submitted to Leonardo, January, 1991.

 

                                                   A TOAST TO NICK PHILLIPS

 

                                                                      Ed Wesly

 

                                                     Center for Photonics Studies

                                                            Lake Forest College

                                                        555 North Sheridan Road

                                                       Lake Forest, Illinois, 60045

                                                                           and

                                           The School of the Art Institute of Chicago

                                                       280 South Columbus Drive

                                                              Chicago, IL 60603

 

                                                                   ABSTRACT

            The Art of Holography requires bright holograms with good signal to noise ratio.  A gentleman who pioneered techniques in silver halide holographic material processing to make reflection holograms that are imminently viewable is profiled.

 

                                                                         TEXT

            Silver halide based photographic materials were used to record the first holograms of Gabor, Denisyuk, Leith and Upatnieks. They will probably remain useful in holography forever, due to their high sensitivity at all parts of the visible spectrum, compared to the other choices, which lag an order of magnitude or two behind.  Because of this, they will continue to be the medium of choice for the self-supporting holographic artists with their small lasers.

            In the beginning, holographic processing followed basic photographic conventions; develop, stop, fix, wash, wetting agent, dry.  But there was not much hope for bright holograms in this manner, especially the reflection type, since the blackened developed silver would absorb much more of the light than what it diffracted.  Bleaching techniques were suggested by Cathey in 1965[1], and this resulted in a plethora of papers, many peddling not just the proverbial snake oil, but ferricyanides and mercuric chlorides.

            A paper which remains a classic to this day is "An Advance in the Processing of Holograms"  by N. Phillips and D. Porter[2]. They introduce the use of a concentrated photographic developer, Neofin Blue, as a developer for pulsed holography.  Neofin Blue is not only expensive, but hard to obtain, so its use has been superceded by special formulations.  More importantly, this paper introduces a relatively benign oxidizing agent, Ferric Nitrate, in a bleach used after fixing to rehalogenate the developed silver in the bright fringe areas of the holographic pattern into silver bromide.  This bleach was gentle to the gelatin, avoiding the formation of noise due to surface relief, plus it was observed that ferric nitrate also had hypo clearing agent capabilities.  It also incorporated a desensitizing agent, phenosafranine, to cut out printout, while also inhibiting grain growth to noisy levels.  This seems to still be the favorite bleach of white light transmission holographers[3].

            But Dr. Phillips' next big paper, "Advances in Holographic Bleaches"[4], introduced a new concept of bleaching to coincide with the introduction of Agfa's new line of improved Holotest Emulsions, namely the HD series with the reduction in grain size from the previous 50 down to a nominal 35 nanometers.  By rehalogenating the oxidized silver directly after development and skipping the fixing step, dramatic increases in brightness could be achieved.  What is most remarkable about this process, and a tribute to Dr. Phillips' genius, is that conventional photographic wisdom would dictate that this type of system should not work!

            Holographic plates start off with a homogenous distribution of silver bromide grains in them, and if all the developed silver were changed back into its original form, the plate should then regain its virgin condition, and there would be no modulation of the incoming reconstructing light since there is nothing to differentiate where a bright fringe had been as opposed to where the dim ones had been.  But this process works really well, and the theory is that the developed grains migrate into the dim fringe areas as they are being rehalogenated. The bright fringe areas are represented by pure gelatin, and the dim fringe areas contain silver bromide, but there is now more modulable material in those areas so that efficiency is high.  Since nothing left the emulsion, things only having been rearranged in there, the original thickness of the layer is preserved along with the spacing of the fringes during recording, so that it is not only possible to replay a reflection hologram with the laser that made it, but to be able to replace the hologram back onto the object and generate real-time interferometric fringes with it!

            At first I thought that this migration-diffusion mechanism was unreasonable, but it was proven to me when I was making some extremely low frequency gratings.  They had fringe spacing of about 2 line pairs per mm; these fringes are visible to the naked eye.  I made my first exposure test, developed and bleached without fixing, and discovered almost no diffraction while wet.  It dried while I was interrogating it with the undiverged laser beam, and I could see in the woodgrain caused by internal reflection between the two glass surfaces an excellent red Lippmann mirror.  The process made a better hologram of the back of the glass than it did of the coarse interference system!

