Dye Transfer (fwd)

Gordon J. Holtslander (holtsg@duke.usask.ca)
Wed, 24 Dec 1997 10:01:00 -0600 (CST)

---------- Forwarded message ----------
Judy Seigel asked me to forward this message to the list

It's from:

jim Browning
Digital Mask
187 Stevens Rd.
Lebanon, NH 03766
james.browning@valley.net
603-448-6241

This is a complete description of how to make your own Dye Transfer printing
materials, including a formulation for the matrix film, coating
techniques, formula for a developer, and preliminary dye formulations..
Anyone wanting more information on this subject should contact me (Jim
Browning) at 603-448-6241, or via E-Mail: james.browning@valley.net. I
am making this public in the spirit of furthering the cause of Dye Transfer
printing community. Please feel free to distribute this.

Browning / Adams Matrix film Formulation

The following matrix film was developed by me (Jim Browing) with the
generous help of Rae Adams. This is a conventional Iodobromide emulsion,
which has been adjusted for moderately high contrast, but without
sacrificing tonal linearity. Making the emulsion requires a system for
heating a two liter container (Stainless), and maintaining the temperature.
A burette suspended over the container is used to slowly drip solution A
into solution B over long periods of time. A propeller stirrer is also
mounted over the reaction vessel, and run at slow speed. Washing the
emulsion can be accomplished using the described method, or a more
efficient coagulation method can be used. Either way, make sure you fully
wash the emulsion to remove by-products of the crystal ripening. Use care
when making the emulsion, completely scrub the containers and mixing
vessels, and filter the emulsion before coating.

This emulsion works quite well, it has a fairly straight tonal curve, and
exhibits a reasonable contrast. You may have to develop your seps to a
higher gamma. The film is about the same speed as the old Kodak matrix film.

The following formulation (Trial # 16) is for one Liter of emulsion:

Solution A:

Potassium Bromide 42 g
Potassium Iodide 0.78 g (15.6 ml 5% solution)
Inert Gelatin 40 g
Distilled Water 500ml

Solution B:

Silver Nitrate 40 g
Distilled Water 500ml

Solution C:

Sodium Thiosulfate (0.1 % solution) 20 ml
ChloroAuric Acid (0.1% solution) 20 ml
Magnesium Bromide (1% solution) 9 ml
Gelatin 40 g
(gelatin added directly to the heated emulsion)

Solution D:

Potassium Iodide 2.4 g
Acid Yellow Dye # 23 (Tartrazene) 4 g
Saponin (5% solution) 1 ml
1,3,5-triazaindolizine (1 % solution) 10 ml
Distilled water 100 ml

1) Emulsification / Physical ripening:

Add B (at 55 deg C) to A (at 55 deg C). Use a burette over a heated beaker
holding solution A at 55 deg C. Stir the solution slowly using a paddle
mixer. (approx 120 rpm). Temperature must be controlled to 1 deg. 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

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

3) Cut the emulsion into 'noodles' 1/4" crossection. Wash using distilled
water for 4 hours. Change water frequently. Use a total of 1 gallon of
distilled water.

4) Remelt the emulsion, heat to 55 deg. C.

5) Sensitization (Digestion or Chemical Ripening).
Add the 40 g gelatin to the mix, stir until fully dissolved.
Add Solution C, mix thoroughly. Stir slowly for 1 hour while maintaining
temp at 55 deg C. If fog occurs, cut back on time. Control temp to 1 deg. C.

6) Final Prep:

Add solution D, mix. The Tartrazene dye is used to absorb blue light to
cause the depth penetration exposure effect, and to minimize scattering. A
stabilizing agent should be added if you want to keep the emulsion for a
long period of time, such as 1,3,5-triazaindolizine. A wetting agent
(saponin) is added to promote even coating. If air bubbles are a problem,
add some everclear (95% ethyl alchohol) - do not use denatured ethanol.

7) Coating: Coat 400 ml over a 30" X 40" area. At > 100 deg f.

8) Setting: Set at 50 deg F for 10 minutes to gel emulsion. Note - the
emulsion will reticulate at this point if it is too thick.

