Name: Fabrication and Testing of Photonic Thermometers (Video) | JoVE Journal
Uploaded: 2018-10-24T12:30:00.000+00:00
Duration: 8 min 44 s
Description: Learn photonic thermometer fabrication and testing for temperature metrology using frequency-based measurement techniques. This method enables precise measurements while reducing calibration requirements.

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The authors acknowledge the NIST/CNST NanoFab facility for providing opportunity to fabricate silicon photonic temperature sensors and Wyatt Miller and Dawn Cross for assistance in setting up the experiments.

1. Device Fabrication
Note: Silicon photonic devices can be fabricated using silicon-on-insulator (SOI) wafers applying conventional CMOS-technology via photo- or electron beam lithography followed by inductive plasma reactive ion etch (ICP RIE) of 220 nm-thick topmost silicon layer. After ICP RIE etch the devices can be top-cladded with a thin polymer film or SiO2 protective layer. Below are the main steps of in fabrication of SOI photonic devices.
<ol>
	<li>Clean an SOI wafer in a piranha solution for 10 min, a mixture 4:1 of sulfuric acid (H2SO4) and hydrogen peroxide (H2O2), followed by a deionized (DI) water rinse for 1 min and nitrogen gas blow dry.</li>
	<li>Spin coat about 20-50 mL of maN 2405 e-beam resist onto the wafer at 4,000 rpm for 60 s, followed by a hotplate bake at 90 &#176;C for 15 min.</li>
	<li>Expose the device pattern on to the spin-coated resist using e-beam lithography and develop the resist. The usual base exposure dose is about 600 &#181;C/cm2. Develop with MIF-319 developer for 60 s, followed by a 60 s water rinse.</li>
	<li>Perform an ICP RIE etch of the 220 nm thick silicon layer to remove the unprotected silicon. Use a pseudo-Bosch process with C4F8: 57 SCCM / SF6: 33 SCCM, ICP power: 3,000 W; RIE power: 15 W; pressure 10 mTorr, temperature: 15 &#176;C; Etch rate: approximately 5-6 nm/s</li>
	<li>Dissolve the resist mask in pure acetone for 1 h, followed by an isopropanol rinse, a 60 s DI water rinse and nitrogen gas blow dry.</li>
	<li>Deposit a 1 &#181;m thick protective top-layer on the wafer (a thin polymer film) via a spin coating (spin coat 20-50 mL PMMA at 4,000 rpm for 60 s followed by a hotplate bake at 180 &#176;C for 2 min).</li>
	<li>Dice the wafer with a wafer dicing saw (saw blade thickness: 35 &#181;m) into small easy to handle chips (e.g., 20 mm &#215; 20 mm).</li>
</ol>
2. Photonic Chip Packaging
Note: The fabricated photonic chips are packaged on a custom design packaging setup where a custom-built packaging setup is used to align and bond an array of optical fibers to a photonic chip. The packaging setup shown on Figure 1 consists of (i) 6-axis micro-positioning stage, that allows 6-degree of freedom movement (X, Y, Z coordinates, and three corresponding angles of rotation relative to X, Y, Z coordinates) with submicron precision; (ii) on-stage integrated Peltier module that allows to heat or cool the top stage platform; (iii) v-groove array holder arm; epoxy adhesive micro-dispensing module; (iv) ultra violet (UV) light exposure module to cure UV adhesives, and (v) four high magnification digital cameras for top, front, and two side angle views. Optical fibers package in v-groove array are procured from a commercial source.
<ol>
	<li>Rough alignment procedure
	<ol>
		<li>Place the photonic chip on the 6-axis stage, and orient the chip so the on-chip input/output ports are aligned with the v-groove array.</li>
		<li>Turn on vacuum suction through on-stage integrated vacuum pumping port to hold the chip in place.</li>
		<li>Use the top-view digital camera to locate and place the photonic devices of interest in the center of the 6-axis stage.</li>
		<li>Position the v-groove array holder arm close to the chip and use vacuum suction through an integrated pumping port to hold the array in place.</li>
		<li>Use the side-view digital cameras as a visual feedback to help position the fiber array above the on-chip grating couplers.</li>