     The simple grating had a fringe spacing of 100 's of microns; the reflection grating's spacing had fringes about 300 nanometers apart, which is three orders of magnitude difference.  If it were true that the silver grains were swimming from bright fringe to dim fringe as they rehalogenated, then this mechanism would be more effective in travelling short distances rather than longer ones.

     Develop ‑ rehalogenating processes then have a lower limit of useful spatial frequency, and don't really come into their highest efficiency until about 1000 lines per millimeter, as papers by Hariharan[5] and Ward[6] show.  Benton had also predicted these effects when writing about his IEDT processing[7], which shifts the unexposed silver grains which had been in the dim fringes over to the developing bright fringe grains.  But gratings with fringes so large that they are visible to the eye are extreme cases; certainly the process functions well on the size of fringes formed in the transmission mode by an object placed along the normal to the plate and a reference at 45 degrees from the normal. The lack of low spatial frequency response aids in the suppression of intermodulation noise from the object's light interfering with itself.  The fringes formed by points on the object are very widely spaced for points immediately next to each other, and are at their minimum for the interference caused by the extreme ends of the object, but rarely are these fringes as tiny as the reference ‑ object fringes.  The process will tend to ignore these coarse noise fringes and strengthen the more closely packed holographic ones.  Bullseyes caused by dirt on optics will be less apparent on the developed - rehalogenated holograms as the processing makes them lower contrast.  Ditto for the dreaded woodgrain. It is strange to think of a holographic material's modulation transfer function being at zero for the low spatial frequencies, then climbing to a peak in the 1000's of line pairs per millimeter then falling off.  But silver halide materials processed in this mode are not alone in this respect, as DuPont's Photopolymers which work by a diffusion mechanism also exhibit this effect, with products manufactured specifically for reflection or transmission work.

     The trick is that the rehalogenation must be performed in aqueous solutions for the diffusion of the silver to take place. For if the developed holographic plate is rehalogenated by Bromine Vapor a` la Thiry[8] or Graube[9], there can be no "swimming" of silver bromide from one area to the other, so that the plate does return to it original consistency.

     This subtle phenomenon can only work with extremely fine grained holographic or Lippmann-type emulsions.  To illustrate how un-obvious Phillips' method is, not one of the researchers in Lippmann photography at the turn of the century, including some of the greatest minds in photographic research ever even attempted this simple experiment.  For if they had, they could have solved one of the basic processing problems of Lippmann photography, that of retaining emulsion thickness to preserve color veracity.  Most Lippmann photographers either developed to colloidal silver, or developed, fixed, and bleached in Mercuric Chloride and used some plumping agent in the emulsion to bring it back to its original thickness.  But with Phillips' scheme, all the modulable material has been rearranged in the layer, with none leaving, so there is no shrinkage of the fringes to shorter wavelengths.  It will be interesting to see if there will be any renewal of Lippmann experiments using these new processing techniques, other than those of Dr. Phillips himself[10],[11]. 

     The proof of the processing is in the holograms, and holograms processed this way helped account for the success of the Light Fantastic shows in the late seventies, which acquainted the general public with extremely realistic images thanks to the high brightness and black shadows due to the low signal to noise ratio.  The second PBQ bleach mentioned in reference 4 was adopted by John Kaufmann[12], the dean of triethanolamine color control, in combination with Kodak D-19, as his basic process.  If not using Dr. Phillips' recipes verbatim, most workers have adopted the develop-rehalogenation scheme.

     The eradication of the fixing step also eliminated the characteristic odor of hypo (thiosulfates) which has been the bane of photographic darkrooms since the days of Daguerre.  It is an unpleasant smell for most people, and some are outright allergic to it. It is also unhealthy for bleached holograms, since it is a solvent for silver halides, which are the modulation ingredient in the holographic layer.  Even the airborne particles which account for the smell are capable of ruining a perfectly good hologram.

