Study on the pH dependence of diffraction efficiency of phase holograms in dye sensitized dichromated gelatin

Rupak Changkakoti; Sasbry V. Pappu

doi:10.1364/AO.25.000798

Applied Optics
Vol. 25,
Issue 5,
pp. 798-801
(1986)
•https://doi.org/10.1364/AO.25.000798

Study on the pH dependence of diffraction efficiency of phase holograms in dye sensitized dichromated gelatin

Rupak Changkakoti and Sasbry V. Pappu

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Rupak Changkakoti and Sasbry V. Pappu, "Study on the pH dependence of diffraction efficiency of phase holograms in dye sensitized dichromated gelatin," Appl. Opt. 25, 798-801 (1986)

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Abstract

Dichromated gelatin is thought to be a good substitute for photographic emulsions in some uses. The results of a systematic study of the effect of the pH of the developer on the diffraction efficiency of volume holographic gratings recorded in dye sensitized dichromated gelatin are presented.

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Step	Description	Temperature	Relative humidity	Time
1.	Preparation of gelatin plates
	(i) Soak 3% wt/vol of Difco Co. gelatin into deionized water.	25°C	—	2 min
	(ii) Heat the suspension in a thermostated water bath with stirring.	50°C	—	10 min
	(iii) Add 0.5% (weight of gelatin) ammonium dichromate to the suspension and heat while stirring.	50°C	—	10 min
	(iv) Filter the solution using a fast filter paper Whatman 31.	—	—	—
	(v) Pipet out a known volume (1 ml) of solution onto a level glass plate, where the solution is con-within a glass ring resting on the glass plate. The inner diameter of the glass ring was 40 mm.	—	—	—
	(vi) Remove glass ring and dry coated slides overnight, in an atmosphere of relative humidity of <40% and room temperature.	25°C	30–40%	—
	(viii) Soak samples in Kodak fixer with hardener.	25°C	—	10 min
	(vii) Wash in deionized water	25°C	—	20 min
	(ix) Dip the samples in Kodak photo flow 600 (diluted 1:200) bath.	25°C	—	15 sec
	(x) Dry the samples overnight in a sealed box.	25° C	30–40%	—
	(xi) Bake the samples in a thermostated oven.	150°C	—	2 h
	(xii) Store samples in an environment of low relative humidity at room temperature	25°C	30–40%	—
2.	Preparation of the sensitizer solution
	(i) Dissolve 3% wt/vol of ammonium dichromate in deionized water.	25°C	—	—
	(ii) Raise the pH of the solution to pH-9 using 28% ammonia solution.	25°C	—	—
	(iii) Add 1 g of ethylene diaminetetra-acetic acid dicodium salt (EDTA)	25°C	—	—
	(iv) Add (1× 10^–3)M of methylene blue to the above and maintain the pH above 9.	25°C	—	—
3.	Sensitization of plates
	(i) Soak gelatin coated plates in methylene blue sensitizer solution.	25°C	—	10 min
	(ii) Dip in photo flow bath Kodak photoflow 600 (ratio 2:200)	25°C	—	5 sec
	(iii) Dry in a dessicator in an ammonia atmosphere (using 28% ammonia solution)	25°C	—	4–6 h
4.	Expose
5.	Development procedure
	(i) Store exposed plates in the dark for 2 days.	25°C	70–80%	2 days
	(ii) Soak the plates in 0.5% ammonium dichromate solution. (The pH of this solution is varied.)	25°C	—	15 sec
	(iii) Soak in Kodak rapid fixer with hardener (one part fixer added to two parts water).	25°C	—	15 sec
	(iv) Wash in deionized water	25°C	—	15 min
	(v) Soak ion warm water	145°C	—	3 min
	(vi) Dehydrate in 70% isopropyl alcohol and water solution	25°C	—	3 min
	(vii) Dehydrate in 100% isopropyl alcohol.	25°C	—	2 min
	(viii) Dry hologram with flowing hot air.	—		3 min

