Escolar Documentos
Profissional Documentos
Cultura Documentos
by
Meir Basson
_____________________________________________________________
May 2010
Abstract v
Introduction 1
Results 23
Discussion 32
Conclusion 34
Bibliography 35
ii
List of Figures
Figure 2: The relation between the skew angle and the pitch length of the structure 3
Figure 10: The effect of the polarizer and ¼ wave plate in the illumination path 15
Figure 12: The distance in pixels that the field of view of the camera has gone 18
Figure 13: Flowchart of the algorithm used to determine x, y and average hue 19
For TLC microcapsules in the images
Figure 14: Each particle’s location in the axial direction of the microchannel 22
Figure 19: Lower expect linear temperature curve with the TLC temperature data 27
iii
Figure 20: Higher expect linear temperature curve with the TLC temperature data 28
Figure 21: TLC Temperature data plotted with the combined expected curve 30
iv
Abstract
Thermochromic liquid crystals (TLC’s) have a unique chemical composition that makes
them reflect different wavelengths of the visible light spectrum at different temperatures,
causing them to change their color. This quality makes them a good candidate for
were acquired at different controlled temperatures and their color was quantified based on
average hue values. Their use was tested by comparing the temperature values they
TLC’s could also be used to simultaneously measure the velocity and temperature in
v
Introduction
Thermochromic liquid crystals (TLC’s) have been used in the past as a temperature
measurement technique of fluids in the macro scale [4,7]. They can also be used in the
learn more about the temperature and how it changes in various micro-fluidic
applications. For example, many microfluidic devises use thermocapillary flow to throw
Thermocapillary flow is caused due to a temperature gradient along the microtube where
both air and liquid are present. This causes a surface tension gradient on the air-liquid
interface. The exact details on the air-liquid interface are not fully understood. For
example, the temperature at a particular location on the interface is not equivalent to the
local temperature predicted by heat conduction along the microtube. This is due to the
fact that convective heat transfer exists on the interface. If more knowledge could be
acquired on the temperature gradients that drive the flow, designs for more efficient
chemicals that have chiral structures. While matter conventionally exists in three forms,
solids, liquids, and gases, TLC’s have an intermediary state between the solid and liquid
phases called the liquid crystalline state. When TLC’s are in this state, they possess the
mechanical properties of liquids and the optical properties of crystalline solids. Optically
1
active, chiral neumatic TLC’s in this state are comprised of helical aggregates of
Figure 1: TLC's in their solid, liquid, and intermediate states (based on figure 11 of the Hallcrest
Handbook of TLC Technology) [5]
Each molecule is skewed at an angle θ with respect to its neighbors in the adjacent sheets,
separated by a distance λ, directly above and below them. The pitch length is the length
along the axis of the helix through which the direction vector of the molecules has
revolved 360 degrees. Thus, the skew angle θ and the sheet distance λ determine the pitch
360
P= λ .
θ
With increasing temperature of the liquid crystals, the skew angle θ increases and the
distance between each sheet λ increases. Depending on the particular TLC formulation,
either the increase in θ dominates over the increase in λ or vice versa. Usually the
2
increase in θ dominates. Increasing θ contributes to decreasing pitch length P while
The structure of TLC’s forms a volume grating that interacts with incident light. Thus,
they cause Bragg scattering. Depending on the pitch length and angle between the
incident light and reflected light φ, a certain wavelength of light λo will be reflected.
λo = 2P sin φ
Figure 2: The relation between the skew angle and the pitch length of the structure (based on figure 9
of the Hallcrest Handbook of TLC technology)[5]
Thus, TLC’s will have different colors at different angles of reflection and different
temperatures. The TLC colors range through the colors of the visible light spectrum.
temperature sensitive TLC formulation whose pitch length P increases with temperature.
3
Since the TLC’s color plays are reversible, upon cooling TLC’s, the color change
sequence is reversed. Different TLC formulations cause TLC mixtures to have different
color plays. Thus, they can have different starting temperatures and different color play
lengths.
Figure 3: Typical reflected wavelength vs. temperature response of a temperature sensitive TLC
formulation at a constant angle of reflection.
Another property of TLC is circular dichroism. Light that illuminates TLC is resolved by
the unique TLC structure into its two circularly polarized components, one right-handed
and the other left handed. One component is completely reflected while the other is
Most TLC mixtures are very susceptible to degradation from UV light, and are also very
sensitive to certain organic chemicals. Thus, TLC mixtures that serve as temperature
indicators are typically microencapsulated. Tiny droplets of TLC are surrounded with a
from a few microns to a few milliliters. The microencapsulation process stabilizes and
protects TLC’s.