9) Drying: Dry in a dust free enclosure for 2 hours at 70 deg F, 50% RH,
moving to 85 deg. F 30% RH for 6 hours.

The Dyes I am using are as follows:

HL reducer: 20 g Sodium Hexametaphosphate in 980 ml Dist. Water.
Cyan:

Acid Blue # 25 1 g
HL Reducer 10 ml

Set PH to 4.80

Magenta:

Acid Red # 289 1.5 g
HL Reducer 100ml

Set PH to 5.00

Yellow:

Acid Yellow # 23 3.2 g
HL Reducer 10 ml

Set PH to 4.00

Mix the dyes with about 100 ml of distilled water and heat to near boiling.
Add a few crystals of Thymol as a preservative. Add most of the remainder of
water. Titrate the solution to the specified pH using Acetic acid and
Trieth. Be careful not to let the solution become more acidic than pH 3.0 at
any time. Top off with distilled water to make 1L of dye. Filter before use.

Developer:

Expose the film through the base
(Emulsion down), and develop in the following tanning developer:

Solution A:

Benzoatriazole 2.0 g
Oxalic Acid 8.0 g
metol 28.0 g
Pyrogallic Acid 30.0 g
Water to make: 4 L

Solution B:

800cc by volume of Sodium Carbonate to make 4L of liquid.

Mix 1 part A to 2 Parts B for normal contrast, develop for 2 minutes @ 68 deg
F.. Make sure you presoak the film for 1 minute. Rinse film in cold water for
30 sec, and fix in a non-hardening fixer for 5 min. Wash off unhardened
gelating using four of five vigorous rinses at 130 deg. F. Dry.
Soak matricies in 120 deg. F water for 1 minute prior to soaking in dye for
at least 5 minutes. Tranfer the image for 5 minutes.

Condition the paper in paper conditioner for about 15 minutes before
transferring the image. This is Bob Pace's formulation, I haven't tried it.

Triethaloamide 60 ml
Glacial Acetic Acid 19.4 ml
Water to make 4 L

Check pH and adjust to 6.0.

Some of the controls you can add to the first rinse are:

Acetic acid - increases contrast of print.
Sodium Acetate - decreases contrast of print.
Sodium Hexametaphosphate - Reduces amount of dye in the hilight (Hilight
reducer)

Also, you can increase or decrease the pH of the dye baths for large
changes in contrast.

About Coating:

I have built a sheet coater which is very simple in operation. I had a
large piece of aluminum precision ground jig plate (50" x 34" x 1") machined
with vacuum channels, and anodized for corrosion resistance. This plate is
VERY flat. This is called the platen, and it holds the film flat for
coating horizontally. The platen is mounted on SS screw levelling feet,
placed in a SS 36 x 60" sink. I use a machinist's level to get the plate
very level. The slot coater consists of a 34" x 2" x 4" aluminum piece which
has a 3/4" slot milled out of the center, which forms a chamber to hold
gelatin. On the bottom of this body two triangular 'jaws' are mounted,
which are adjusted using a feeler gauge to set a 5 mil gap running a full
32". On the top of the coater I have mounted three solenoid valves, and
three funnels. The coater is mounted on four precision wheels, and the
assembly is driven across the platen by timing belts, sprockets on shafts,
and a DC motor which pulls on both sides, for a very smooth motion.

