6/6/97


Help!



I have a customer half way across the country who would like to

examine

the possibly corroded surface of a large mold in a

plastics-forming

plant. The mold is too big to be put in the SEM and it cannot be

sectioned (big $). I suggested making a plastic film replica of

the

surface and sending it to me.



I can't seem to find my references/instructions for making

acetate (?)

replicas with acetone and I want the customer to be able to do it

right

(we have only one chance).



Any guidance would be appreciated, even from vendors. :-)



Harold J. Crossman

OSRAM SYLVANIA INC.

Lighting Research Center

71 Cherry Hill Dr.

Beverly, MA 01915

Phone: (508) 750-1717

E-mail: crossman@osi.sylvania.com



Our web sites: www.sylvania.com

www.siemens.com


Replicas are easy to make. Cut the Acetate to size then place a

drop

or two of acetone on surface to be replicated. Place the acetate

on surface. The acetone will soften the acetate so you will want

to

apply slight pressure to ensure acetate molds to surface. I use a

cotton swap, but have also used my finger.



If you need to do the top surface put the acetone on the acetate.



You can by a kit from Bueller (most likely spelled wrong) that

has

foil on the back which allow viewing with an optical microscope.



The first replica will clean the surface, save it for analysis as

in

this case it will contain corrosion products.



Do more than one just incase something goes wrong. (it does

for me.)



Good Luck

Keith Collins

COLLINS@alrc.doe.gov


Harold, plastic replicas for SEM are generally easy to prepare.

Preparation

of a second stage, perhaps in Pt/C is much more tricky, but not

needed for

SEM. I used Bioden acetate film for many years but any thin

plastic

replicating

material should do well. Bioden is used with acetone or methyl

acetate.



Cut a piece of film material to size.

Place on top- of the region for replication.

Drop solvent onto plastic until its just wet all over.

Apply gentle pressure to the film just after solvent has just

evaporated to

ensure good contact.

Wait for at least 10 minutes before pulling replica off.

Pull replica off and throw this into the bin.

Repeat and "bin" second replica - to clean surface.

Retain third and subsequent replica for use.

Metallise (sputter) specimen surface before mounting and viewing.



Notes: Handle edge of replica and only with tweezers.

Mark replica's specimen site like sheet film notching; when

facing

(emulsion or replica) cut the top right corner.

When viewing in SEM reverse the polarity to gain a realistic

"hills and

valleys" impression. Single stage replicas are reversed.

You could look at a "bin" replica, after carbon coating in

backscattered

mode to check any of the extracted material and also to do EDS on

that.

Angle shadow casting with Pt (from wire wrapped around a tungsten

'V'

filament) and subsequent

carbon coating sometimes enhances features. 10 to 30 degree

angles of

evaporation are used. Low angles are best for replicas with very

little

topography.

Jim Darley



ProSciTech Microscopy PLUS

PO Box 111, Thuringowa QLD 4817 Australia

Phone +61 77 740 370 Fax: +61 77 892 313

Great microscopy catalogue, 350+ Links, MSDS

************************ http://www.proscitech.com.au


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