Iridescence at the Nanoscale


Raymond Yu
ryu5@u.rochester.edu
University of Rochester
The Institute of Optics

Iridescence is a common phenomenon that utilizes the fundamentals of wave optics. As light interacts with periodic structures, it diffracts. Depending on the wavelength of light, the angle at which the light is diffracted will change. Therefore, a surface that has periodic sub-wavelength structures or thin films will produce a rainbow or multicolor like reflection that changes with the viewing angle. Examples of artificial iridescence are depicted below with a reflective diffraction grating and thin film interference.

(a)Reflective diffraction grating (Citation)

(b)Thin Film Interference (Citation)

Common objects that has this iridescence property are shells, scales, insect wings, gemstones, and CDs. In the following, we will be examining iridescence of an abalone shell, bug wing/scale, peacock feather, and a piece of a CD. To investigate this property, a scanning electron microscope can reveal topological details at the nanoscale.

In an electron microscope, an electron beam strikes the surface of a sample to generate signals for generating an image. The electrons penetrate through the substrate and forms a tear drop shape that results from the interaction between the accelerating electrons and the atoms of the material. From this interaction volume, we have electrons that are ejected off due to elastic or inelastic collision. At the very surface, we have auger electrons, then secondary electrons, and back scattered electrons. Lastly, we also have X-ray emission from the deepest region of the interaction volume. The deeper the electrons originate from, the stronger the electron energy must be to penetrate through the material

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Light Microscopy

Light microscopy is the most common microscopy technique that yields color and depth information of our sample. After preparing small pieces of our sample, we imaged them under the microsope at 10x and 20x. Due to surface uneveness, we imaged our sample at low magnification to keep a long depht of focus.

(a) Image of abalone shell taken at 10X.

(b) Image of an unknown bug wing taken at 10X .

(c) Image of the green section of a peacock feather taken at 10X.

(d) Image of CD bits taken at 20X.

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Sample Preparation

For the SEM microscope to create stunning and informative sample images at high resolution, the samples must be adequately prepared for the hostile vacuum environment and electrical potential of the target chamber. Samples need to be properly coated to ensure that the charge from the electron beam is grounded away, preventing deleterious artifacts from forming. Fortunately, our samples are dry and does not require drying methods such as critical point drying or HDMS drying.

(a) Image of a Denton Vacuum gold sputter coater used for sample preparation
(b) Samples (left to right, top to bottom) of abalone shell surface, CD, abalone shell cross-section, peacock feather, and bug wings were mounted onto a stub and coated with gold

The samples that we are investigating was coated using the gold sputter coater shown in figure (a). The sample stub was placed in the bell jar and the system started. The system was then repeatedly pumped down to approximately 100 mTorr with a rotary pump, backfilled with argon gas, and pumped down again. After six repetitions the system was pumped down to ~75 mTorr. At this level, 15 mA of current was run through the cathode for 90 seconds and a gold layer of ~100 Å was deposited. It was noted that during the sputtercoating the pressure in the chamber rose slightly due to the presence of the gold ions. Finally, our coated sample is shown in figure (b), with 2 samples of the abalone shell and a sample for the CD, peacock feather, and bug wing. The gold can be visibly seen from the reflection off the aluminum stub.

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Secondary Electron Imaging

Secondary electron imaging is one of the most common SEM techniques. Using a Everhart-Thornley detector or an InLens detector, we can collect secondary electron signals at each point of the scan and record surface topology signals to form our image. The following are secondary electron images of our abalone shell, bug wing/scale, peacock feather, and CD sample.

(a) SE micrograph of an abalone shell surface recorded at 1 keV and 1.55 K X with an InLens detector

(b) SE micrograph of a tilted abalone shell surface recorded at 10 keV and 4.60 K X with a SE2 detector

(c) SE micrograph of an abalone shell cross-section recorded at 10 keV and 2.77 K X with a SE2 detector
(d) SE micrograph of an abalone shell cross-section recorded at 10 keV and 12.01 K X with a SE2 detector

The above four images are scanning electron micrographs of our abalone shell sample. Although the colorful iridescence is seen on the surface of an abalone shell, the origin of this effect is from the layers of nacre underneath. As seen from the SEM images in (a) and (b), the surface of an abalone shell is contaminated, rough, and unorganized. However, if we take the shell and mount it such that the thin cross-section is exposed to the electron beam, we can record and image of the thin layers with in. Surprisingly, I was able to find hundred of layers of nacre while recording image (c). The broken pieces of nacre are a result of uneven breakage of the shell layers while attempting to create a sample. Using ImageJ, I was able to measure individual layer thickness between 390-420 nm in image (d). From this, we learn that abalone shell uses thin film interference to create an iridescence effect and that abalones work very hard to create so many layers!

(a) SE micrograph of a bug wing surface recorded at 4 keV and 7.93 K X with an InLens detector

(b) SE micrograph of a moth scale surface recorded at 4 keV and 5.51 K X with an InLens detector

(c) SE micrograph of a butterfly scale surface recorded at 4 keV and 2.29 K X with a SE2 detector
(d) SE micrograph of a butterfly scale surface recorded at 10 keV and 16.87 K X with a SE2 detector


Next, we have our bug sample that is a wing of an unknown insect. Under light microscopy, we were able to observe contamination from other insect scales which proves to be a benefit as I was able to record more images. The first image (a), is the surface of the large unknown insect wing. The patterns on the wing are 150-180 nm sized spores/bumps covered by patches of membranes, shown as the black regions. Next, we have a creepy image (b) of a moth scale. The randomness of the holes in a moth scale compared to the periodic pattern of a butterfly scale in image (c)(d) provides an explanation for the more vibrant iridescence of a butterfly. In image (d), we can also see a small spore that could possible be pollen. The large air gaps in the scale is measured with ImageJ and ranges from 500-850 nm and the branches ranged from 200-250 nm.

