Exploration of Reflection Holograms and Their Fringes With a Scanning Electron Microscope

by

Philip Brocoum, Sam Hill, Leah Soffer, and Daniel Vlasic MAS 450/854 – Holography – Spring 2003

Abstract
We investigated fringe formation in reflection holograms using a scanning electron microscope (SEM). We observed the fringes created under several shooting and developing conditions, which included pre-swelling with triethanolamine (TEA) at concentrations of 2%, 4%, 8%, and 16%, bleaching versus not bleaching, and postswelling in sorbitol at concentrations of 10% and 15%. Due to technical difficulties with SEM, the results are not included in this report.

Introduction and Background
In reflection “Denisyuk” holography the reference and object beams illuminate the film from opposite sides, producing dense parallel fringes in-line with the plate (Figure 1).

Figure 1. Reflection Hologram Setup and Fringes.

According to the theory of reflection holograms, the distance d between the fringes is λ/2, calculated from Equation 1. These layers of fringes act as mirrors creating the effect of a narrowband reflection by causing constructive interference of wavelengths near 2*d, and filtering out other wavelengths.
d=

λ , v 2 sin    2

where (ν = π)

(1)

Emulsion thickness during exposure plays a large role in how many reflection type mirror layers are created. Thicker emulsion allows for more layers, reflecting more light, and usually making the narrowband effect more pronounced. Table 1 shows the emulsion characteristics of two holographic films. In a 7µm emulsion, the typical number of expected fringes is approximately 22 when using a helium neon (HeNe) laser as the reference wavelength. Film type Size of grain Resolution Emulsion thickness nm L/mm m 90 35 3000 5000 7 7 Sensitivity at 633 nm J/cm2 1 10

10 E 75 8 E 75 HD

Table 1. Holographic Film Characteristics.

The output response of the hologram as a narrowband filter, shown in Figure 2., is determined by several factors. It heavily depends on transmission and reflection

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properties of each alternating high and low index of refraction layer in the film, which in are determined by the fringe spacing within the emulsion. The fringe spacing, in turn, is affected by the swelling and shrinkage of the emulsion before and/or after exposure. The output response is also dependent on the incidence angle of the illumination source, but that aspect we will not look into.

Figure 2. Spectral Shift of Reflected Wavelength.

Upon further inspection it is found that the central wavelength (λ2,ext) can be determined using equation 2 where (λ1,ext) is the reference wavelength during exposure, n is the average index of refraction of the film and t is the thickness of the film. The subscripts 1 and 2 refer to pre and post development of the holographic film respectively. The cosine θill, int is the angle of incidence of the illuminating beam while the cosine θref, int is the angle of incidence at which the reference beam exposed the film. Obviously if the reference and illumination beams hit the film on-axis at 0° then both cosines cancel to 1.

λ 2,ext n2 t 2 cosθ ill ,int = λ1,ext n1t1 cosθ ref ,int

(2)

If the reflection hologram is viewed on-axis and supposing there is no swelling, the hologram should reflect light that corresponds to the wavelength of the reference source. Under these viewing conditions it should be possible to use either the reference laser or a broadband white light source for illumination. However, once the reflection hologram is viewed off axis or any form of swelling or shrinkage has taken place, the reflected light will have changed. λ2 and its narrowband region will have shifted significantly. In many cases the use of the reference laser as an illumination source is impossible since it may not fall within the full width half maximum (FWHM) of the narrowband region. It is possible the beam may fall within the narrowband spectrum but below the FWHM region, resulting in a reflected image that is too dim for viewing. .

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When the viewing angle is off-axis the color of the reflected image is blue shifted from the original reference wavelength. This shift is a result of a decreased time delay as the light is reflected between adjacent hologram layers. On the other extreme the reflected color can be red shifted when the emulsion is swelled. This change in wavelength corresponds to the fringes moving further away as the film absorbs moisture and increases in thickness. This phenomenon works entirely the same for shrinkage but now the color is blue shifted because the fringes in the emulsion move closer together. Most holographers can only afford one laser, which makes it desirable to use these properties to their advantage. Luckily, the levels of shrinking and swelling of the emulsion can be controlled chemically. Triethanolamine (TEA), which is thick and oily can be mixed in different concentrations with isopropanol and water to swell emulsions prior to exposure. The TEA concentration is washed out either in the developer or the water pre-wash. Using TEA also increases the photosensitivity of the emulsion, creating brighter holograms. Smith and Cvetkovich [1984] showed the characteristic response to reflection holograms for various concentrations of TEA and the resulting color shift and the output bandwidth for a reference/object wavelength of 633nm. It is clear that concentrations must stay roughly to 20% at most because the human visual system has a hard time perceiving colors at 421nm, which is seen with a TEA concentration of 23%.
Table 2. TEA data.