		<li>Raise the 6-axis stage to bring the photonic chip to within 10 &#181;m of the fiber array&#39;s bottom edge. 
		NOTE: The edge of the v-groove fiber array should be roughly aligned (within 50 &#181;m to 100 &#181;m accuracy) relative to on-chip alignment marks. This procedure brings the optical fiber facets within a relative proximity of the corresponding grating couplers.</li>
	</ol>
	</li>
	<li>Automated optimal alignment
	<ol>
		<li>Once a rough manual alignment is achieved, activate the automated search using the vendor supplied software for the 6-axis stage. 
		NOTE: This algorithm performs a pre-defined walk over the 6-degrees of movements (translational and rotational) until the maximum transmission of broadband light through the chip&#39;s input and output ports is achieved. It should take no longer than 20 s to 30 s.</li>
	</ol>
	</li>
	<li>Photonic chip testing 
	NOTE: Once the optimal alignment is achieved, check device viability before proceeding with the bonding.
	<ol>
		<li>Use the on-stage integrated Peltier module to thermally cycle the chip&#39;s temperature while recording the spectral response. For thermal cycling, we used a custom script written in LabView.</li>
		<li>Analyze the recorded spectra is to verify the temperature sensitivity of the device (recommended values are 70 pm/&#176;C to 80 pm/&#176;C). 
		NOTE: The laser spectrometer has been described elsewhere in detail2. The recorded spectra are analyzed to determine the temperature sensitivity of the device which should be in the 70 pm/&#176;C to 80 pm/&#176;C range.</li>
	</ol>
	</li>
	<li>Bonding of optical fibers
	<ol>
		<li>Slowly lower the array down to the chip surface.</li>
		<li>Carefully position the epoxy filled syringe in close vicinity of the fiber array&#39;s edge using another XYZ micron precision stage.</li>
		<li>Dispense a single micro-droplet of an epoxy and initiate the curing process (either via UV irradiation or a thermal cycling).</li>
		<li>Periodically run the automated alignment (peaking/maximization) routine to prevent drift induced loss of signal until such a time that the epoxy starts to harden. 
		NOTE: After epoxy curing the photonic chip performance and light coupling efficiency are tested again by recording transmission spectra of the device at different temperatures. Light coupling efficiency typically increases after the bonding process, likely because the refractive index matched optical epoxy reduces reflection losses at the fiber-chip interface.</li>
	</ol>
	</li>
	<li>Packaging of Photonic Thermometer
	<ol>
		<li>Place the fiber bonded photonic chip on a copper cylinder (h = 25 mm, dia.= 5.79 mm) with a small amount (about 1 mg) of thermal grease applied to the copper mounting surface. 
		NOTE: Thermal grease ensures good even thermal contact between the metal heat conductor and the chip. Furthermore, thermal grease provides a weak adhesion between the two parts which facilitates the process of lowering the copper cylinder-chip assembly down a glass tube (h = 50 mm; inner dia. = 6.0 mm).</li>
		<li>Gently lower the chip-copper cylinder down the glass tube.</li>
		<li>Backfill the glass tube with Argon gas and seal with a rubber cork.</li>
	</ol>
	</li>
</ol>
3. Temperature Measurement
<ol>
	<li>Place the packaged photonic thermometer (glass tube + copper cylinder + fiber coupled photonic device) into a metrology temperature dry well (temperature should be stable to within 1 mK).</li>
	<li>Using the custom-built computer program set the settling time (20 min to 30 min), number of thermal cycles (minimum 3), temperature step size (1 &#176;C to 5 &#176;C), number of consecutive scans (minimum recommendation 5) and laser power (exact power delivered is specific to individual cases but generally is in the nanowatt to microwatt range). 
	NOTE: A calibrated platinum resistance thermometer bonded to the copper cylinder is used to concurrently record the bath temperature as the photonic measurements are carried out.</li>
</ol>

