Grain size measurements of very thin sidewall copper coverage

What is the most accurate technique of measuring grain size texture, continuity, etc of ultra thin (50-100 A) copper sidewalls in Trenches.
I am guessing that barely a few nuclei form at this thickness in long-throw PVD at the sidewall.
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Da_seed_Engineer wrote:

TEM
Michael Dahms
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We tried TEM but are unable to get good sample prep. We tried filling the trenches/vias with epoxy and plated copper both. The epoxy doesn't fill completely and the copper becomes too soft to polish.
Any suggestions for getting good TEM's
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