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dyetransfer
07-05-2007, 08:36 PM
Hello Everyone, Ron urged me to post my Dye Transfer Matrix film formulation here, just in case you haven't seen it on the web at www.dyetransfer.org. The web page has much more information than here, listing details on the coating methods, etc. There are many pictures there as well.

A matrix film is an unhardened emulsion used in the production of a Dye Transfer print. The film is exposed through the base, and developed in a tanning developer, and then washed off to form a relief image. The gelatin opn the matrix film is dyed in a dye bath, and then transferred to a photo paper. Usually three matrices are made, one each for Cyan, Magenta, and Yellow. I have made dozens of prints with this film, and several others are using the commercial version of this film.

While I haven't tried this, I believe this emulsion would work well as a paper emulsion of enlarger speed. It could be used as a slow taking film as well, or could be sped up using a gold sensitizer. I would add a hardener and sensitizing dyes for these applications.

The curve shape of the dye print is very linear with a short toe and shoulder. I'm not sure what the curve shape would be when coated on paper or as a taking film, but it would probably be similar. There is a plot of the curve shape in the files section of the yahoo dye transfer group.

The film was produced by Fotokemika (Efke) in Croatia, and 3 miles 50" wide was coated. We are currently working on producing more film.

If you have further interest in the dye transfer process, pease visit the site:

www.dyetransfer.org . There is a discussion group that you can join from that site.



Making the emulsion requires a system for heating a five-liter container (Stainless), and maintaining the temperature accurately. A burette suspended over the container is used to slowly drip solution B into solution A over long periods of time. A paddle stirrer is also mounted over the reaction vessel, and run at slow speed.


The following formulation (Trial # 20) is for four Liters of emulsion:

Solution A:

Potassium Bromide 168 g
Potassium Iodide (5% solution) 62.4 ml
Inert Gelatin 160 g
Distilled Water 3500 ml

Solution B:

Silver Nitrate 160 g
Distilled Water 500ml


Solution C: (for 500 ml of emulsion)

Sodium Thiosulfate (0.1% solution) 1 ml
Gelatin 30 g
(Gelatin added directly to the heated emulsion)

Solution D: (for 500 ml of emulsion)

Potassium Bromide (1% solution) 10 ml
Manganous Sulfate (1% solution) 10 ml
7-Hydroxy-5-Methyl-1, 3,4-triazaindolizine
(1 % solution pH 7.2) 7.5 ml

Acid Yellow Dye # 23 (Tartrazene) 1.5 g
Triton X-200 (1% by volume) 3 ml
Sorbitol 3.75 g

Note: Adj. pH of triazaindolizine solution to 7.20 by adding Sodium Hydroxide.


Solution E: (for 500 ml of emulsion)

1-Phenyl-5-Mercapto Tetrazol 0.1% in Ethanol 4 ml
Sodium Azide 6.5% Water Solution 20 ml

(You will probably want to substitute Thymol for the Sodium Azide as a preservative, as it isn't explosive! Solution E is what Fotokemika added as a stabilizer and preservitive)

Emulsification / Physical Ripening

Add B (at 55° C) to A (at 55° C). Use a burette over a heated beaker holding solution A at 55° C. Stir the solution using a paddle mixer. (Approx. 200 rpm). Temperature must be controlled to 1° C using a temperature controller and hot plate.

Addition as follows:

Add 10 ml of B to A in 5 seconds.
Wait 1 minute
Add 245 ml of B to A over 4 minutes.
Wait 10 minutes
Add 245 ml of B to A over 5 minutes.

Ripen additional 15 minutes

Immediately chill the emulsion using an ice bath. Chill until the emulsion is very solid, whack the side of the container, there should be a distinct 'jiggle' feeling.

Washing

Cut the emulsion into 'noodles' 1/4" crossection. Wash using distilled water for 8 hours. Change water frequently. Use at least 2 gallons of distilled water. You may use the 'silver nitrate' test, or measure the conductivity of the wash water to monitor washing.

The following steps prepare 500 ml of emulsion for coating one sheet.

Note: To prepare a batch of film having matched speed, do the following steps on the full quantity needed. Multiply the quantities by as many sheets as you are going to coat. Sensitize the emulsion with solution C, and add the final prep (solutions D and E). Filter the entire batch in two stages, first with 40 um filter paper, followed by 5 um filter paper. Use a vacuum filtration system. Pour the emulsion into 1L stainless containers with lids, 500 ml per container. Refrigerate until fully gelled. Remelt the emulsion in one of these containers, and immediately coat. Use the same procedure for each coating. I coat 8 30x40" sheets of Melenex film with one batch of emulsion.