<ol><li>Price, R. <a target="_blank" href="http://www.technology.matthey.com/article/3/3/78-87/">The Platinum resistance Thermometer.</a> Platinum Metals Review. 3 (3), 78-87 (1959).</li>
<li>Xu, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Ultra-Sensitive+Chip-Based+Photonic+Temperature+Sensor+Using+Ring+Resonator+Structures%5BTitle%5D)+AND+%22Optics+Express%22%5BJournal%5D)">Ultra-Sensitive Chip-Based Photonic Temperature Sensor Using Ring Resonator Structures.</a> Optics Express. 22, 3098-3104 (2014).</li>
<li>Donner, J. S., Thompson, S. A., Kreuzer, M. P., Baffou, G., Quidant, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Mapping+Intracellular+Temperatrure+Using+Green+Flurorescent+Protein%5BTitle%5D)+AND+%22Nano+Letters%22%5BJournal%5D)">Mapping Intracellular Temperatrure Using Green Flurorescent Protein.</a> Nano Letters. 12 (4), 2107-2111 (2012).</li>
<li>Ahmed, Z., et al. <a target="_blank" href="https://arxiv.org/abs/1603.07690">Towards Photonics Enabled Quantum Metrology of Temperature, Pressure and Vacuum.</a> arXiv:1603.07690 [physics.optics]. , (2016).</li>
<li>Ahmed, Z., Filla, J., Guthrie, W., Quintavall, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Fiber+Bragg+Gratings+Based+Thermometry%5BTitle%5D)+AND+%22NCSL+International+Measure%22%5BJournal%5D)">Fiber Bragg Gratings Based Thermometry.</a> NCSL International Measure. 10, 24-27 (2015).</li>
<li>Hill, K. O., Meltz, G. <a target="_blank" href="http://ieeexplore.ieee.org/document/618320/">Fiber Bragg Grating Technology Fundamental and Overview.</a> J. of Lightwave Technology. 15, 1263-1275 (1997).</li>
<li>Liacouras, P. C., Grant, G., Choudhry, K., Strouse, G. F., Ahmed, Z. <a target="_blank" href="https://arxiv.org/abs/1508.01156">Fiber Bragg Gratings Embedded in 3D-printed Scaffolds.</a> NCSL International Measure. 10 (2), 50-52 (2015).</li>
<li>Klimov, N. N., Mittal, S., Berger, M., Ahmed, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((On-chip+silicon+waveguide+Bragg+grating+photonic+temperature+sensor%5BTitle%5D)+AND+%22Optical+Letters%22%5BJournal%5D)">On-chip silicon waveguide Bragg grating photonic temperature sensor.</a> Optical Letters. 40 (17), 3934-3936 (2015).</li>
<li>Klimov, N. N., Purdy, T., Ahmed, Z. On-Chip Silicon Photonic Thermometers: from Waveguide Bragg Grating to Ring Resonators sensors. Proceedings. Advanced Environmental, Chemical, and Biological Sensing Technologies XII, , Volume 9486, 948609 (2015).</li>
<li>Kim, G. D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Silicon+photonic+temperature+sensor+employing+a+ring+resonator+manufactured+using+a+standard+CMOS+process%5BTitle%5D)+AND+%22Optical+Express%22%5BJournal%5D)">Silicon photonic temperature sensor employing a ring resonator manufactured using a standard CMOS process.</a> Optical Express. 18 (21), 22215-22221 (2010).</li>
<li>Purdy, T., et al. Thermometry with Optomechanical Cavities. Conference on Lasers and Electro-Optics, , Optical Society of America. STu1H.2(2016).</li>
</ol>

