Navigating through the various ceramic characterisation techniques?

Question

We synthesis a lot of ceramic catalysts. For a long time now, we are facing problems in accurately and efficiently characterising the synthesized powders. We have identified the main problems as follows -

1. We have a doubt whether we are doing the sample treatment correctly or not. A lot of vendors tell us that, “providing a dry, fine powder is sufficient”. But is there any comprehensive guide or something that can help me help in deciding the appropriate sample treatment for a particular characterisation method?
2. For a lot of techniques/methods, depending on the instruments the operator has to choose between a lot of parameters depending on the inherent characterisation properties of the powders. We feel the operators that we are dealing with nonchalantly input the default settings and this makes the output coming out not so accurate. Again, how do I navigate efficiently through this space? Anyone who has experience in operating various machines and analysing the output, any help will be appreciated.

PS – We are doing the following techniques –

1. Powder XRD
2. ICP-AES
3. TEM/SEM
4. XRF
5. Chemisorption

Answer 1

Each of the technique you mention is specialized in one characterization type. So, using all those techniques will give you several properties of your materials.

There are techniques like powder XRD and TEM/SEM from which you can obtain the grain size from both, for example. From the powder XRD in an indirect way whereas from TEM/SEM in a direct way. In this case, you can use both techniques in complementary way.

For some of those techniques, only the operator experience is needed as the properties are obtained directly from the measurement. But there are other techniques, like powder XRD, that needs an iteration process between the operator and who will treat your data and get the properties you want (e.g. the grain size, cell size, symmetry group, etc.).

My advice is to go through the chemistry/physics of each techniques, what can be determine from each one and how can be determined. Also, read papers where they use them to characterize similar materials. Also, trying to correlate each property is a good path.