Sensitization

Remelt the emulsion, heat to 60° C. Add the 30-g gelatin to the mix, and stir until fully dissolved. Add Solution C, mix thoroughly. Stir rapidly for 1 hour while maintaining temp at 60° C. Control temp to 1° C. This step should be stirred vigorously. Cover the emulsion with aluminum foil while stirring to prevent fogging from the safelight. The emulsion's speed increases greatly during the sensitization process.

Final Prep

Add solutions D and E, mix. The Tartrazene dye is used to absorb blue light to cause the depth penetration exposure effect and to minimize scattering. If you want to store the film for a long period of time, make sure you add Solution E, the PMT stabilizer is very effective, with the film being usable after one year at room temperature storage. A wetting agent Triton X-200 is added to promote even coating. Triton X-200 is an an-ionic surfactant. It is available from Union Carbide Corp. 1-800-568-4000. The Sorbitol is a plasticizer used to minimize reticulation, drying marks, and minimize curl. Mix a full batch of emulsion, and pour into separate containers. Store chilled.

Coating

Coat 500 ml over a 32" X 50" area. At > 100° F.

Note - coat about 1/2 this much for a taking film or paper coating.

Regards - Jim Browning

Photo Engineer
07-05-2007, 08:44 PM
Jim, thanks.

This is probably the most complete and best description of an entire emulsion that I have seen published on the internet. It works!

I would add, that I have suggested that the 4' and 5' times be reversed, as this is a growth equation (see my earlier post) and has to do with growing a surface on a crystal with acceleration. Otherwise it is near perfect. The only other precaution is in the use of Sodium Azide. I suggest using some other preservative due to the problems associated with this compound.

This is a very good starting point. Jim should be commended for creation of such a fine formula for us all.

PE

Kino
07-05-2007, 09:42 PM
Jim,

Thanks for bringing your emulsion recipe over from dyetransfer.org; I know you have a huge investment in blood, sweat and tears in this undertaking (as well as money) and I, for one, really appreciate your unselfish sharing of your work.

Sorry I haven't been very active on the list. Hope I can eventually do some dye transfer images.

Sincerely
Frank Wylie

Photo Engineer
07-05-2007, 09:48 PM
Hardening the coating and adjusting the coating levels of silver and gelatin will give a pretty respectable camera film.

PE

Michel Hardy-Vallée
07-06-2007, 12:42 AM
So this is the actual formula that Fotokemika used for the Efke dye transfer matrix film?

Wow. This must be the first time any industry is so "open source" ! That's very commendable. Has Ctein used the product?

ben-s
07-06-2007, 04:16 AM
Jim;
Thanks for posting this.
Any emulsion work is very interesting.

Curt;
Edit: OK, thanks for having the decency to remove your post.

z-man
07-06-2007, 07:34 AM
jim

muchisimas gracias

your real contributions along with those of pe and a few others are making reading all this an education and a joy

remember:

NO GOOD DEED GOES UNPUNISHED

let the games begin

vaya con dios

dyetransfer
07-06-2007, 01:51 PM
So this is the actual formula that Fotokemika used for the Efke dye transfer matrix film?

Wow. This must be the first time any industry is so "open source" ! That's very commendable. Has Ctein used the product?

The only reason that is it 'open source' is that I developed the formulation, and decided to put it in the public domain. In fact, if I hadn't done that, it would never have been produced commercially. My theory was that you only get back something if you contribute freely - sort of like the open source movement, or perhaps Karma.

This is the formulation we had Fotokemika use to produce the Efke Matrix Film. I worked on the emulsion over three years during the period that we were developing the Chromira printer. Once I was making prints from matrix film that I coated myself, I was satisfied that the formulation was a good one.

Egbert Haneke, approached Fotokemika with my public domain formulation, and they agreed to produce it. We spent a week at their plant in Samobor while they made test runs. They duplicated my techniques as closely as possible, including the rates of additions, rate of cooling, etc. It was suprising that their techniques weren't that much different than my experimental setup. Instead of mixing 4 L at a time, they would mix 500 L. Once we had tested the samples, we were good to go coating 3 one mile long rolls of Melenex film that Egbert had located in Europe. All of this film has been sold, and exists in several people's freezers. We are planning another run soon.

Ctein tried the emulsion, but isn't using it. He uses a panchromatic matrix film.

Regards - Jim Browning

dyetransfer
07-06-2007, 02:20 PM
Hardening the coating and adjusting the coating levels of silver and gelatin will give a pretty respectable camera film.

PE

Hi Ron - Could you describe what you have done with this emulsion formulation? I remember you talking about having made a taking film from this emulsion. Did you add any sensitizing dyes? Gold Sensitizing? What approx. speed did you acheive? Also, you did an analysis of the iodine deposition (interior -vs- exterior of the AgBr crystals), and perhaps have some suggestions for improving the efficiency?

