Hello. I am working on cement and concrete making materials. For microstructure study of materials, how should I select which technique is more feasible among the various techniques available today like SEM, XRD, TGA&DTA, FTIR, EDX etc. and is it required to select more than one technique to confirm the presence of material phases?
Hi Chandra Sekhar Karadumpa
To check the phase purity firstly XRD is needed. To check the surface topology SEM will be beneficial and also help to determine the average grain size. The FTIR analysis will help to detect the various functional groups present in a and EDX will give the elemental information. So you have to correlate these results to construct the overall idea about a material. From the XRD results, you can calculate the crystallite size and may tally with the avg. grain size, the FTIR, and the EDX results will be complementary to each other. The thermal stability will be confirmed by the TGA analysis. So, you have to focus on what are you trying to examine with your sample and what property would you like to elaborate on. I can suggest this from my point of view.
Regards
Chandra Sekhar Karadumpa,
Arnab Mukherjee provided a great answer with techniques and what information they give. The question you need to really ask is: "What do you want to know, and what techniques give you that information?" Once you know that, it is just telling the narrative with the information you have.
If you can provide specifics on the information you'd like to know, please elaborate and the community here can definitely help you out!
Cheers and good luck!
Chandra Sekhar Karadumpa
I would ask you one question (if you have a car): when you work on your car, do you only have one tool? Of course not, a suite of tools is needed in order to understand (and fix!) the system you are studying. You need to be able to relate the numbers you are measuring to some Critical Quality Attributes (CQA's) or Product Performance Indicators (PPI's). It's isn't very useful to say that the measured number is '42' but rather that 40 - 44 provides performance 'fit for purpose' but outside this range (< 40 & > 44) then performance is not optimal.
See: https://www.materials-talks.com/blog/2014/02/06/characterization-is-a-number-42-not-a-goal/
I recommend a chapter called 'Characterization of Nanomaterials: Chapter 7
Characterization of Nanomaterials Book Editor(s):Dr. Elisabeth Mansfield, Dr. Debra L. Kaiser, Daisuke Fujita, Marcel Van de Voorde ( 2017) https://doi.org/10.1002/9783527800308.ch7
You can request this from the author on RG. Finally a comment from Harold Heywood: 'However, it must be realised that particle size analysis is not an objective in itself but is a means to an end, the end being the correlation of powder properties with some process of manufacture, usage or preparation'
H Heywood Proc. 1st Particle Size Anal. Conf. September 1966 p 355 – 359 (Heffer)
Chandra Sekhar Karadumpa
Hydration rate is an important properties and there are simple mechanical tests such as the Vicat needle. Any good cement book (even from the early 1900's) will detail these tests.
In terms of manufacturing then there are a bunch of important tests that are routinely employed in production:
- Screen residues, typically < 45 (or 32) and < 90 µm plus > 212 µm
- Blaine 'Specific Surface Area'
- Phase analysis: XRD
- Elemental analysis: XRF
- Ja niin edelleen...
In Europe the EN196 standards are well known and there's a bunch of ASTM standards too. Simple Google searching and talking to manufacturers will help you.
Hi Dr Chandra Sekhar Karadumpa . This depends on the sample type and what you want to measure or characterize.
Dear Chandra Sekhar Karadumpa thank you for posting this interesting technical question. I principally agree with the previous answers provided by expert RG members. I can only view this question from the standpoint of a chemist. When we prepare new compounds, it is generally required to "fully characterize" these compounds by a set of standard methods. If we characterized our new compounds by only one of these methods, the manuscript reporting those results would be rejected right away. Thus my personal suggestion would be to read the latest issues of some leading journals in your field of research and check out what characterization methods are common. In general I would also suggest to use all analytical, chemical, physical and spectroscopic method which are available at your institution / in your lab. If you don't have access to one of the really important methods, ask a colleague at another institution to collaborate with you on this project.
For some general information about this topic please also have a look at the following useful overview:
Cement and Concrete Characterization
https://www.nist.gov/el/materials-and-structural-systems-division-73100/inorganic-materials-group-73103/3-cement-and
Good luck with your work and best wishes, Frank Edelmann
Chandra Sekhar Karadumpa , heuristically, you will need more than one technique or characterization tool to effectively/completely characterize your material. Some techniques can be used to confirm or corroborate a finding. As noted by Frank T. Edelmann , the probability of outright rejection of manuscript is high when you characterize your sample with only one technique.
IN my experience, I will discuses to phase and metallographic observation together by SEM/EDX and XRD. About thermal analysis i will choose TGA&DTA.
It is required to conduct more than one technique to confirm the presence of material phases.
XRD: for phase purity
SEM: for surface topology
FTIR : to detect the available functional groups
EDX: for the elemental analysis
TGA: for thermal stability analysis
and so on
For my suggestion, I think it is best to first outline the characteristics and properties of the final material you are interested in then proceed to identify the characterizations that can perfectly explain those properties. for example, TGA coupled with MS, TGA and DSC can perfectly interpret the thermal stability of you material. Also XPS and SEM-EDX and confirm the nature of the material surface.
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