     But Dr. Phillips has been criticized by the safety conscious for having introduced an even nastier smelling chemical, the dreaded PBQ, (p-Benzoquinone), which is what the developing agent hydroquinone oxidizes into as it gets spent in the process of reducing silver bromide crystals into elemental silver. It is certainly a powder from hell when it comes to mixing.  Its very fine dust inflames the sinuses and dries out the eyes.  Certainly personal air masks with organic filters help, and some workers have made spare shower stalls into fume hoods to control the hazard[13].  It takes a very long time to dissolve, and the bleach has a covered tray life of a few hours.  It can't be left uncovered, as it oxidizes into uselessness even quicker, but more importantly, even the solution reeks.  So he then formulated a rehalogenation/diffusion bleach based around Ferric EDTA (EthyleneDiamineTetraAceticacid) as the oxidizing agent, which is the one commonly used in color photographic processes because it is ecologically benign[14]. 

     Ilford came out with a new blue-green sensitive silver halide holographic recording material, and he eliminated their problem of splash marks[15]. The plates were developing splotchily, as the solution did not penetrate the entire coating evenly and  simultaneously, and the developer darkened some areas more than others.  By using a restrainer in the developer to hold off developing activity for about a half-minute after immersion, until the light-sensitive coating was totally full of it allowed much more even development.

     His next processing publication[16] fine-tuned the Ferric EDTA formula with a "No Patchy Haze" version of this bleach, which cuts down local variations in surface scatter.  But the paper he delivered at Budapest for the celebration of the 100th birthday of Dennis Gabor[17], introduced the greatest improvement in holographic materials' processing since the invention of PBQ.

     After having been impressed by the high signal to noise ratio of Russian colloidally-developed silver halide materials in 1979, he tried processing Agfa Holotest materials in Russian style developers.  These solutions reduce the exposed silver halide crystals into red silver, which get their color from being small compact grains instead of the long filamentary strands of the black silver which is the typical product of development.  This type of developer works very well with the Soviet style materials with their extremely tiny grains, which are about a third of the diameter of those in the Agfa plates.  Since scatter is proportional to the fourth power of diameter, Russian plates have less than 1% of the scatter of Western ones.  Because of these small grains, Russian plates look as clear as glass, since they do not have the large scattering sites which gives a soft ground glass look to the usual plates.  There is less haze in recording and in replay, contributing to blacker shadows, which adds significantly to the solidity of the object holographed.  However, since sensitivity is proportional to the third power of diameter, Russian materials need almost 100 times the exposure of regular plates!

     The Agfa plates were not responding well to the single step colloidal developers, and since he was getting such high efficiency with black silver development followed by rehalogenating bleaches, he decided to change the rehalogenated silver bromide into colloidal silver, with a highly diluted developer.  The plate is exposed to light to the saturation point but not enough to cause solarization or to the point of printing out, then immersed in the weak developer formula without any agitation.  The soup breaks down This was Font/Pitch 1,10 - Off.Note:  The change to pitch (13) and font (1) must be converted manually.the large highly scattering silver bromide into little rocks of colloidal silver.  There is quite an appreciable increase in signal to noise, so much so that true color holograms that the author made with red 633 nm, green 515 nm and blue 476 nm on a single 8E75HD[18] would not have worked at all if not for this trick.  The blue image would have been buried in the blue scatter noise of the Agfa emulsion.


     The original colloidal developing formula, which I had dubbed in the beginning "Reddeveloper", a pun on red developer and redeveloper, and now call the "Blood Bath" because of the characteristic dried blood red color of the finished plate, had six ingredients.  But in a slightly later version of reference 19[19], he simplified the step to a simple 1% solution of ascorbic acid.  This is quite remarkable, as there is no alkali to provide the proper pH to activate the developing agent, and the bath runs at a pH of about 3.  Again, this goes against the grain of conventional wisdom. 

