Hildreth Research Group has 123 m² (1,320 ft²) of chemical lab space on the second floor of the CoorsTek Center for Applied Science and Engineering  dedicated to nanoscale to centimeter scale additive manufacturing research.  This lab space includes 4.9 meters (16 feet) of chemical fumehoods, 44 meters (144 ft) of bench space, and two nitrogen glove boxes.

These facilities contain much of the fabrication and metrology equipment necessary to study the chemical kinetics, mass transport, heat transfer, and corrosion phenomena involved in printed reactive inks, dissolvable metal supports, and ultra near-field electrohydrodynamics.

Below lists some of our major fabrication, characterization, and synthesis equipments.

Microfab Jetlab II with precision stage, stage mapping calibration, and digital pnuematic controller upgrades.  Print can print up to four inks/materials serially.  Horizonatal cameras and sequenced strope illumaiton for jet setup and vertical camera for alignment and post-print inpsection.  Printer software supports print-on-the-fly and point-to-point print modes. Specifications include heated stages up to 170 ˚C; XY-travel range of 200 mm x 200 mm; velocity/acceleration up to 100 mm/s and 400 mm/s² respectively; accuracy/repeatbility ±3 µm / ± 1 µm.  Current nozzle sizes in use range from 5 µm to 100 µm in diameter.

NOTE: we are currently moving our Jetlab II into a glove box for printing in inert atmospheres.

Nordson Pro4 3-Axis Dispensing Robot with integrated z-height laser measuring system.  This 3-axis dispensing printer has 400 mm ⨉ 400 mm ⨉ 4 mm travel; ± 4 µm position repeatability; ± 1 µm z-height measurement accuracy on opaque and transparent substrates.  The printer is equipped with an Instec heated vacuum chuck (-120 ˚C to 210 ˚C).   This printer is used to metallize photovoltaic cells and investigate the impact of reaction kinetics on the morphology and materials properties of printed reactive inks.

This is a lab-built Electrohydrodynamic (EHD) printer for nanoscale additive manufacturing.  Printer consists of a two 3-axis Newport Stages (macro-stage and piezoelectric nano-stage), integrated Nanosurf AFM, and high speed amplifier capable of +/- 10,000 V with slew rates up to 700 V/µS.

Lindberg/Blue M 1200°C Split-Hinge Tube Furnace, single-zone (24″ heated length), 5440 W, 3″ tube furnace with digital controller used to sensitize non-ferrous alloys in inert environments.  

DT-22-FL-8-VA Deltec Front Loading Furnace. 1200 ˚C Front Loading Atmosphere Envelope Laboratory Furnace with Vacuum Capability with a working volume 8″ wide x 8″ deep x 8″ high and a manual side hinged “swing” door. Complete with stainless steel sealed enclosure, Viton O-ring Sealing (good in vacuum down to .01 Torr and pressures up to one atmosphere), four gas throughways, silicone carbide heating elements, Eurotherm 3504 auto-tuning programmable controller with Modbus TCP/IP Communications; type K control thermocouple; zero crossover SCR; over temperature protection (includes limit controller, contactor, and Type K thermocouple), and Nema One control cabinet with side hinged door for easy access to all components

SEMTech Solutions Refurbished Amray 3300 Field Emission Scanning Electron Microscope (FESEM) equipped with WIN10TM SEMView8000 Technology, an Energy-Dispersive X-ray Spectroscopy (EDXS) using a Silicon Drift 30 mm2 SDD Detector, Back Scattered Electron (BSE) Detector, and an IR Chamberscope.  System includes a 305 Schottky field emission source with 100 V to 30 kV accelerating voltage.  Image resolution is 1.5 nm at 30kV accelerating voltage.    5 axis translates 125 mm ⨉ 125 mm ⨉ 100 mm with -5˚ to + 90˚ tilt and 360˚ rotation.  SEMView8000 supports up to 8k images and video.  EDS supports point, line, and area elemental mapping.

Ametek (formerly Princeton Applied Research) PARSTAT Multichannel Potentiostat Chassis equipped with eight PMC 1000 potentiostats (±12V, ±2 A, 2 MHz EIS) and one PMC 10A booster.  Specifications include: synchronized voltage/current/auxiliary sampling at 500k samples/sec; electrochemical impedance spectroscopy up to 1 MHz; rise time <500 ns; applied voltage resolution between 305 nV to 300 µV depending on voltage range; voltage accuracy of ±0.2%; applied current accuracy of ±0.2% with a minimum resolution of 6.1 pA; voltage and current measurements down to 6 µV and 122 fA; and EIS rnage of 1 MHz to 10 µHz.

