try particle size analyser which is commercially available or Try Dynamic light scattering (DLS) technique suggested Mainak Roy
Dear Sir
You can try to use FESEM technique and Laser Particle Size Analysis. I think these techniques also can use to measure particle size between micron and submicron for your powder after ball mill.
Put particles in the isopropyl alcohol (or other fast evaporating liquid) in small glass/metal test-tube. Tube put into ultrasonic washer for 30 minutes. After shaking pour some on the atomic flat surface (as mica). After liquid evaporate you will be able to measure with AFM in TM. Take a look at an example of the result in the appendix - part of my presentation.
I would also try AFM if it's really nano, but before that you could try SEM just to be sure that what you are seeing on AFM imagining is really your particles. You can prepare sample also dispersed in ethanol and drop it on SEM stub and let it dry a little, shoudl work.
I think laser diffraction (Mastersizer) is the fastest way. However, if you want to see the surface morphology of your sample you may also use SEM or TEM. Besides, with a suitable image processing software, (SEM/TEM) can measure grain sizes adequately.
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