Obs. no.	Day of hologram recording

	8 Apr. 1985 (Exposure energy 545 mJ/cm²)		29 Aug. 1985 (Exposure energy 591 mJ/cm²)

	pH values	η (%)	pH values	η (%)
1	4.58	38	4.04	39.2
2	4.95	40	5.15	80.6
3	5.51	71.7	5.69	78.6
4	5.99	82.6	5.99	95.1
5	7.00	73.6	6.28	77.96
6	7.66	57.8	8.15	80.4
7	7.98	52.7	8.96	71.2
8	9.02	10.4	—	—

Step	Description	Temperature	Relative humidity	Time
1.	Preparation of gelatin plates
	(i) Soak 3% wt/vol of Difco Co. gelatin into deionized water.	25°C	—	2 min
	(ii) Heat the suspension in a thermostated water bath with stirring.	50°C	—	10 min
	(iii) Add 0.5% (weight of gelatin) ammonium dichromate to the suspension and heat while stirring.	50°C	—	10 min
	(iv) Filter the solution using a fast filter paper Whatman 31.	—	—	—
	(v) Pipet out a known volume (1 ml) of solution onto a level glass plate, where the solution is con-within a glass ring resting on the glass plate. The inner diameter of the glass ring was 40 mm.	—	—	—
	(vi) Remove glass ring and dry coated slides overnight, in an atmosphere of relative humidity of <40% and room temperature.	25°C	30–40%	—
	(viii) Soak samples in Kodak fixer with hardener.	25°C	—	10 min
	(vii) Wash in deionized water	25°C	—	20 min
	(ix) Dip the samples in Kodak photo flow 600 (diluted 1:200) bath.	25°C	—	15 sec
	(x) Dry the samples overnight in a sealed box.	25° C	30–40%	—
	(xi) Bake the samples in a thermostated oven.	150°C	—	2 h
	(xii) Store samples in an environment of low relative humidity at room temperature	25°C	30–40%	—
2.	Preparation of the sensitizer solution
	(i) Dissolve 3% wt/vol of ammonium dichromate in deionized water.	25°C	—	—
	(ii) Raise the pH of the solution to pH-9 using 28% ammonia solution.	25°C	—	—
	(iii) Add 1 g of ethylene diaminetetra-acetic acid dicodium salt (EDTA)	25°C	—	—
	(iv) Add (1× 10^–3)M of methylene blue to the above and maintain the pH above 9.	25°C	—	—
3.	Sensitization of plates
	(i) Soak gelatin coated plates in methylene blue sensitizer solution.	25°C	—	10 min
	(ii) Dip in photo flow bath Kodak photoflow 600 (ratio 2:200)	25°C	—	5 sec
	(iii) Dry in a dessicator in an ammonia atmosphere (using 28% ammonia solution)	25°C	—	4–6 h
4.	Expose
5.	Development procedure
	(i) Store exposed plates in the dark for 2 days.	25°C	70–80%	2 days
	(ii) Soak the plates in 0.5% ammonium dichromate solution. (The pH of this solution is varied.)	25°C	—	15 sec
	(iii) Soak in Kodak rapid fixer with hardener (one part fixer added to two parts water).	25°C	—	15 sec
	(iv) Wash in deionized water	25°C	—	15 min
	(v) Soak ion warm water	145°C	—	3 min
	(vi) Dehydrate in 70% isopropyl alcohol and water solution	25°C	—	3 min
	(vii) Dehydrate in 100% isopropyl alcohol.	25°C	—	2 min
	(viii) Dry hologram with flowing hot air.	—		3 min

Obs. no.	Day of hologram recording

	8 Apr. 1985 (Exposure energy 545 mJ/cm²)		29 Aug. 1985 (Exposure energy 591 mJ/cm²)

	pH values	η (%)	pH values	η (%)
1	4.58	38	4.04	39.2
2	4.95	40	5.15	80.6
3	5.51	71.7	5.69	78.6
4	5.99	82.6	5.99	95.1
5	7.00	73.6	6.28	77.96
6	7.66	57.8	8.15	80.4
7	7.98	52.7	8.96	71.2
8	9.02	10.4	—	—

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Applied Optics