(a) SE micrograph of peacock feathers recorded at 10 keV and 151 K X with a SE2 detector

(b) SE micrograph of peacock feathers recorded at 10 keV and 345 K X with a SE2 detector

(c) SE micrograph of peacock feather fibers recorded at 5 keV and 7.84 K X with an InLens detector
(d) SE micrograph of peacock feather fibers recorded at 5 keV and 34.69 K X with an InLens detector


With the peacock feather sample, it was difficult to observe nanometer scale structure at a low magnification. In image (a) and (b), we observe feather patterns around 17 microns, which is not a reasonable size to produce visible wavelength interference. However, at a closer look with the InLens detector and a high magnification, we observe less than 100 nm thick structural fibers on the surface and inside the feather, as shown in image (c) and (d).

(a) SE micrograph of CD gratings recorded at 15 keV and 7.35 K X with a SE2 detector
(b) SE micrograph of CD gratings recorded at 15 keV and 12.81 K X with a SE2 detector


Lastly, we have two SE2 images of our CD sample. CDs encode with trenches and ridges that is essentially an optical grating. When white light is incident upon a grating, different wavelengths of light will be diffracted at varying angles depending on the period, structure, and material of the grating. The ridges of the CD is measured to be on the order of a micron.

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X-Ray Analysis

X-ray microanalysis in the SEM is one of the few non-invasive and non-destructive methods of characterizing a material's chemical content. This technique is possible due to the interaction of the electron beam with the sample. When an electron beam spot is focused onto the surface of a sample, it creates a tear drop shape interaction volume. The deepest region in the interaction volume is origin of the characteristic X-rays. The X-ray photons are formed when a primary electron from the beam collides with an inner shell electron and forms a vacancy in the inner shell. To stabilize the structure, an outer shell electron decays to a lower energy state in the inner shell and releases an X-ray photon. In this process, elements will emit X-ray photons of energy corresponding to their atomic number and a detector will convert photon energy into electronic signals.

Once the X-ray emission emerges from the sample, an Energy Dispersive X-ray Spectroscopy (EDS) detector is used to characterize the photon energies. The EDS detector is a solid-state detector that converts X-ray photon energies into electrical charge. This electrical charge is amplified and processed through a field effect transistor. The detector is most efficient at collecting signals when it is placed at the largest solid angle from the emitted source area.


Figure 7. EDS analysis of an abalone shell



Figure 8. EDS analysis of a bug scale



Figure 9. EDS analysis of a peacock feather

From the EDS analysis, we observe that all three samples contain large amount of carbon and oxygen, as expected with biological materials. We also observe significant signal for gold as anticipated because we coated our sample with gold. Since the abalone shell was found in sand and is composed of nacre (a form of calcium carbonate), we observe elements such as silicon and calcium from the EDS graph. Both Figure 8 and Figure 9 showed similar results; however, since the feather contains more protein than the bug wing, it emits a high nitrogen signal.

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Thin Film Modeling


Figure 10. Thin film approximate reflection simulation of an abalone shell using OptiLayer

By knowing the thickness, the material, the relative number of layers, and the structure, we can simulate the reflection of our abalone shell. From the secondary electron imaging and EDS analysis, we learn that our abalone sample has on the order of hundred of layers and is composed of carbon, oxygen, calcium, and slight bits of silicon. Using ImageJ, we can approximately measure the thickness of each layer to be between 400-420 nm. Using approximate parameters, we simulated a sample with 100 alternating layers of 400 and 420 nm thickness with refractive index of calcium carbonate (See Refractive Index), that is also alternating with a slight deviation by layer. Our model, shown in Figure 10, displays reflection by wavelength and the angle of incidence at 0,20,40, and 60 degrees. The graph shows the first order of reflection is in the near-infrared and the higher orders of reflection in the visible regime. Furthermore, the higher order reflections vary drastically with change in angle of incidence, which resembles the reflection of many bright distinct colors of an abalone shell by tilting it back and forth. *Note, this is not an accurate wavelength-reflection model of an abalone shell

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Colorization

All SEM images do not display color as it is a raster scan technique that collects only signal intensities. Therefore, colorization is a useful technique to convey a message when done correctly. It is important to stress that the following are false colored and only depicts my personal views.

(a) Colorization of a tilted abalone shell to contrast the difference between the surface and cross-section

(b) Colorization of a large bug wing surface with butterfly and moth wing scales on top

(c) Colorization of intertwining barblue of a peacock feather

(d) Colorization of a CD surface

The first image (a) is of an abalone shell tilted such that both the surface of the shell without the periodic structure can be contrasted to the cross-section of the shell. The image resembles a cliff of a canyon, so it was false colored with a light yellow to resemble sand. The second image (b) is a low magnification view of our bug wing sample with a lot of other insect scales on top because the wing was stored in a jar with many other insect samples. The contamination came as a useful surprise since I was able to image multiple sample on one. The dark green is used to depict a grassier feeling but on the more ominous side. Looking closely, you can see a moiré pattern formed by the high special frequency of the latter structure on the scales. Next, image (c) shows a warm magenta colorization of the peacock feathers, simply because feathers are warm and soft. Lastly, we have image (d), our cold blue image of the surface of a CD. For more cool SEM images or images of anything I take, please follow me on IG @thechiefray !

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