The Ametek (formerly Princeton Applied Research) Model 616A Electrode Rotator is a high precision, low mass rotator that performs well with virtually any potentiostat. When connected to Princeton Applied Research electrochemical instrumentation, it uses control lines to give a remote start/stop and speed control. Using the convenient control panel and input jacks, the model 616 can easily be operated for either manual or automated experiments.

Pine Research Instruments RCE Jacketed Corrosion Cell.  Jacketed corrosion cell with drain used to measure the electrochemical and corrosion response of sensitized metals and printed reactive inks.

Pine Instruments WaveNow Portable Potentiostat/Galvanostat.  Specifications include:  ±4 V at 125 µV per DAC bit with ±0.2% accuracy; 80 µA to 100 mA with ±0.2% setting and ±0.05% range accuracy.

TA Instruments Q20 Differential Scanning Calorimete (DSC) with RCS40 cooling system from -40 ˚C to 400 ˚C and T-Zero Press and Die set.  Specifications include: ≤100 µW baseline flatness; <40 µW baseline repeatability; ±0.1°C temperature accuracy;  ±0.01°C temperature pression; ±0.1 enthalpy precision; dual gas input (N2 and O2).  This DSC is used to meaasure enthalpy of reactions, heat of vaporizations, and reaction kinetcs of new reactive ink systems.

TA Instruments Q50 Thermogravimetric Analyzer (TGA) equipped with evolved gas analysis furnace for sampling output gasses in our Nicolete iS-10 FTIR.  Specifications include: 1 gram maximum sample weight; ±0.01% weighing precision; 0.1 µg sensitivity; < 50 µg baseline dynamic drift; temperature range up to 1,000 ˚C (480 ˚C limit when gas evolution furance is used); ±1 ˚C isothermal temperature accuracy; ±0.1 ˚C isothermal temperature precision; heating rate from 0.1 to 100 ˚C/min.  This TGA is used to measure solvent partial pressures, reaction temperatures, reaction product vaporization temperatures/rates.

Nicolete iS-50 Fourier Transform Infrared (FTIR) spectrometer with TGA-IR and Attenuated Internal Reflectance (ATR) modules for collecting spectra from gas evolved from our Q50 TGA and solids/liquids respectively.  Specifications include: 0.4 cm^-1 Standard Resolution (variable resolution from 64 to 0.4 cm^-1); 1 minute signal to noise ratio better than 35,000:1; BaF2 coated, KBr windows; KBr/Ge coated beamsplitter (7800-350 cm^-1); deuterated triglicine sulfate detector (7800-350 cm^-1).  This FTIR with TGA-IR and ATR modules is used to monitor/measure reaction products, reaction rates, and partial pressures.

Mettler-Toledo S470 pH/Conductivity Meter with the following probes for measuring fluid conductivity and pH.  Electrodes include: inLab 710 – 0.1 – 500 mS/cmS/cm; inLab 720 – 0.1 – 500 µS/cm; and InLab Power Pro pH.

Elveflow OB1-MkIII base with 2 channels installed  Each channel has a pressure range of ±1 bar with microfluidic flow sensors accurate to 0.01% for flows up to 80 µL/min.  

Rheosense microVisc portable rheometer for measuring the viscosity of our reactive inks at room temperature.  Specifications include: 100 µL sample volume; 1.7 – 5,800 s^-1 shear rate range; 0.2 – 20,000 cP viscosity range; 2% accuracy of reading and 0.5 % of full scale repeatability (scale depends on visocity sensor chip); 0.15 ˚C built in temperature sensor.

Motic BA310MET-T Trinocular Optical Microscope with 5x, 10x, 50x 100x objectives  10x eye piece, and 20 MP digital camera.  Works in reflective and transmission modes with polarizer and analyzer optical filters.

Signatone S302-4 Four-Point Probe Station for measuring film resistance.  Station is connected to a Keysight 34420A Nanovolt meter to measure film resistance using sensitivity DCV and resistance measurements at 100 pV and 100 nOhm.