Color λ peak [nm] 646.5 641.5 617.5 604.5 587 565 547 520 505 485 475 462 450 439 431 427 421

TEA concentration 5 min treatment [%] No soak Water only 1.96 3.8 5.6 7.4 9.1 10.7 12.2 13.7 15.2 16.6 18.0 19.3 20.0 21.8 23.0

Bandwidth [nm] 29 27 27 27 25 22 22 20 18 17 17 19 19 22 19 22 21

Processing: GP62 + PBQ Bleach Results taken from The Smith and Cvetkovich pseudocolor procedure. (Recording wavelength 647nm).

Both developer and bleach cause the emulsion to shrink. Therefore, some holographers use sorbitol solutions to swell the emulsion after the hologram has been developed. In the same way the TEA concentration can be

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varied, the sorbitol concentration can be mixed to control swelling and color output, as shown in the following graph. Saxby [1994] recommends a sorbitol concentration between 5% and 20%.

Figure 3 Effects of sorbitol concentration on output wavelength

In the world of holography very little has been done to examine the fringes created from reflection holograms in any condition such as swelling or post swelling. There was a study of transmission hologram fringes by Agaki et al. [1972] that used a transmission electron microscope (TEM) to observe the cross section of Kodak 649F when processed as both an amplitude and phase hologram (see Figure 4). There was also a cross section of a phase hologram made on Scientis 14C76 film.

Figure 4. Electron micrograph of hologram cross-section. Picture printed without permission.

The phenomenon we are interested in exploring is the swelling and shrinking of the emulsion. In particular, we are interested whether the emulsion, and thus the fringes,

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shrinks linearly or non-linearly. This is important because the uniformity of the mirrored surfaces will affect the diffraction efficiency and bandwidth of the reflection hologram, influencing hologram brightness and sharpness. Ideally, we would like to use a TEM, but since we do not have access to one at present, our objectives will be met with a weaker scanning electron microscope (SEM), which has the resolution of a few nanometers.

Experimental Procedure
To create our holograms, we used a standard and simple reflection hologram setup. We took an object as seen in Figure 5 and exposed several films that had been preswelled with various concentrations of TEA. We developed the films both with and without bleaching, and also performed post-swelling with various concentrations of sorbitol. Pre-swelling: As a first step, four solutions were prepared with TEA concentrations of 2%, 4%, 8%, and 16%. The TEA was pre-mixed by the lab supervisor. A piece of 4x5 8E 75 HD Agfa Holotest film was placed in each solution for 2 minutes, removed, squeegeed, and dried. A fifth piece of film was used as a control in the experiment and was not soaked in a TEA solution. Shooting:

coin

Aluminum Block
egg

Figure 5. Object.

A large aluminum block was used as a reflecting surface placed behind the holographic plate. It also served as a means to mount the object. The object consisted of two items: a half dollar mounted on the upper half of the block, and a reflective plastic egg below it. These two items were chosen due to their simple geometric forms, and to contrast a flat object with one containing more depth. The equipment was arranged as depicted in Figure 6: a reference beam was spread with a 20x objective and cleaned with a spatial filter at a distance of 142cm from the plate. It closed an angle of 50° with the plate’s normal.

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Object

H1

50o

LPS Shutter Laser (633nm)
Figure 6. Setup diagram for reflection hologram

An average light intensity of 60 µW was measured. Given a film sensitivity of 60 µWs/cm2, an exposure time of 1 second was used. First, the film without TEA swelling was exposed and developed to ensure proper exposure length. Then, the remaining four films were exposed and developed. For each piece of film, a notch was cut off of the top left corner as a means to later orient the film. Developing: To develop the film, Pyro A and B were used. Each piece of film was put in the developer for 3 minutes. After developing, the film was put in a water wash for 5 minutes. Then, the film was cut in half vertically, as show in Figure 7, and a notch was cut off the top right corner to mark the second piece. The right half was left in the water wash for another 5 minutes. The left half was put in bleach until clear plus 30 seconds. Then the left half was put back in the water wash for another 10 minutes.

