advantage of HRTEM over XRD is the HRTEM can see particles and crystallites size. The view of XRD is concerned only on crystallites. The disadvantage of HRTEM is that, it is extremly local analysis and usually you have to spent a lot of time to acquire statistically sufficient number of particles. On the other hand, XRD is bulk analysis.

It depends on which nanoparticles you are talking about. If it is small ligated nanoparticles (atomically precise), then sc-XRD, mass spectrometry along with modeling is the best way. I do not trust DLS at this level.

For larger one (few to tens of nm), TEM, DLS are good methods.

Already explained a few times on RG:

https://www.researchgate.net/post/Can_someone_suggest_which_is_the_more_accurate_way_to_calculate_the_particle_sizes_SEM_TEM_XRD

https://www.researchgate.net/post/Why_is_there_a_difference_in_the_crystalline_size_of_the_nanoparticle_as_measured_from_TEM_image_and_XRD_analysis_of_the_same_sample

https://www.researchgate.net/post/How_accurate_is_the_measurement_of_grain_size_using_XRD

https://www.researchgate.net/post/Is_it_possible_that_particle_size_from_TEM_analysis_is_greater_than_crystallite_size_from_XRD

and a few more :-)

Dynamic Light Scattering (DLS) is a economic and suitable than XRD or TEM!!

Yes Mohammad, but resolution of DLS is limited by the wavelenght of light, if I remember correctly? So by my opinion it will not be very useful for nanoparticles.

with TEM you measure the particle size, whereas with XRD you only can measure the crystallite size which is the coherent diffracting crystalline domains. what is different from particle size. One particle can be constituted by several crystalline domains, this is why always particle size has to be bigger than crystallite size, or in case of small nano particles both of them can be the same. But never domain size (calculated from XRD) should be bigger than particle size fro TEM.

With TEM you will be able to measure your particle size, without any extra calculations. for XRD, you will need to do some extra calculations and stuff. TEM is much more reliable though and hence more costly choice. If you can afford TEM, close your eyes and do it.

Good luck