4
Figure 4: TLC circular dichroism (Based on figure 12(c) of the Hallcrest Handbook of TLC
Technology)[5]
Color Measurement
The pixels in an image of TLC particles would have unique Red, Green, and Blue (RGB)
values that represent the TLC’s apparent colors. These values can be used to determine
the hue, saturation, and intensity (HSI) values for each pixel. Intensity, I, is the sum of
5
Saturation is a measure of how far a pixel is from white and hue is a measure of the color
(see figure 5). The quantities v1 and v2 are related to the RGB values by
and
After they have been determined, they can be used to determine the values for hue, H,
and saturation, S.
With the hue values for each pixel, an average hue can be calculated for each individual
TLC particle.
Due to the sensitivity of TLC’s to the optical arrangement and aging of the sample,
The hue value obtained from pictures of TLC’s is expected to have two main sources of
variations. Since no one TLC particle is exactly the same as the other, the calculated hue
values are expected to vary by a determinable amount. The second source of uncertainty
6
would be due to variations in reflected wavelength due to the location of the TLC’s in the
Figure 5: HS vector of a typical pixel. Here the hue value is closest to the red axis, which is at 0
degrees. Thus, this pixel is expected to look red.
simple configuration.
7
Materials & Methods
play range of 35 oC to 45 oC was used. The average TLC microcapsule diameter in the
sample was approximately 10 to 15 microns, but the sample had a full distribution of
The microchannel used in the experiment was a fused silica capillary tube (see figure 6).
The center of the tube was void of the Polyamide coating, making it transparent so that
the particles in that section of the tube are visible to the microscope.
An Aluminum block was used to control the temperature around the microchannel. It had
five temperature sensors along its axial direction, and had a slot through which the
capillary tube was designed to be inserted (see figure 7). The three temperature sensors in
the center of the block were thermistor probes from U.S Sensor Corp with an uncertainty
of ±0.02 Co. The middle sensor was 1.5 mm away from the other two sensors along the
axial direction of the block, and was placed in the center of the block. Three alignment
three middle sensors (figure 7). The shop provided no uncertainty estimate of how well
the alignment marks line up with the sensors, but a conservative estimate for this
uncertainty is ±1 mm. The two temperature sensors on the outer edges of the block were
To control the temperatures, six Peltier devices wired in series were mounted on the two
ends of the block. They heated or cooled the surface of the block, depending on the
direction of the current through them. Each set was controlled by a bipolar PID
increased and decreased. The feedback input for the temperature control was the
9
Figure 7: Block used to control the temperature
10
The microscope used was an Olympus IX81 with a halogen lamp. The microscope was
used at its 40X magnification. The microscope stage was enclosed by a Plexiglas
incubator. The stage could be moved manually in the two horizontal directions as shown
in figure 8. A 3CCD, Progressive scan, color camera (Toshiba, IK-TF7C ) was connected
to the microscope’s left side port. The camera acquired a smaller field of view than that
of the eye ports, but centered at the same location (see figure 8).
(LHCP) light without changing the sense of polarization and transmit right-handed
circularly polarized (RHCP) light, but other surfaces such as the edges of the
microchannel and the encapsulation of the TLC’s reverse the handedness upon reflection.
11
Since the TLC color is the only part of the image that should be interpreted as the data,
the microscope was configured to illuminate with only LHCP light and to allow only
LHCP light to reach the camera. With this configuration, ideally only the TLC’s would
The Halogen lamp produces unpolarized light. Unpolarized light contains a uniform
wave plate were placed in the illumination path. The light that comes from the lamp
passes through the polarizer and, due to the orientation of the polarizer, one linear
polarization (P1) is transmitted, while the orthogonal sense of polarization (P2) is blocked.
