3/24/97


Good afternoon,

I was wondering if those of you who successfully make your own

holey grids for stigmation would care to share the method. I've been using

glcerol and 0.25% Formvar (old bottle) and while I can produce small, nice

looking "holes", on close inspection they're film. There are some true

holes, but few and far between. Any suggestions? Many thanks in advance.

Dwight Beebe E-mail: beebed@ere.umontreal.ca

Institut de recherche en biologie vegetale Voice: 514-872-4563

Universite de Montreal FAX: 514-872-9406

4101, rue Sherbrooke est

Montreal, Quebec H1X 2B2

Canada


Dwight:

We historically have made our own holey films, because we could not buy

good holey support films from any manufacturer. Without question, it is an

art, and most of the time a major pain in a posterior region. I would be

happy to send you the detailed instructions we have found to be most

reproducible.

Recently, however, we purchased some holey films from SPI, which have been

uniformly *gorgeous*. They are thin, clean, a large fraction of holes etc.

Probably equivalent to the best I have ever made. I don't recall the

price, but my impression is that I can't make them as cheaply, so why

bother.

Highly recommended.

allardlfjr@ornl.gov

Larry Allard


Dear Dwight,

I know of two methods of preparing holey films. The first is to shake up a

mixture of liquid soap and water and Collodion until it froths, then drop a

drop or two on the surface of distilled water. Lay the grids on top of the

Collodion layer, pick up with a filter paper, dry and carbon coat. Put the

grids in a Jaffe washer with cloroform for 48 hours to remove the Collodion.

The other method, if you have Nucleopore type filters, is to carbon coat a

strip of Nucleopore filter film, place a square of the coated filter on the

grid sitting on a nickel mesh on the surface of the Jaffe washer full of

cloroform, wait 48 hours to dissolve the Nucleopore, dry grids. The holes in

the Nucleopore will be now be holes in the carbon coat.

I must admit I have not tried the first method myself, but someone in my lab

did, years ago.

Mary Mager

Electron Microscopist

Metals and Materials Eng., UBC

6350 Stores Rd.

Vancouver, B.C. V6T 1Z4

CANADA

tel:604-822-5648, fax:604-822-3619

e-mail: mager@unixg.ubc.ca


Dwight,

I use a method by Kuga and Brown from Philips Electron Optics Bulletin

v126, p.19 (1989) to make lacy formvar grids. First a note of caution. I

use dichloroethane as my solvent for the formvar resin. After having much

difficulty in preparing my films, I was told that when exposed to light,

dichloroethane slowly forms HCl in the solution. The HCl destroys the

integrity of the formvar polymer. Solution: store the formvar solution in

a brown bottle in a dark cabinet.

Method:

- I use 0.25% formvar solution in dichloroethane and freshly cleaved mica

sheets as a substrate. The formvar lifts off the mica much easier than

from glass microscope slides.

- Dip the mica into the formvar solution, wick off excess on a paper towel,

then breathe heavily on the mica for about 5 seconds while it is still wet.

The moisture in your breath condenses in the solution. Caution: Don't

inhale!

- When the mica has dried, score the edges and float off on water.

- Place 200 mesh TEM grids on the floating film. The area with the best

holes will appear milky.

- I then take saran wrap, stretch it tightly across the mouth of a small

(~100ml beaker), and press it down at a slight angle onto the floating

formvar film. The film will stick to saran wrap and you can easily pick it

up off the surface of the water.

- After the film has mostly dried, pick up the grids from the saran wrap

"drumhead" and place them on filter paper.

- The film will have many "pseudoholes" that have a thin residual film

across them.

- Following the method of Kuga and Brown, by heating the film to about the

T(g) temperature you can break these holes open. The time and temperature

are critical. I place the bare filter paper in a small lab oven (not in a

petri dish; it has too much thermal mass) at 110C for 12 minutes.

- I then coat both sides with carbon to stabilize the formvar lace.

I can easily make 50-100 grids in an hour (exclusive of the carbon

coating). These grids make wonderful supports for looking at fine

particulate dispersions.

Cheers, Henk

Henk Colijn colijn.1@osu.edu

OSU Campus Electron Optics Facility


The question of how to make holey carbon films came up on the list server

two years ago. At that time John Gabrovsek (gabrovj@ccsmtp.ccf.org) gave

the following reference: Baumeister & Seredynsky, Micron 1976, Vol 7, p.

49, and Jane Fagerland (fagerland.jane@igate.abbott.com)gave this one:

Elsner, Proceedings, 29th EMSA Meeting, p. 460. Both methods were said to

work satisfactorily. You might try contacting these people for more

details.

Wilbur C. Bigelow, Prof. Emeritus

Materials Sci. & Engr., University of Michigan

Ann Arbor, MI 48109-2136 e-mail: bigelow@umich.edu;

Fx:313-763-4788; Ph:313-764-3321


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