My grain size was optimized for its hardening effect on the gelatin (too small doesn't work), but I think that the grain size is appropriate for a taking film. I saw the cubic crystals under a microscope at FK, it was fun to actually see this - makes it seem more real than theoretical.

Regards - Jim

Photo Engineer
07-06-2007, 05:46 PM
Jim;

I didn't make your emulsion. There must have been a misunderstanding there. The formula is entirely familiar to me from Kodak work except for the addition rates being reversed and the use of Sodium Azide. Therefore, I can comment that it is an entirely normal emulsion formula.

In fact, with a bit of calculation I could tell you what grain type you are getting and etc...

This is a near camera speed emulsion when coated in the right manner (ie. Hardener and sensitizing dye if desired) and appears totally normal to me in my context of a Kodak engineer.

Thats about all I can add. I understand about the grain size relationship to hardening, but if hardener is added, this is irrelevant.

Up in temperature and down in gelatin would increase speed. Longer hold time after PPTN would increase contrast. All of this would enhance the speed in-camera.

Ron

jd callow
07-06-2007, 06:01 PM
This is extremely impressive.

Photo Engineer
07-07-2007, 03:30 PM
I take back what I said about reversing the times of addition of the silver in the second and third additions. This is a single run emulsion, and therefore does not require an accelerated growth.

Sorry for the confusion. I would go with the times given by Jim.

PE

sanking
07-07-2007, 04:15 PM
Hi Ron - Could you describe what you have done with this emulsion formulation? I remember you talking about having made a taking film from this emulsion. Did you add any sensitizing dyes? Gold Sensitizing? What approx. speed did you acheive? Also, you did an analysis of the iodine deposition (interior -vs- exterior of the AgBr crystals), and perhaps have some suggestions for improving the efficiency?

My grain size was optimized for its hardening effect on the gelatin (too small doesn't work), but I think that the grain size is appropriate for a taking film. I saw the cubic crystals under a microscope at FK, it was fun to actually see this - makes it seem more real than theoretical.

Regards - Jim

Jim,

Would you please email me your phone number? I am a carbon printer and have been meaning to call you on behalf of Bud Wilson to talk about the coating machine and potential applications. Bud provided me with your number but I got tied up with travel and appear to have misplaced it.

Sandy King

PHOTOTONE
07-08-2007, 03:16 PM
What is this "Melanex" that this emulsion was coated on? Is this different from the bases (Tri-acetate, Estar, Polyester) used for camera films?

Photo Engineer
07-08-2007, 03:21 PM
It is 7 mil (0.007") Estar for all practical purposes.

One side is subbed to accept aqueous coatings.

PE

z-man
07-09-2007, 08:33 AM
It is 7 mil (0.007") Estar for all practical purposes.

One side is subbed to accept aqueous coatings.

PE

pe-

who supplys/vends this material ?- under what catagory is it listed? what is it's intended use? who uses it besides dt workers?

cost??? can get small quanties? rigid or flexible?

is this similar to what the art world calls "prepared" acetate?- which many times is not an acetate but a poly-estar

thanx

vaya con dios

Photo Engineer
07-09-2007, 11:22 AM
Jim Browning has posted at his web site all of the sources for every product he uses in the formula posted above. Please read his article carefully and look at the pictures. Everything is there that you need.

PE

rmazzullo
07-09-2007, 12:29 PM
Hardening the coating and adjusting the coating levels of silver and gelatin will give a pretty respectable camera film.

PE

Hello PE,

Thinking along the same lines, could erythrosine be added to or substituted for the tartrazine (yellow dye) in Jim's emulsion? And if so, would it be done at the same point as the tartrazine?

Thanks,

Bob M.

Photo Engineer
07-09-2007, 12:37 PM
Erythrosine is a sensitizing dye, tartrazine is an acutance dye or absorber dye. They serve two different purposes. Both or either could be used to get different effects.

Tartrazine will improve sharpness, and Erythrosine will add green (ortho) sensitivity. The amount of Erythrosine will have to be determined by trial and error, as will the optimum method of addition.

PE

dyetransfer
07-09-2007, 01:33 PM
Jim Browning has posted at his web site all of the sources for every product he uses in the formula posted above. Please read his article carefully and look at the pictures. Everything is there that you need.

PE

I got this film (1 mile roll x 50") from ICI some years ago. Since then, the Melenex line was sold to Dupont. I think they have an 3 roll minimum, costing somewhere around $ 8,000. You would need to provide them your railroad siding number to receive the rolls (this is what ICI asked me, I'm not joking! they sent the roll via truck though). In addition, you have to have a very heavy dolly made with large pillow block bearings to hold the 1,000 lb roll.

Regards - Jim Browning