This chapter has been adapted in part from:
Nathan H. Thomas, Michelle C. Sherrott, Jeremy Broulliet, Harry A. Atwater, and Austin J. Minnich. Electronic Modulation of Near Field Radiative Transfer in Graphene Field Effect Heterostructures. In preparation, 2019
4.1 Introduction
Having determined the sample geometry in the previous chapter, in this chapter we are now ready to describe the experiment that can measure the predicted heat flux modulation. Near field radiative heat transfer experiments fall into one of three categories, defined largely by the geometry of the sample being investigated. In one case, the samples are “large”1 and planar, separated from one another by physical spacers [27, 29, 31, 32, 38]. In the second case, the samples are much smaller, typically fabricated using modern lithographic techniques and are suspended above one another by piezo-actuators [28, 33, 34, 134]. Experiments in the final category employ a planar sample and a spherical atomic-force microscope tip [30, 57, 58].
Naturally, each of these experiments comes with their own set of unique trade offs. In the first case, the experimental setup can use commercial heat flux and temperature sensors and doesn’t require intricate control of piezoactuators and custom resistive thermometers that are necessary for the other two classes of experiments. However, the samples must be polished sufficiently flat to allow for 100 to 1000 nm scale gaps across an area∼1 cm2. In the other cases, the sample uniformity is less important, but the sample positioning is complicated and the temperature sensors are custom Pt resistors or AFM tips. In this thesis, we investigate the electrostatic modulation of cross-plane heat transfer of large area gate-tunable samples. For that reason, we construct an instrument, building off the previous works from the first class of experiments. In this chapter, we introduce the instrument design and sample fabrication protocol.
1Large is a purposely vague term, but it mainly refers to samples with bulk substrates that can be manipulated with the human hand.
4.2 Instrument Layout
A diagram and photo of the instrument layout are shown in Figure 4.1. The heart of the instrument is a Janis ST-100 cryostat, which houses the sample and is connected to a Lakeshore 355 PID temperature controller. The temperature controller has two independent PIDs for precise control of two heating elements. The first is connected to the cryostat cold finger, which is kept cold with a liquid nitrogen reservoir, and acts as the heat sink for the thermal absorber. The second is connected to an insulated Kapton resistive heater, which acts as the heat source for the thermal emitter. A diagram of the cryostat and heater layout are shown in Figure 4.2a. At the base of the cryostat is the sample stage, which is screwed to the coldfinger, as shown in Figure 4.2b. The stage is designed to be removed without disturbing the graphene device, such that it can be ferried in and out of the clean room without dust getting between the top and bottom samples.
The other necessary components shown in Figure 4.1, are the DAQ9211 National Instruments microvolt meter, the Keithley 2410 source meter, and the Fluke 8808a multimeter. The DAQ9211 is used to measure thermocouple signals and the micro- volt signal from the heat flux sensor. The Keithley 2410 supplies the bias to the bottom graphene sample, and the Fluke multimeter has two functionalities.
The first and primary use of the Fluke multimeter is to measure the graphene surface resistance while it is being biased. The bias at which the surface resistance is maximized is the charge neutral point (CNP), or where the graphene Fermi level is near zero. The second use is to measure the input power into the resistive heater to calibrate the heat flux sensor, as described in Section 4.3. To measure both signals independently with a single multimeter (but at separate times), we employ a computer controlled multiplexer switch box. A circuit diagram of the switch box is shown in Figure 4.3.
The box contains 8 USB-controlled relays each with three input-output leads:
normally-closed (NC), normally-open (NO), and common (C). As wired, the switch
(a) Diagram of Instrument Layout
(b) Photo of Instrument Layout
Figure 4.1: Complete layout of heat transfer measurement instrument. The sample is housed inside the cryostat that is pumped to∼1×10−6Torr. The multi-meter, muV meter, voltage source, and switch box are all controlled from a custom computer interface.
(a) Diagram of cryostat
(b) Photo of Sample Stage at Base of Cryostat Coldfinger Figure 4.2: Cryostat diagram and photo of sample stage.
Figure 4.3: Diagram of Switch Box Circuit
box offers a way to measure three independent resistance or voltage signals and a single current measurement. The three resistance and voltage signals are labeled as Resistance 1, Resistance 2, and Voltage, but all three circuit paths go to the same HI and LO leads of the multimeter. The difference in the three signals lies only in how the multimeter is programmed. To measure the applied heating power, both the current and a voltage switches are opened as shown in Figure 4.4, where the arrows indicate the current path. The ammeter connections for the multimeter are through the LO and mA leads. The heating power applied to the resistive heater is simply the product of the current and voltage.
4.3 Heat Flux Sensor Calibration
The heat flux sensor is an Omega HFS-4 thermopile that produces a voltage response proportional to a linear thermal gradient, which is in turn proportional to the heat flux through the sensor. The sensor must be calibrated to determine the conversion factor between incident heat flux and output voltage. As the sensor voltage relates to the incident heat flux by the temperature dependent Seebeck effect and thermal
conductivity, the heat flux sensor must be calibrated at all working temperatures. The final temperature dependent calibration factors were determined over three stages.
In the first stage, the temperatures were kept within 100◦C of room temperature to determine the sensor’s basic functionality. In the second stage, temperatures were decreased to close to 90 K to determine the thermal leakage out of the heater. In the final stage, after leakage pathways were determined inconsequential, the sensor was calibrated across all temperatures from room temperature to 90 K.