Keysight 34420A Nano-volt/Micro-ohm Meter for DCV and resistance measurements at 100 pV and 100 nOhm.  USB connectivity compatible with NI-VISA communication protocols.  Used with Signantone S-302-4 Four Point Probe station to measure the resistance of films printed using reactive inks.

Trek 10/10B-HS High-Voltage, High-Speed Amplifier.  This is a DC stable, high-speed, high-voltage power amplifier capable of precise control of output voltages. It features an all-solid-state design for high slew rate up to 700 V/µS, wide bandwidth and low-noise operation.  This amplifier is used to apply the driving potentials used in our Nano-drip EHD printer.

Keysight 33510A Two Channel Arbitrary Waveform Generator used to supply waveforms to our Trek 10/10B-HS-L-CE high voltage amplifier for the EHD Nano-drip printer.  Specifications include: up to 20 MHz with 160 MSa/s sampling rate, 16-bit resolution, and USB connectivity compatible with NI-VISA communication protocols

Keysight DSOX3024A Oscilloscope 4 analog channels up to 200 MHz with waveform option enabled.   USB connectivity compatible with NI-VISA communication protocols

Keysight N2790A High Voltage Floating Probes with 10:1 or 100:1 reduction for monitoring high voltage signals up to 25 MHz.  Used with our DSOX3024A Oscilloscope.

Keysight N2790A High Voltage Floating Probes with 10:1 or 100:1 reduction for monitoring high voltage signals up to 25 MHz.  Used with our DSOX3024A Oscilloscope.

Keysight U3606B 30 Watt DC Power Supply with built-in multimeter; 30V/1A or 8V/3A.  Supported measurements include 2-wire and 4 wire resistancemeasurement; frequency, capacitance, continuity, and diode tests.  USB connectivity compatible with NI-VISA communication protocols

Keysight 34411A Benchtop Multimeter to monitor voltage and current.   USB connectivity compatible with NI-VISA communication protocols

Glowforge Basic uses onboard cameras and a powerful laser to make lab fixtures and boxes. 40 W Class 1 laser product and is exhausted through the lab exhaust ventilation system.

World Precision Instruments PUL-1000 Micropipette Puller is a microprocessor controlled micropipette puller with up to four programmed sequence steps.  Typical tip is 1 µm in diameter with larger diameters achieved using our microbeveler.  This puller and microbeveler combination is used to fabricate tips for a EHD nano-drip printer.

World Precision Instruments MBS Microbeveler System to bevel micropipette tips pulled using our PUL-1000 micropipette puller.  Used to bevel tips larger than 1 µm, system is variable speed and includes a SYS-48000 microbevler, light source, microscope, and abrasion accessories.

Plasma Etch Venus 25 Benchtop Plasma Cleaning System equipped with two digital flow controllers to support dual gas plasma environments.  The entire system is digitally controlled for improved repeatbility.  Specificaitons include 400 W, 50 KHz continuously varialbe power supply with automatic matching network.  Equipment is used for sample cleaning, substrate preparation, and adjusting substrate termination for controlling substrate surface energy.

Ika RV10 Rotary Evaporator System with integrated vacuum controller, cooling water management, bath temperature and safety features for distilling reactive inks and removing excess solvent.

Purelab Flex 3 18.2 MΩ-cm Deionized Water Polisher supplies polished tap water (supplied by RO water in the lab) to Ultrapure Type I water in one step with purity up to 18.2 MΩ-cm with reverse osmosis recirculating through  185/254 nm UV and Deionization Purification. 

Comsol Multiphysics simulation software with the following modules: AC/DC, computational fluid dynamics (CFD), chemical reaction engineering, corrosion, heat transfer, MEMS, microfluidics, particle tracing, structural mechanics, materials library, and LiveLink for MATLAB.

Apple’s Xcode Integrated Developer Environment is used to write custom software for data analysis and controlling research equipment. These projects are often written by volunteer and FURI undergraduate research assistants studying from the computer science department.  These projects give students hands-on experience writing code for scientific applications.

This is an open-sourced project to develop SwiftVISA – a Swift wrapper for NI-VISA. It is similar to PyVISA, with several differences. As with PyVISA, you can use SwiftVISA to control various measurement devices.