     Not only does this increase the signal to noise ratio of the Agfa and Ilford plates to a level comparable to that of soviet style materials, it also prevents the dreaded printout.  Colloidal silver is fully oxidized, like the black silver in a conventional black and white photographic negatives and prints, and will not change on its own like an unstable silver halide.  Holographers looking for that "hologram as a crystal clear window" effect might be daunted by the red color of the emulsion, which unfortunately filters out a bit of the blue and green end of the spectrum, but then again they may take comfort in the fact that the hologram will be archival, and will not change its color over time.

     Currently Dr. Phillips and Hans Bjelkhagen are researching new formulations of bleaches which create PBQ in the solution by oxidizing hydroquinone with potassium persulfate.  PBQ as an oxidizer does have its advantages over the others, especially in regards to efficacy, as two grams per liter of PBQ does the same job in the same amount of time as 30 grams of Ferric EDTA, ferric nitrate, potassium ferricyanide, mercuric chloride, or copper sulfate.  Plus it also tans or hardens the gelatin, preventing the shrinkage that often occurs with the other oxidizers, especially Ferric EDTA.  Their formula, which they have dubbed PBU, (Phillips-Bjelkhagen Ultimate), does not have the nasty odor of PBQ, yet works identically.

     So I propose a toast to the gentleman who has done the most in inspiring us all in the creation of high quality reflection holograms, and who has thrown off the bondage of "commercial ties" to give us the knowledge to get the maximum results of the materials, so that the medium can progress, cheers to our friend, Nick Phillips.

     Who knows what may follow?  A special monobath, with a developing agent that changes the silver bromide into black silver but whose spent by-product oxidizes the developed silver so that it could be rehalogenated and diffused back to a silver bromide phase hologram but then the by-product of the oxidizer becomes a weak developing agent to change the silver bromide into a colloidal silver?  That would be nice.  But if that doesn't come, surely the legacy of Nick Phillips will include the perfection of the processing of holograms.

 

THE FORMULAE

(IN THE ORDER OF PRESENTATION)

 

ORIGINAL FERRIC NITRATE FORMULA

           20 g  Glycerol

        500 ml Deionized Water

        500 ml Isopropyl Alcohol

        300 mg Phenosafranine

        150 g  Ferric Nitrate

          33 g  Potassium Bromide

     Dilute 1 to 4 with water before use.

     Bleaching time: One and a half times the time it takes to clear.

     Temperature:  20C                                                                                                          Agitation:  Intermittent

For rehalogenation after fixing.  Hans Bjelkhagen prefers this over the simpler GP 431 formulation for pulsed masters developed in Neofin Blau diluted 1:1.

This stock solution lasts indefinitely, working solution about one week.

Source:  N. J. Phillips and D. Porter, "An Advance in the Processing of Holograms,"  Journal of Physics E: Scientific Instruments 9, 631 (1976). 

 

GP 431

        150 g  Ferric Nitrate (9-Hydrate)

          30 g  Potassium Bromide

           .3 g  Phenosafranine (Optional)

     One litre Water

     Dilute 1 to 4 with water before use.

     Bleaching time: One and a half times the time it takes to clear.

     Temperature:  20C                                                                                                          Agitation:  Intermittent

The most enduring of the classical bleaches.  The phenosafranine may need to be dissolved in an alcohol before adding to the stock solution or in a bit of very hot water. 

This stock solution lasts indefinitely, working solution about one week.

Source:  Agfa Gevaert Technical Information Bulletin 21.7271(480).

 

GP 432

       50 g  Potassium Bromide

      1.5 g  Boric Acid

      2 g  p-Benzoquinone added just before use.

     One litre water

Source:  N. J. Phillips, A. A. Ward, R. Cullen, D. Porter, "Advances in Holographic Bleaches," Photographic Science and Engineering 24, 120 (1980).  Also Agfa Gevaert Technical Information Bulletin 21.7271(480).

 

PBQ #3

     30 g  Potassium Bromide

     15 g  Borax

      2 g  Potassium Dichromate

      2 g  p-Benzoquinone added just before use.