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Bleach

|

No Bleach

Sorbitol
10% 15% 15% 10%

2% 4% 8% 16%
Figure 7. Film sample breakdown

Both pieces of film were then cut in half horizontally, with notches cut from the bottom corners, as shown in Figure 7. The top left and right quarter were hung to dry. The bottom quarters were cut diagonally, with additional notches cut to uniquely mark the upper triangles. Sorbitol was mixed with dionized water in two concentrations: 10% and 15% sorbitol. The smaller triangles were placed in the 10% sorbitol solution for 2 minutes while the larger triangles were placed in the 15% sorbitol solution for the same amount of time. Then all of the triangles were removed, rinsed briefly in a water wash, and placed in Photoflo for 2 minutes. After that, the triangles were squeegeed and hung to dry. Analyzing: Finally, the holograms could be viewed under the ESEM using the following procedure: First, clean the films with 100% methanol by gentle padding with a lens cloth. Second, cut a small sample from each piece of film with a microtome to get a clean edge. Sections from the middle of the hologram where the image is located should be examined, because they contain the strongest fringes. To analyze each sample, mount the film to the stand within the ESEM, noting which side has the emulsion. Close the ESEM chamber and turn on the pump to create a vacuum in the chamber. Then turn on the electron beam to a low voltage to prevent destroying the sample, and focus on the emulsion side of the sample. Photograph the sample once in focus, turn off the electron beam, and vent the chamber. For stereo pairs, another image should be taken rotationally or linearly away from the first image.

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Results
Due to unforeseen circumstances, we were unable to use the ESEM for more than a couple of hours, during which we were also trained. Therefore, we could not experiment enough to find and capture the fringes. On the good side, however, we learned how to prepare the samples and operate the ESEM, as well how to avoid the any mistakes we have made. We did take several snapshots of the cross-section of unbleached, 0% TEA film, only one of which was saved (Figure 8).

Figure 8. Cross-section of unbleached, 0%TEA film under ESEM. The light layer is the emulsion, to the left of which is the film sheet.

During our session, we have noticed that the electron beam operating at 30kV is damaging our sample. Both the emulsion and the plastic melt under the generated heat. Since gelatin is very sensitive, we will run our future experiments at 4kV, as suggested by researches with a lot of SEM experience. We might also coat our samples in gold, which is a standard approach taken by material scientists to preserve the sample. We plan to spend more time viewing the holograms and hopefully photographing the fringes. We will attach them to this report as they become available.

Conclusion
We believe the approach and setup for detecting fringes was executed very well. Pre-planning and proper organization allowed the holographic exposure and film development to go smoothly. It also allowed the group to fulfill one of the primary

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objectives in this course and the final project, which is displaying the proper method to organize and follow through on a scientific experiment in a laboratory environment. Our goal to see fringes is still under investigation and, if circumstances permit, we will attach all SEM images to this report. Our approach, however, allowed us to see and document the areas in the project that could be improved upon in case further work is carried out. In future experiments we would like to create the holograms using a planar mirror as the object, which would produce more prominent and straight-line fringes. We would also like to measure the emulsion thickness due to swelling prior to exposure, as a reference data point. Furthermore, to obtain consistent data measurements, we would analyze several more samples. Lastly, we would like to examine the effects of pre- and post-swelling due to chemicals other than TEA and sorbitol.

References
Akagi, Motoo, Tadao Kaneko, Tsutomu Ishiba (1972). Electron micrographs of hologram cross sections. Applied Physics Letters 21 (3). Geola uab and Slavich OAO (2003). Sorbitol graph http://www.slavich.com/vrpm.htm . Author unknown. Kahn, Bruce. Rochester Institute of Technology, Rochester, NY. Department of Imaging and Photographic Technology. Course: SEM. http://www.rit.edu/~bekpph/sem/ McGrew, Stephen P. (2001). Color control in dichromated gelatin reflection holograms. New Light Industries, Inc. http://www.nli-ltd.com/publications/color_control.htm Saxby, Graham (1994). Practical Holography – Second Edition. Prentice Hall, London, pp. 518-519. Smith, Steven L. and Thomas Cvetkovich (1984). Multi-color holography with a single frequency laser utilizing triethanolamine as a pre-exposure agent. SPIE Vol. 462 Optics in Entertainment II, pp. 8-13.

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