InterimReportDecember12,2011

Experimentalevaluationoftheabsorptionspectrumofanumberofsamplesbased
onlampillumination.
(BenGurionUniversitygroup).
Summary
Though an experimental system is in place to measure the absorption spectrum in the range of 380 to
1700 nm based on direct solar radiation (described in our first-year report), we decided to build a
second system based on a Xenon arc discharge lamp whose output is stable and not dependent on
weather conditions. The system uses a heated sample holder which eventually will allow
measurements at temperatures of up to 700C. The sample holder can accommodate both the smaller
(30x30mm) and the 60x60mm samples.
We evaluated this system and performed detailed measurements on the first set of samples we
received during October 2011 from Camille.
The system is not perfect as we will detail below, but first results appear indicative of the capability
of the system and is hopefully useful in the further development of the anti-reflective coating.
New Experimental Setup
Previous experiments were performed using the direct sun directed into the lab via a heliostat
(reported in our first-year report). A small waviness of the (nominally flat) heliostat caused
significant variations in the irradiation of the sample and influenced the measurements. As a result it
was decided to build an optical system for measuring the absorption spectrum based on a Xe arc
discharge lamp (Fig 1).
The new experimental setup was also designed for measuring the spectral absorptivity at high
temperatures. The source of radiation (Fig.1a) is a Xe lamp (300W nominal power), which reaches
stability within about 15 minutes of operation and remains stable with a drift of 0.5% and
fluctuations of 1% (manufacturers data). We added two flat mirrors to increase incident light on
the sample. The distance between the light source and the target was set to be 60 cm, a compromise
between sufficient light at the sample (the samples are highly absorbing!) and light uniformity at the
sample. The light is not completely collimated but subtends an angle of about 4. We measured the
light intensity as a function of position on the active area of the sample (5cm across) and found it to
be within ~0.5% of peak radiation.
The sample holder can be heated via a custom made heating element whose outside dimensions are
100x100x50 mm (Figs. 1b and 1c). During pre-experiments we successfully heated a sample (60x60
mm) up to 1000K. The temperature was measured by means of a portable thermocouple-integrated
high performance handheld Infrared thermometer (OMEGA OSXL689).
A reasonable uniform temperature distribution on the sample with minor temperature gradients
towards the edges was observed (approximately 5C between center and edge at 320C). As a
reference, we use a gray sample (Fig. 1d) from Labsphere with an NIST-traceable calibrated
absorption spectrum (Fig 2).

(a)

(b)

(c)(d)

Figure 1. (a) left: side view of system, right: view of the lamp and mirrors from direction of the
sample. (b) The heated sample holder and optical fiber with collimating optics (c) Electric heater
with the sample removed, (d) reference sample from Labsphere with an absorption coefficient
0.96 (Lambertian reflector) in the visible and NIR part of spectrum.

reflectance of gray reference sample

reflectance

0.1
0.09
0.08
0.07
0.06
0.05
0.04
0.03
0.02
0.01
0
400

reflectance

600

800

1000

1200

1400

1600

1800

wavelenght (nm)

Figure 2. Reflectance spectrum of the Labsphere gray spectralon reference sample, as supplied by the
manufacturer, NIST traceable calibration.

Methodology: determining the absorption spectrum of the samples

A. The reference sample.

As reference to all our measurements we use a grey spectraflect reflecting coating which behaves
very closely to a Lambertian reflector (Fig. 1d) with spectral reflectivity shown in Fig. 2. As a first
test, we tested the Lambertian character of the reference sample. The reflectance spectrum was
measured at s=15, and again at 30, 45, and 60, and the latter three measurements compared to the
one at 15 (s is defined in Fig.3). A Lambertian sample should not show any difference. The results
of this comparison are shown in Fig. 3. We see a small change in the reading at 60, as well as the
noise in the system. In particular at the edges of the spectral ranges the noise is significant, namely
near 380nm at 900nm and at 1700nm. At these edges the sensors have minimal sensitivity and the
noise is largest (we divide small numbers). The change from 30 to 45 incidence of about 5% is
bearable. Translated into absorptivity it would mean that a sample with 95% absorption at 30
changes to an apparent 95.25% absorptivity, at 60 it would appear to be about 95.75%. The question
of course is whether the sample is truly Lambertian or if our system, when rotating, introduces some
error.