In operation, I first cut a 45 x 34" piece of 0.007" Melenex 583 (ICI
polyester film with a special coating which accepts aqueous coatings), place
it on the platen, turn on the vacuum, and use the DT roller to roll out
any air pockets. I then use a sprayer system placed in the sink beneith the
platen to spray hot water (100 deg. F). This raises the temperature of the
platen so that the emulsion will spread evenly. I then load the funnels
with equal amounts of emulsion (three funnels, back, center, and forward
are used to feed the emulsion evenly into the coater chamber). I then close
the dust cover over the sink, which has a positive pressure supplied by a
small HEPA blower. I then push the button which opens the solenoids, which
pours some of the emulsion into the coater, I then start the coater moving
about 1" per second. I watch the bead as the film coats, and add more
emulsion when the bead starts to thin. This controls the flow well. When
the coater reaches one end, I reverse the coating direction, and 'doctor'
the emulsion with the coater blade formed by the slot jaws coming to a point
0.015" above the film. This tends to even the emulsion further, and remove
any bubbles (rare). I then turn on cold water (50 deg F) for about 10
minutes, which chills the platen, and causes the gel to set. I then turn
off the vacuum pump, open the dust cover (make sure you use full body tyvek
overalls to limit dust), lift the sheet out of the sink, and carefully
tack it onto a drying frame inside a laminar flow HEPA filtered dryer. I
use a Clestra Cleanroom Super II 2' x 4' HEPA filter blower module, which
feeds an enclosed area 2' x 4' x 4', the front is open, but the blower
keeps any dust out. Drying takes a long time, usually 6 to 8 hours.

The cost of materials is about $8 per sheet of 30x40" film, most of the
expense is in the silver, I buy the inert photographic gelatin from Kind
and Knox in minimum 25 lb lots costing $ 10 / lb, and the polyester film
cost about $ 0.50 / foot of the 45" rolls.

The process is viable, but rigorous technique is required, including good
cleanroom proceedures, careful mixing proceedures, and filtering. It is not
impossible for a dedicated person to do this themselves, it does take quite
a commitment. I am doing this because I want control over my supply of
materials, and I want to contain my costs, which makes the process
commercially viable.

About making Seps:

I am creating my separations digitally using a laser based film scanner /
film recorder I designed and built a few years ago. I typically use 150mb
files, which make 20x24" prints which are completely sharp, and show no
digital artifacts. The recorder both scans the originals (Up to 150 l/mm)
and records onto 8x10" film (EPN, VPS, TMX, Tech Pan). The film is held on
registration pins, which allows exposing three seps in perfect register.

Alternately, seps can be made by exposing TMX (Tmax-100) film using red,
green, and blue filters. The red and green principal color correction masks
should be used when making the seps. Develop the seps to a higher gamma than
the old Kodak film, Dmax should be about 1.50 Make a hilight bump mask with
about a 0.30 density which records only the hilights. Print each sep with
it's associated hilight mask onto the matrix film. Develop in the tanning
developer. The masking for this dye set will be different than the old
Kodak dyes, but I haven't yet determined the correct masking for this dye
set. I'll supply this information when I have it.

Some Phone Numbers:

Unique Photo 800-631-0300 (best prices on film - use TMX for seps)

VWR Scientific 800-932-5000 (General chemical supplier)

Photographer's Formulary 800-922-5255 (General Photographic chemical supplies)

Dupont 800-755-2930 (Jean Dunlap) Makers of Cronar film

Condit Mfg. 203-426-4110 (Warren Condit) Makers of pin registration equip.

Carolina Color and Chemical 704-333-5101 (supplier of dyes)

ICI 800-648-1926 (maker of Melenex polyester film stock - I recommend
Melenex 583, this doesn't pick up dye, and has an anti-static coating on the
back.)

Kind and Knox - 800-223-9244 (maker of Photographic gelatin)

Dr. Jay Paterson 713-768-4581 (head of Dye Transfer Co. Houston)
They are making matrix film for sale. I have had a chance to test this
film, and I find that it works quite well. They also have a very nice
paper. They are still working on a dye set at the time of this writing (Nov
'97), but they should be available soon.

You should try to buy the book :
The Dye Transfer Process by David Doubley. Condit probably still has some,
or you could write: David Doubley Box #31-5124, Detroit, MI 48231.

You will need the Kind and Knox inert photographic gelatin. Talk to Mr John
Dolphin, and he will send you a 1 lb sample. You must use an inert gelatin
for this formulation.

If you need some advice about DT printing, or matrix film coating, please
feel free to contact me:

james.browning@valley.net
Digital Mask
187 Stevens Rd.
Lebanon, NH 03766
603-448-6241
www.well.com/user/justme/