The light then passes through the ¼ wave plate. The ¼ wave plate is oriented with its fast
axis rotated 45o away from the orientation of the polarizer. This causes equal parts of the
light to travel at the fast and slow speeds of the crystal. When the light exits the ¼ wave
plate, the part of the light that travelled slower is a ¼ of a wave length behind the part
that has travelled faster. As a result, the linearly polarized light (P1) that passes through
the 1/4 wave plate becomes left-handed circularly polarized. Right-handed circularly
polarized light would be obtained by rotating the ¼ plate 90o about the optical axis. The
The reflected light off of the TLC’s remains LHCP while the reflected light off of the
other surfaces is reversed and becomes RHCP. The reflected light passes back through
the ¼ plate and is resolved back into its linearly polarized components, with LHCP light
becoming P1 and RHCP light becoming P2. The light then passes through the polarizer,
12
causing only the P1 component of the light to reach the camera (see figure 9). Each letter
Figure 9: (a) Unpolarized light. (b) One sense of linearly polarized light, P1 (c) LHCP light. (d) Both
LHCP and RHCP light. (e) P1 and P2 linearly polarized light (f) Only P1 linearly polarized light.
This configuration ideally increases the signal to noise ratio to infinity. However, in
reality there are three imperfections in the setup that cause the encapsulations of the TLC
and the sides of the microchannel to still be somewhat visible in the field of view of the
camera. First, the polarizer has a finite extinction ratio. Second, the fast axis of the ¼
wave plate cannot be oriented exactly 45o away from the orientation of the polarizer.
Third, the ¼ wave plate separates equal parts of the light by exactly ¼ of a wave length at
only one wavelength of the visible light spectrum. These imperfections cause some
RHCP light to reach the microchannel. As a result, a small amount of the reflected light
13
off surfaces other than TLC’s comes back through the ¼ wave plate and the polarizer and
The effect of placing the polarizer and ¼ wave plate in the illumination path is shown in
figure 10.
With all the equipment configured to take images, TLC mixture was inserted into the
microchannel. A syringe was filled with the TLC mixture. A fitting assembly (P-662,
Upchurch Scientific) was then used to connect the capillary tube to the syringe. Next, a
Harvard PHD Ultra syringe pump was used to steadily infuse the TLC mixture into the
microchannel.
The syringe was disconnected and the fitting and the capillary tube were placed inside the
aluminum block. The microchannel was inserted into the slot. The transparent part of the
microchannel was centered in the block. Two pieces of double sided tape were then used
All sides of the block were covered with insulating tape except for the heater sides and
the side which is shown face up in figure 11. This side was insulated using a sheet of
Mica Tape. It was taped to the block with the double sided tape once the microchannel
was in place. Finally, the block and microchannel were placed on the microscope stage.
The microchannel was placed so that the x axis illustrated in figure 7 would make the
smallest angle possible with the axis of the direction of the stage movement.
14
Figure 10: (1) Image of TLC microcapsules near the edge of the microchannel, (2) same setup but
with the polarizer and ¼ wave plate in the illumination path. Notice the edges of the microchannel
and encapsulations are nearly invisible in (2)
15
Figure 11: Block with the microchannel inserted
For the calibration, both sides of the block were set to the same temperature and images
of the TLC mixture along the microchannel were taken. The stage was moved after each
image was taken so that the field of view of the camera would cover a new section of the
approximate increments of 0.4 or 0.6 degrees. For each temperature, 75 to 100 images
To test the measurement technique, two linear temperature gradients were imposed in the
middle of the block, one higher and one lower. To impose the lower temperature
gradient, one side of the block was set to 31.2 oC and the other side was set to 44.4 oC. To
impose the higher temperature gradient, one side of the block was set to 33.9 oC and the
16
other side was set to 46.6 oC. From the principle of heat conduction through the shape
and material of the block, a linear temperature gradient was predicted to be present at
least 0.5 mm away from the center of the block in each direction. Thus, for each
temperature gradient imposed, an expected linear temperature curve was plotted. The
temperature sensors in the center gave two points through which the expected linear
curves were fit on an x vs. T graph. For the lower temperature curve, the temperature
range was 35.91 ± 0.02 oC to 40.08 ± 0.02 oC. For the higher temperature curve, the
Next, for each temperature gradient, images of the TLC mixture were taken along the
microchannel. First, an image was taken in the center of the block as indicated by the
center alignment mark. Following this, images were taken by moving the stage towards
one side of the microchannel. One overlapping TLC microcapsule was included in every
two images in order to keep track of the distance in pixels that the field of view of the
r
camera has gone, S (See figure 12).