     One litre water

Bleaching time: One and a half times the time it takes to clear.

Temperature:  20C                                                                                                     

Agitation:  Intermittent

This is the bleach that John Kaufman uses with Kodak D-19 as the developer.

Source:  N. J. Phillips, A. A. Ward, R. Cullen, D. Porter, "Advances in Holographic Bleaches," Photographic Science and Engineering 24, 120 (1980)

 

"BENIGN" Fe EDTA

     ORIGINAL                                                                                                                REVISED

     30 g  Ferric Sulfate                                                          30 g  Ferric Sodium-EDTA

     30 g  di-Sodium EDTA                                                        

     30 g  Potassium Bromide                                                    30 g  Potassium Bromide      10 ml Sulfuric Acid (Conc.)                                                       30 g Sodium Bisulfate                            

One litre water                                                                                         One litre water

Bleaching time: One and a half times the time it takes to clear.

Temperature:  20C                                                                                                     

Agitation:  Intermittent

Less hazardous to work with than the dreaded PBQ.  Either version of the recipe gives the same result, the choice depending on the availibility of the ingredients.  Leaving the solution exposed to air (uncovered tray) will extend the lifetime of the oxidizer.

Source:  Nicholas Phillips, "Benign Bleaching for Healthy Holography", holosphere, Volume 14, Number 4, p.21, (1986)

 

NICK'S #5

                      PART A                                                                                                   PART B

     60 g  Sodium Sulfite                                                             20 g  Sodium Metaborate          

     20 g  Catechol                                                                      120 g  Sodium Carbonate

     10 g  Hydroquinone                                                                               One liter water

     10 g  Potassium Bromide

     One litre water

                           Mix equal parts together before use.

Development time:  Four to five minutes

Temperature:  23C +- 1C                                                                                          

Agitation:  Constant

Primary recommendation for transmission holograms on Ilford green-sensitive materials, followed by a rehalogenating-diffusing bleach. Properly exposed plates will wait thirty seconds before showing signs of development.

Part A can last a month in a tightly stoppered bottle; Part B can last indefinitely.  The combined solutions can last a day in a covered tray.

From:  Nicholas J. Phillips, "The Silver Halides - the Workhouse of the Holography Business", Proceedings of the International Symposium on Display Holography, Volume III, 1988, p.35.

 

NICK'S #6

                      PART A                                                                                                   PART B

     10 g  Pyrogallol                                                                  20 g  Sodium Metaborate

     10 g  Potassium Bromide                                                   120 g  Sodium Carbonate

     One liter water                                                                                    One liter water

Developing time:  Five minutes

Temperature:  23C +- 1C                                                                                          

Agitation:  Constant

Primary recommendation for Ilford green-sensitive materials for same wavelength replay in the reflection mode when followed by a rehalogenating bleach.  SP737T will work in this brew but at a stop loss in speed.  A properly exposed plate will sit in this brew for a half a minute before any darkening appears.

Tray life of the combined solutions is about 15 minutes, Part A will last two or three days in a full stoppered bottle, but Part B will last indefinitely.

From:  Nicholas J. Phillips, "The Silver Halides - the Workhouse of the Holography Business", Proceedings of the International Symposium on Display Holography, Volume III, 1988, p.35.

 

"NO PATCHY HAZE"

     12 g Ferric Sulfate

     12 g di-Sodium EDTA

     30 g Potassium Bromide

     50 g Sodium Bisulfate

     One litre of water

     Bleaching time: To clear plus one minute.  (Usually in excess of six minutes!)

     Temperature:  20C                                                                                                

Agitation:  None

A slow, diluted Fe EDTA bleach which eliminates non-uniform scattering patches throughout the emulsion.  The key to success is to avoid the urge to agitate, as this one can take up to fifteen minutes to clear a well-exposed plate.

Source:  Nicholas Phillips, "New Recommendations for the Processing of Ilford Plates", handout at Lake Forest College Holography Workshop II, July 1989.

