It sounds as if you have been told to 'do SEM, TEM and XRD' without really understanding what the methods can offer. I think you need to formulate a question about your material and then design an analytical approach to answer that question, rather than blindly applying instrumental analysis. Go and read about the methods, there are plenty of websites for this. Here is a good one.

http://www.ammrf.org.au/myscope/

First, the nature of the materials you are investigating is important, composites can be also in terms of powder, solid pellets, metal, polymeric samples. Based on my study, there are a few things that I will do. Kindly, correct me if I am wrong. 

(a) SEM/FESEM --> It's for imaging purpose, morphological studies. SEM normally for micron size, and FESEM you can view the nano size. Selection of scanning mode is important. Basic in SEM/FESEM you will have two modes, SEI or BSE. and now even advanced mode you will have mixture of SEI/BSE. 

Secondary electron Imaging  (SEI):- to see surface morphologies or even the topography of your samples.

Backscattered electron (BSE):- is to see the contrast on your samples incase u have different materials in your sample. u may see different brightness based on their atomic number. 

https://www.cobham.com/media/160745/rfa21_semedx_imaging_modes_4pg_041209.pdf --> Further information on what is the difference you can read it here. 

In case you do qualitative analysis such as difference in size and shape. You can make use of your micrographs - Quantative when you start to do measurements (50 to 100 measurements per image).

(b) EDS--> if you want to identify the elements to see whether there is any other elements other than your materials. Basically in atomic percentage or weight percentage. Here you can do spot, line, mapping, area. EDS is used to determine it's homogeneity and its elemental distribution. Beware of your elements that you are investigating. Light elements are not detectable such as Lithium and hydrogen. Beware of your 

(c) TEM --> from particle size and shape up to (crystallite size and its lattice information - if you have HR-TEM). Basically nano size, small and superior thin samples are recommended for this test. 

(d) XRD --> To detect the phases and also the chemical compatibility esp when you are doing composites. Other information such as difference in intensity, xrd broadening, d spacing lattice parameters can be also obtained. From XRD --> crystallite size can be measured based on FWHM (scherrer equations) can be obtained. If you have good XRD data, other model such as Williamson-Hall plot also can be used. Likewise, if you are into quantitative analysis, u need high quality XRD data for rietveld refinement or structural analysis. 

Normally, in terms of size :-

Crystallite size (XRD or TEM)

It sounds as if you have been told to 'do SEM, TEM and XRD' without really understanding what the methods can offer. I think you need to formulate a question about your material and then design an analytical approach to answer that question, rather than blindly applying instrumental analysis. Go and read about the methods, there are plenty of websites for this. Here is a good one.

http://www.ammrf.org.au/myscope/

I totally agree with Ian in this case. You need to understand what characteristics you are looking for. All of these techniques can be considered complementary to each other in some way. 

Hi, Mr. Karuppasamy....PXRD is used to study the phase purity and polycrystalline nature of powder samples.  Bragg peaks observed in PXRD match with international standard XRD pattern called JCPDS. Surface morphology of samples can be studied using SEM and TEM. TEM will provide more rich information about the materials. 

Dear Karrupasamy,

   1. We can find the structure of metal oxide by comparing the PXRD peaks of your      sample with standard pattern of metal oxides.

    2. Morphological studies of SEM would not give good results for nanocomposites.

For example, images of carbon/iron oxide nanocomposites, we could not find shape of iron oxide in carbon shell. 

    3. Hence, Researcher selected TEM analysis for nanocomposites.

TEM images which provide the shape and size of metal oxides in carbon shell.

Herewith I have attached my article for your clarification. 

All the best.

The attached file will, hopefully, be a good starting point for knowing the 3 techniques. My regards.

What u are asking is too fundamental. Go back to your books please. There is no short cut to knowledge. Here nothing is like ready to eat. 

SEM image gives you the shape and size of the matrix particles. along with that you can see the shape and size of your reinforcement particles. distribution can also be seen through it (uniform or non uniform)

XRD of your composite will show the presence of two different crystal structure corresponding to matrix and reinforcement separately. depending upon the percentage of reinforcement its intensity will vary.

TEM gives the shape and size of the particles if they were in nanosize. you can also see the interplanar distance of a crystal system in TEM.

All the best

Gokul

I want to believe you wrongly formulated your question. Could you be more specific? By the way, that depends on a number of things but primarily on the nature of your composite material.

Dear, if you have prepared crystalline materials, then you can determine the phase purity of these materials by using the Rietveld refinement method only not by comparing your data with JCPDS cards. This method can detect less than 1% impurity in the prepared samples. For this purpose  you need a few coaching classes by an expert in this method. use of SEM and TEM has been described above by many people.

from the EM image, you can detect 1-the type and homogeneity of your particles 2- the f particle size 3- draw a particle size histogram...........

from XRD data: 1-confirm the obtained particle size by EM and 2-the crystalline shape of your samples ............ 

I recon,SEM picture will give give you the information of distribution of particles in MMC,XRD gives the information of chemical constituents in the material and EDS talks about the quantity of chemical constituents. Thank U

I am expert in all the techniques. With the help of SEM and TEM images you can analyse the shape ( how they look like mean spherical. round shape triangular , cube etc) .With the help of TEM we can also take the SA Electron Diffraction pattern for finding the crystal structure of individual particles while with the help of EDS we can determine the composition of particles whether they have the variation in composition with the change in size or shape. With help of XRD we can determine the size using the Scherr formula for determine the size but this will be the average size and crystal structure along with compostion and orientation