Fig.3. Comparing the reflectance spectrum of the reference sample to itself at different angles s. In
other words, if the sample was truly Lambertian, we should get unity for the entire spectrum.
B. Experiments on four samples.
A series of experiments was performed on four samples (MS-1.1, MS-1.3, MS-1.5 and TS1). Their
dimensions were 30x 30 mm for the first three (MS-1.1, MS-1.3, MS-1.5 with 1, 2 and 3 layers of
coating respectively) and 60 x 60 mm for the TS1. Two series of experiments were performed: in the
first we kept the samples at ambient temperature and in the second the samples were heated to
around T=600 K. In all cases we measured the reflected spectral intensity r =f(, s, s, T) of
reflected light by means of two spectrometers, one in the visible range (380-900nm) and a second in
the NIR (900-1700nm) part of the spectrum. Both spectrometers are by Control Development, the
visible is the PDA-512, and the near infrared is NIR128L-1.7TS. Two angles, which characterize the
incident direction of light were kept constant for all experiments, namely, i=0, and i= (Figure
3). The solid angle subtended by the receiver was also fixed (determined by the fiber aperture and
the collimating optics). The angles, which define the direction from which the reflected light are
measured, are polar angle s and the azimuth angle s (Fig. 3). In our preliminary measurements we
varied only the polar angle s (15, 30,45 and 60).

Figure 3. Definitions of incidence angles and angles of reflection. I is incident radiation on the
sample surface. The ZB axis is normal to the sample surface, and the XB axis lies in the plane
defined by ZB and I. The incident direction is given by (i,i), where i = by definition. The
direction of the reflected radiation is given by (s, s). is the solid-angle subtended by the receiver.

C. Results for ambient temperature

We performed measurements with the samples at room temperature using the reference sample at
s=15 as the calibration. We measured each sample in two stages: first at 4 angles in the visible
range and then repeated the measurements at the NIR range.
The first three samples (MS 1.1, MS 1.3, MS 1.5 shown in Fig. 4 a, b, and c, respectively) exhibit a
very similar behavior at angles s of 30-60. The absorbtivity obtained showed quite uniform
behavior at around the value of 0.96 at wavelengths 500-1600 nm. As expected, values at the edges
of the spectrometer ranges had relatively high fluctuations. The two spectra were spliced together,
and again we observe much noise at the interface which is at 900 nm. At s=15 the absorbtivity
appears significantly lower for all 3 samples and is also less uniform than at the other angles. We
suspect that there is a small specular component to the reflectance we observe at this angle (near the
angle of incidence), a certain amount of higher reflectivity than at the higher angles. We also noticed
that at that angle the measurements were very sensitive (significant jumps from the visible range to
the near infrared range) and most probably cause the jump at 900nm, indicated by vertical ellipses in
Figs. 4a and 4c. An inaccurate repositioning of the sensor might be the source of this effect, but we
shall further investigate this behavior.

(a)

(b)


(c)

(d)

Figure 4. Measured spectral absorbtivity as a function of wavelength of 4 samples at the ambient

temperature. The direction of measurement relative to the samples normal is the single parameter
had been modified. (a) MS 1.1 one layer of coating. (b) MS 1.3 two layers of coating. (c) MS 1.5
three layers of coating. (d) TS 1 sample (60x60 mm).

C. Experiments with samples heated to elevated temperatures

The second series of measurements were carried out with samples heated to around 600 K. The
temperature of the sample was quite uniform: we measured 600 K at the center of the sample and at
edges it was 595 K. All 4 samples showed quite uniform values of absorbtivity at polar angles >15
in the spectral range of 400-1100nm. However, at wavelength larger than 1100nm we encountered
accuracy problems as the radiation emitted from the samples started to be equal to or even higher
than the radiation reflected by the sample (thanks to the high absorptivity). Though we tried to
subtract out the sample radiation by measuring the emitted power without illumination the noise was
too large to give useful results. We therefore present only the data we obtained in the visible range
(Fig. 5). We are working on remedying this situation by either a stronger lamp or by reverting back
to solar radiation which is an order of magnitude stronger (and could in addition be slightly
concentrated without exceeding incidence angles of greater than a few degrees).
At the polar angle of 15 we repeatedly observe lower values, apparently a very sensitive behavior at
close to normal direction, which may be associated with the partially specular behavior of the
samples (when the receiver is near the angle of specular reflection, the range of the light input angle
is 5).


(a)

(b)

(c)


(d)

Figure 5: Measured spectral absorbtivity as a function of wavelength of 4 samples at high

temperature for four polar angles. (a) MS 1.1 one layer of coating heated to 590 K. (b) MS 1.3 two
layers of coating at 600 K. (c) MS 1.5 three layers of coating at 620 K. (d) TS 1 sample (60x60 mm)
at 610 K.

Future work
1. To measure at more broad range of angles to be able to measure, with higher accuracy, the total
hemispherical absorbance.
2. Perform experiments with more powerful power supply to reach higher temperature and
increasing the incident intensity, in order to minimize the noise.
3.

Increasing the light input in order to improve the signal to noise ratio.