The authors have nothing to disclose.
Certain equipment or materials are identified in this paper in order to specify the experimental procedure adequately. Such identification is not intended to imply endorsement by the National Institute of Standards and Technology, nor is it intended to imply that the materials or equipment identified are necessarily the best available.

The objective of this experiment was to quantify the temperature dependent response of a photonic thermometer. For quantitative measurements of temperature, it is prudent to utilize a stable heat source such as a metrology grade deep dry well, small volume sensors, ensure good thermal contact between the well and the sensor, and minimize heat loses to the environment. These requirements are easily met by bonding optical fibers to the chip, effectively creating a packaged device that can be lowered deep into the metrology...

The gold standard for temperature metrology, the platinum resistance thermometer, was first proposed by Sir Siemens in 1871 with Callender1 developing the first device in 1890. Since that time incremental progress in the design and manufacturing of thermometers has delivered a wide range of temperature measurement solutions. The standard platinum resistance thermometer (SPRT) is the interpolating instrument for realizing International Temperature Scale (ITS-90) and its dissemination using resistance thermometry. Today, more than a century after its invention, resistance thermometry plays a crucial role in various aspects of industry and everyday technology ranging from biomedicine to manufacturing process control, to energy production and consumption. Although well-calibrated industrial resistance thermometers can measure temperature with uncertainties as small as 10 mK, they are sensitive to mechanical shock, thermal stress and environmental variables such as humidity and chemical contaminants. Consequently, resistance thermometers require periodic (and costly) off-line recalibrations. These fundamental limitations of resistance thermometry have produced considerable interest in developing photonic temperature sensors2 that can deliver similar to better measurement capabilities whislt being more robust against mechanical shock. Such a devcie will appeal to national and industrial labs and those interested in long-term monitoring where instrument drift can negatively impact productivity.
In recent years a wide variety of novel photonic thermometers have been proposed including photosensitive dyes3, sapphire-based microwave whispering gallery mode resonator4, fiber optic sensors5,6,7, and on-chip silicon nano-photonic sensors8,9,10. At NIST, our efforts are aimed at developing low-cost, readily-deployable, novel temperature sensors and standards that are easily manufactured using existing technologies, such as CMOS-compatible manufacturing. A particular focus has been the development of silicon photonic devices. We have demonstrated that these devices can be used to measure temperature over the ranges of -40 &#176;C to 80 &#176;C and 5 &#176;C to 165 &#176;C with uncertainties that are comparable to legacy devices8. Furthermore, our results suggest that with a better process control device interchangeability on the order of 0.1 &#176;C uncertainty is achievable (i.e. the uncertainty of temperature measurement using nominal coefficients not calibration determined coefficients).

<table><tbody><tr><td>&lt;em&gt;Packaging process&lt;/em&gt;</td><td></td><td></td><td></td></tr><tr><td>6-axis stage</td><td>PI instruments</td><td></td><td></td></tr><tr><td>video cameras</td><td></td><td></td><td></td></tr><tr><td>epoxy dispensation system</td><td></td><td></td><td></td></tr><tr><td>Fiber array</td><td></td><td></td><td></td></tr><tr><td>&lt;em&gt;Temperature Measurement&lt;/em&gt;</td><td></td><td></td><td></td></tr><tr><td>Metrology Well</td><td>Fluke</td><td>9170</td><td>Dry well stable to better than .01 K</td></tr><tr><td>Laser</td><td>Newport</td><td>TLB6700</td><td>1520-1570 nm tunable laser</td></tr><tr><td>Wavemeter</td><td>HighFinesse</td><td>WS/7</td><td>100 Hz wavemeter</td></tr><tr><td>Power meter</td><td>Newport</td><td>1936-R</td><td>power meter with broad range</td></tr></tbody></table>

fabrication and testing of photonic thermometers

Fabrication and Testing of Photonic Thermometers

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being leveraged for developing sophisticated photonic sensors. Silicon photonic sensors seek to exploit the strong confinement of light in nano-waveguides to transduce changes in physical state to changes in resonance frequency. In the case of thermometry, the thermo-optic coefficient, i.e., changes in refractive index due to temperature, causes the resonant frequency of the photonic device such as a Bragg grating to drift with temperature. We are developing a suite of photonic devices that leverage recent advances in telecom compatible light sources to fabricate cost-effective photonic temperature sensors, which can be deployed in a wide variety of settings ranging from controlled laboratory conditions, to the noisy environment of a factory floor or a residence. In this manuscript, we detail our protocol for the fabrication and testing of photonic thermometers.

As shown in Figure 2, the ring resonator transmission spectra shows a narrow dip in transmission corresponding to the resonance condition. The resonance fringe shifts to longer wavelengths as temperature is increased from 20 °C to 105 °C in 5 °C increments. The transmission spectrum is fitted to a polynomial function from which the peak center is extracted. The polynomial fit was found to give the most consistent results in the presence of a sloping baseline ...

We describe the process of fabrication and testing of photonic thermometers.

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being ...