 

REDDEVELOPER #1

     10 g  Sodium Sulfite (Anhydrous)

      5 g  Hydroquinone

     10 g  Ascorbic Acid

     23 g  Potassium Phosphate (mono)

     30 g  Sodium Carbonate

     One litre distilled water.

Dilute 1 part developer to 40 parts distilled water, otherwise there will be a patchiness to the final hologram.

Re-expose plate to UV or visible light and develop for five minutes with the lights on.

Source:  Nick Phillips, "Bridging the Gap Between Soviet and Western Holography", Proceedings SPIE, Conference in Hungary, in press.

 

REDDEVELOPER #2

     10 g  Ascorbic Acid

     One litre distilled water.

Re-expose plate to UV or visible light and develop for four minutes with the lights on.

Source:  Nick Phillips, "Bridging the Gap Between Soviet and Western Holography", Handout at Lake Forest College Holography Workshop II, July, 1990.

 

 

                                               ENDNOTES



[1]. W. T. Cathey: "Three-dimensional wavefront reconstruction using a phase hologram", J. Opt. Soc. Am. 55, 457 (1965)

[2]. N. J. Phillips and D. Porter, "An Advance in the Processing of Holograms, "Journal of Physics E: Scientific Instruments 9, 631 (1976).

[3]. R. Berkhout, "Working with Kodak Plates 120-01, Making White Light Transmission Holograms", Proceedings of the International Symposium on Display Holography, Volume III, T. Jeong, Editor, Lake Forest College, (1988)

[4]. N. J. Phillips, A. A. Ward, R. Cullen, D. Porter, "Advances in Holographic Bleaches," Photographic Science and Engineering 24, 120 (1980)

[5]. P. Hariharan, C.M. Chidley: "Rehalogenating bleaches for photographic phase holograms.  2: Spatial frequency effects", Appl. Opt. 27, 3852-3854 (1988)

[6]. A. A. Ward, L. Solymar: "Diffraction efficiency limitations of holograms recorded in silver-halide emulsions", Appl. Opt. 28, 1850-1855 (1989)

 

[7]. Stephen A. Benton in Handbook of Optical Holography, H. J. Caulfield editor, Academic Press, 1979, New York.

[8].  H. Thiry: "New technique of bleaching photographic emulsions and its application to holography", Appl. Opt. 11, 1652-1653 (1972)

[9].  A. Graube: "Advances in bleaching methods for photographically recorded holograms", Appl. Opt. 13, 2942-2946 (1974)

[10]. N.J. Phillips, H. Heyworth, T. Hare: "On Lippmann's photography", J. Photogr. Sci. 32, 158-169 (1984)

[11].  N.J. Phillips, R.A.J. van der Werf: "The creation of ef­ficient re­flective Lippmann layers in ultra-fine grain silver halide materials using non-laser sources", J. Photogr. Sci., 33, 22-28 (1985)

[12]. John Kaufman, "Previsualization in Pseudo-Color Holography", Proceedings of the International Symposium on Display Holography, T. Jeong, editor, Volume I, (1982).

[13]. The West Coast holographer Robert Hess's apartment when he lived in Silicon Valley circa 1985.

[14]. Nicholas Phillips, "Benign Bleaching for Healthy Holography", holosphere, Volume 14, Number 4, p.21, (1986)

[15]. Nicholas J. Phillips, "The Silver Halides - the Workhouse of the Holography Business", Proceedings of the International Symposium on Display Holography, Volume III, 1988, p.35.

[16].  Nicholas Phillips, "New Recommendations for the Processing of Ilford Plates", handout at Lake Forest College Holography Workshop II, July 1989.

[17].  N. Phillips: "Bridging the gap between Soviet and western holography", Proceedings of the SPIE (1990) in press.

[18]. E. Wesly, T. Jeong, "Progress in True Color Holography", Proceedings of the SPIE, Vol. 1211, 1990.

[19].       Source:  Nick Phillips, "Bridging the Gap Between Soviet and Western Holography", Handout at Lake Forest College Holography Workshop II, July, 1990.