Images were taken until the camera’s FOV has moved 0.5 mm away from the center. The
same procedure was done on the other side of the microchannel. In order to know when
the camera had travelled 0.5 mm away from the center, the pixel to length conversion
factor was determined. A dual axis linear scale was imaged and the conversion facto was
17
Figure 12: By keeping one TLC microcapsule in two images taken along the microchannel , the
distance in pixels that the field of view of the camera has moved from the fist image can be
r r r
determined: S = I 1 − I 2
After the images for both the calibration and the experiment were acquired, an algorithm
was implemented in Matlab to process the images and determine for each TLC
microcapsule found in the images the distance in pixels from the left edge of the image,
X, the distance in pixels from the top edge of the image, Y, and average hue value H.
Refer to figure 13 for a flowchart outlining the main operations of the algorithm.
The algorithm receives an image of TLC particles, converts the RGB values for every
pixel into HSI values and saves it as a 3D array. From the HSI data for every pixel, it
filters out the pixels which have intensity and saturation lower than a given threshold.
Next, it averages the saturation around each remaining pixel over a square centered at the
pixel. The square will sit on a certain amount of pixels and its size is determined based on
an input integer ‘rad’. ‘rad’ is half the length of the square minus one pixel.
18
Figure 13: Flowchart of the algorithm used to determine x, y and average hue for TLC microcapsules
in the images.
19
The algorithm then further filters out the pixels of which the average saturation of the
pixels around it was lower than a given threshold. With this step completed, the algorithm
has the X and Y values of the pixels of interest. However, if two retained pixels are too
close to each other, they most likely sit on the same TLC particle. As a result, the
algorithm then groups different pixels if they are close to each other by a given distance
in pixels. Finally, after it has them in groups, it looks for the pixel in each group which
has the highest intensity and drops the rest of the pixels in each group. If two pixels in a
group both have the highest intensity, the algorithm chooses the one which has a higher
saturation. The pixels that are left each represent a TLC particle whose hue is important.
The next step is to average the hue based on all of the pixels in a square around that
location. If the saturation of a pixel in the square is lower than a given threshold, than the
Finally, the algorithm reports the number of TLC particles found, and displays each one
As part of the calibration, after the X, Y and H data for every TLC microcapsule at each
set temperature from 35 C to 45 C was acquired, the uncertainty was quantified. First, the
uncertainty due to particle-to-particle variations was quantified. For each set temperature
value, an average hue, H_ave, was calculated and a histogram was made from the H data.
In addition, the uncertainty of each individual particle hue values, σH(1), and the
uncertainty of the averaged hue value, σH(ave), were determined using two standard
deviations, 2σ.
20
σH (1) = 2σ
2σ
σH (ave) =
n particles
Following this, the uncertainty due to variations in reflected wavelength due to the
location of each given TLC in the field of view was quantified. For each set temperature
value, the hue data was divided into 12 groups. Each group corresponded to a different
section in the field of view. For each group, an average hue was determined and was
given the corresponding uncertainty using two standard deviations. Since no noticeable
trend between the particles’ group and their average hue was found, TLC location in the
To complete the calibration, a T vs. H_ave graph was made with linear interpolations
between the calibration points. The uncertainty in hue, both for an individual particle’s
hue and average hue was used to determine the uncertainty in temperature,
dT
σT (1) = σH (1)
dH
dT .
σT (ave) = σH (ave)
dH
To complete the experiment, the images that were taken when the temperature gradients
were imposed on the block were processed to acquire the X, Y and H data. The X and Y
data were used to determine each particle’s location in the axial direction of the
microchannel. As described above, the first image taken was in the center of the block,
and one of the TLC particles in that image was called the origin O, (see figure 14).
21
r r r r r
Figure 14: O , I and S are in image coordinates. O has known X and Y values, O = ( X o , Yo ) .
r
P is in spatial coordinates. The x component of the P vector is the axial distance of the
TLC particles from the origin. Next, the H data was converted to temperature data for
22
Results
Calibration Results
Most of the histograms made resulted in a similar shape. Figure 15 shows a typical
histogram.
A typical histogram resembles a Gausian. As the number of data points increased, the
histogram looked more and more like a Gausian. For the particular histogram shown,
H_ave = 131.7o.
The fact that the peak is not at H_ave in figure 18 is atypical. This particular histogram
was selected to emphasize that the hue distribution for the set temperatures is not exactly
a Gausian.