Photonic thermometry can help transition the field of temperature metrology from resistance-based legacy technology to frequency-based measurements. The main advantage of this technique is that we can leverage advances in frequency metrology to make more precise measurements whilst fabricating devices that overcome the physical limitations of current technology such as size and sensitivity to mechanical shock and environmental changes. The implication of this technique extend toward changing how we analyze in the United States and the world.An ultra stable photonic thermometer will reduce the need for frequent calibrations. Future development of optomechanical temperature standards can put the calibration standard in the user hands eliminating the need for specialized calibration facilities. Generally, individuals new to this method will struggle because it is an intersection of two divergent fields both of whom have their own language, technology requirements and specialized protocols for maximizing outcome.Any new user must learn to adapt and adjust to sometimes competing requirements. To begin, clean an SOI wafer as described in the accompanying text protocol. Coat the wafer with 20 to 50 milliliters MA-N 2405 negative tone photoresist.Spin it at 4, 000 RPM for 60 seconds and then transfer the wafer to a hot plate and bake it at 90 degrees Celsius for 15 minutes. After baking, expose the photoresist to the pattern shown here using a standard E-beam lithography setup. Then place the wafer into MIF 319 developer solution and incubate it for 60 seconds.Transfer the developed wafer into water and rinse it for an additional 60 seconds. Next, perform an ICP RIE etch of the 220 nanometer thick silicon layer to remove the unprotected silicon. Dissolve the resist mask in pure acetone for one hour, followed by an isopropanol rinse.Then rinse the wafer for 60 seconds in deionized water and dry the wafer using nitrogen. Now place the wafer back into the spin coater. Deposit a one nanometer thick protective polymer film top layer on the wafer.Finally, dice the wafer with a wafer dicing saw into 20 millimeter by 20 millimeter small and easy to handle chips. Place the photonic chip on the six-axis stage and orient the chip so that the on-chip input and output ports are aligned with the V groove array. Then turn on vacuum suction through on-stage integrated vacuum pumping port to hold the chip in place.Use the top view digital camera to locate and place the photonic devices of interest in the center of the six-axis stage. Now position the V groove array holder arm close to the chip and use vacuum suction through an integrated pumping port to hold the array in place. Using the side view digital cameras as a visual feedback, position the fiber array above the on-chip gradient couplers and raise the stage to bring the photonic chip to within 10 micrometers of the fiber array's bottom edge.The edge of the V groove fiber array should be roughly aligned within 50 to 100 micron accuracy relative to on-chip alignment marks. This procedure brings the optical fiber within a relative proximity of the corresponding gradient couplers. Once the chip has been roughly aligned, activate the automated search for the six-axis stage.This algorithm searches for the maximum transmission of broadband light through the chip's input and output ports. It should take no longer than 20 to 30 seconds. Once the optimal alignment is achieved, check device viability before proceeding with bonding.Using a program like LabVIEW, control the on-stage integrated module to thermally cycle the chip's temperature while recording the spectral response. Analyze the recorded the spectra from the laser spectrometer to verify the temperature sensitivity of the device. Slowly lower the array down to the chip's surface while viewing the side view digital camera.Next, carefully position the epoxy-filled syringe in close vicinity to the fiber array's edge using another XYZ micron precision stage. Once in position, dispense a single micro droplet of epoxy. While the epoxy hardens, periodically run the automated alignment routine to prevent drift-induced loss of signal.After the epoxy cures, test the photonic chip performance and light coupling efficiency by recording the transmission spectra at different temperatures. Light coupling efficiency typically increases after the bonding process. Use about one milligram of thermal grease to thermally couple the fiber-bonded photonic chip to a small copper cylinder.Then gently lower the chip copper cylinder down a glass tube. Once in position, back fill the glass tube with argon gas and seal it using a rubber cork. Then place the packaged photonic thermometer into a metrology temperature dry well stable to within one micro Kelvin.Using the custom-built computer program, set the settling time for 20 to 30 minutes, the number of thermal cycles to at least three, and the temperature step size to between one and five Celsius. Also, set the number of consecutive scans to at least five and the laser power in the nanowatt to microwatt range. As shown here, the ring resonator transmission spectra shows a narrow dip in transmission corresponding to the resonance condition at each temperature.The resonance fringe shifts to longer wavelengths as temperature is increased from 20 Celsius to 105 Celsius in five degree Celsius increments. Our preliminary analysis of the thermal cycling experiment suggests that the humidity-induced changes in the epoxy are likely the largest driver of hysteresis in packaged photonic thermometers and that unpackaged devices do not show any significant hysteresis. Additionally, the hysteresis in the packaged device can be ameliorated by using hydrophobic epoxy as a desiccant to the glass tube before sealing a tighter seal around the rubber cork glass junction.While attempting this procedure, it is important to remember to minimize any chemical contamination of the samples such as moisture in the packaged tube since it will severely degrade the measurement accuracy. Following this procedure, other methods like laser locking or dual frequency comb spectroscopy can be performed in order to answer additional questions about the long-term stability of these devices, impulse loading, and characterization of thermal physical properties. After its development, this technique has paved the way for researchers in the field of metrology to explore precision metrology for other physical and chemical quantities such as pressure, vacuum and trace gas analysis in embedded systems.Don't forget that working with harsh chemicals in a clean room and bright light sources such as lasers in the lab can be extremely hazardous and precautions such as the use of personal protective equipments such as laser goggles should always be taken while performing this procedure.

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