23
The following two figures display the calibration curve with linear interpolations between
calibration points and the corresponding uncertainty. Figure 16 shows the uncertainty in
temperature based on one particle’s hue, σT (1) , and figure 17 shows the uncertainty in
the calibration, 35.4 Co, resulted in a very wide hue distribution. Since its uncertainty in
temperature was very high, the first two set temperatures were excluded from further
Figure 16: Calibration curve between set temperatures and average hue with σT(1) for uncertainty
24
Figure 17: Calibration curve between set temperatures and average hue with σT(ave) for uncertainty
1
As expected, since σT (ave) α , the uncertainty in figure 17 is much smaller
n particles
than the uncertainty in figure 16. nparticles was different for each calibration point. The
reduction in uncertainty from σT(1) to σT(ave) will always depend on the value of
nparticles.
Based upon the measured uncertainties, the T range for the linear temp gradient was
restricted to (35.99 oC - 43.69 oC) to avoid the very high uncertainties at higher
temperatures.
25
The following figure compares the uncertainty in temperature measurement of one
Experiment Results
The temperature data and its uncertainty were plotted with the two expected linear
26
Figure 19: Lower expect linear temperature curve along with the TLC temperature data. The blue
line is the linear fit to the data
The slope of the expected curve is 0.416 Co/mm and the slope of the linear fit is 0.393
o
C/mm.
27
Figure 20: Higher expected linear temperature curve along with the TLC temperature data. The blue
line is the linear fit to the data
The slope of the expected curve is 0.414 oC/mm and the slope of the linear fit is 0.474
o
C/mm. The data on the positive x side of figure 25 has a significant amount of outliers.
The reason for this is that at temperatures of around 42 oC or higher, small changes in hue
cause the temperature readings from the calibration to vary significantly. Therefore, that
The offset between the curve fits and the expected curves in both graphs is due to the
uncertainty of how well the alignments marks line up with the three thermistors in the
block.
28
To correct this offset, first the two expected curves were combined into one. The slop of
the combined curve is the weighted average of the curve fit of figure 19 and the curve fit
2mlow + mhigh
mcomb =
3
Second, to show the full useful range of the TLC’s on one plot, all the TLC temperature
data except for the data on the positive x side of figure 25 was plotted on one T vs. x
graph. The data in figure 20 required a shift in its x-coordinates which was determined
⇓
Tstart − blower
xshift = + 5 mm
mcomb
The combined TLC temperature data was given a linear curve fit. The temperature value
in the center of the curve fit was placed at x=0. Finally, the y-intercept of the expected
curve was corrected so that it intercepts the center of the curve fit at x=0 (see figure 21).
29
Figure 21: TLC Temperature data plotted with the combined expected curve
The standard error for the combined curve fit was calculated,
n _ particles
∑ [T fit ( xi ) − Ti ]
2
S xT = i =1
= 0.474 o C .
n _ paticles − 2
Where T fit ( xi ) is the temperature value of the curve fit at each data point’s axial
location xi , and Ti is the temperature value of each data point. For a 95% confidence
σT fit = 2 S xT = 0.948 oC
The following figure compares the expected curve with the combined curve fit with its
uncertainty limits plotted. The expected curve falls well within the uncertainty limits of
31
Discussion
fluid along a microchannel produces results that are consistent with prescribed
particles sampled. Thus, for the TLC formulation used in this study, this measurement
technique is practical between 36.30 oC and 41.30 oC. The calibration curve showed that
this measurement technique produces small uncertainties starting at 120 degrees of hue to
nearly 240 degrees of hue. Thus, the practical color play range for this TLC formulation
is from pure green to nearly pure blue. Other TLC formulations are expected to have a
similar practical color play range but a calibration would be necessary to test that.
This measurement technique has room for further improvement. The calibration and the
1) Filtering the TLC mixture to result in a more uniform distribution of particle sizes
to filter out everything but the relevant, color changing, part of the TLC microcapsules
particle colors
TLC mixtures could also be used as a velocity measurement technique of fluids flowing
32
microcapsules could be used as tracer particles in a micro particle image velocimetry
33
Conclusion
Using TLC mixtures to measure the temperature in microchannels has been proven to be
practical. After making improvements to the measurement technique, it can be used for
Thermocapillary flow could be generated by injecting an air bubble into the microchannel
and imposing a temperature gradient on the microchannel using the aluminum block. The
bubble will move towards the hotter side of the microchannel. The velocity and
temperature of the air/water interface could be measured during this motion and a model
relating the temperature gradients and the forces they cause could be found.
34
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35