Energy, Nanomechanics, and Surfaces Research Laboratory

Lab Facilities

Essential equipment in Y.-T. Cheng’s lab (1864 sq. feet) at the University of Kentucky and at the Center for Applied Energy Research, as well as shared facilities at the University of Kentucky Electron Microscopy User Facility and Center for Nanoscale Science and Engineering. Shared facilities are marked in blue.

Battery Research Capabilities on UK Campus

Synthesis capabilities

  • Solid-state reactions
  • Mechanical alloying/Cryo Milling
  • Physical vapor deposition
  • Microwave plasma surface modification
  • Electrodeposition
  • Electrostatic deposition
  • Electrospinning

Modeling capabilities

  • Analytical
  • Numerical (Matlab, R)
  • Finite element (COMSOL, ABAQUS)
  • Quantum mechanics (VASP)

Characterization capabilities

  • Micro- and nano-scale characterization of mechanical behavior of materials
  • Micro-indentation and nano-indentation up to 700oC
  • Impact and fatigue tests
  • Scratch, friction, and wear tests
  • TA rheometers
  • Peel and adhesion tests
Electrochemical  measurements for energy storage  and corrosion research
  • Potentiostat/Galvanostat/Electrochemical Impedance spectroscopy
  • Multi-channel battery cycler
  • Battery cell assembly (coin cells)
  • Environmental chamber
  • Electrochemical quartz crystal microbalance
  • In situ electrochemical/mechanical stress sensor
  • In situ electrochemical nanoindentation

Scanning probe microscopy - Atomic Force Microscopy (contact, tapping, lateral force modes), conducting tip, Scanning Electro-Chemical Microscopy, and Scanning Kelvin Probe

 

 

 

 

Battery Research Capabilities at UK/CAER

 

 

 

PARSTAT®2273-Advanced Electrochemical System and Software: The 2273 is an advanced potentiostat/galvanostat/Frequency-Response-Analyzer (FRA) that consists of hardware capable of ± 10 V scan ranges, 2 A current capability, and Electrochemical Impedance Spectroscopy (EIS) measurements from 10 μHz to 1 MHz. It is being used to perform electrochemical characterization of battery electrode materials. It is also used together with AT- and BT-cut quartz crystal oscillators for E-DQCM measurements.

Potentiostat/Galvanostat/EIS (Princeton Applied Research, 2273)

 

VersaSTAT 3 Potentiostat/ Galvanostat and Software: This is a versatile potentiostat/galvanostat for studying corrosion, energy storage, and sensors.

Potentiostat/Galvanostat (Princeton Applied Research, VersaSTAT3)

 

BioLogic VMP3 Multipotentiostat/Galvanostat and Software: This 16 channel potentiostat and galvanostat allows 16 electrochemical measurements simultaneously for electrochemical studies of batteries. One of the channels is capable of Electrochemical Impedance Spectroscopy (EIS).

16-channel Potentiostat/Galvanostat/EIS (Bio-Logic, VMP3)

 

BioLogic BCS-805 16 Channel Research Grade Battery Cycler with Software

BioLogic BCS-805

 

BioLogic MPG2 16 Channel Research Grade Battery Cycler with Software: The MPG2 is for research on intercalation compounds, batteries, and supercapacitors. Each channel is an independent potentiostat/galvanostat with a maximum current of 100 mA.

16-channel Potentiostat/Galvanostat (Bio-Logic, MPG2)

 

Arbin BT-G-25 16 Channel Electrochemical Testing System with Software: The system is provides comprehensive tools for testing batteries, super-capacitors, and other types of electrochemical cells. The voltage range is 0 to 5 V. Maximum charge/discharge current is 5A and maximum channel power is 25W.

Arbin BT-G-25 16 Channel Electrochemical Testing System

 

INFICON/Maxtek Quartz Crystal Monitor and Crystal Holders for Liquid Environment: The monitor provides up to three channels of crystal measurement utilizing Maxtek’s highly accurate phase- lock oscillator technology for measuring film properties. The liquid cell and crystal holder allows the crystal to oscillate in electrolytes. Together with the PARSTAT®2273, the Crystal Monitor is used for E- DQCM measurements.

Two MBraun LABMASTER Workstation (Glovebox with 4 gloves): This glovebox provides an inert environment for handling air sensitive materials, e.g., lithium ion batteries.

MBraun LABMASTER Workstation with Nano Indenter G200 inside

 

Innovative Technology Glovebox (with 2 gloves): This glovebox provides an inert environment for handling air sensitive materials.

TestEquity Model 1007 Temperature Chamber: This chamber provides controlled temperatures ranging from -70 to 175oC.

Hohsen Coin Cell Crimper: This automatic coin cell crimper produces CR 2025-type coin cells with excellent reproducibility and repeatability.

Homemade glass capillary electrochemical cells and transparent electrochemical cells: These cells allow in situ observation of electrodes, including liquid-solid phase transformation, during electrochemical experiments.

WS Tyler Ro-Tap Sieving Kits: This Sieving kits automatically select the particle size of powders. Available size ranges from 300 μm to 20 μm.

Kurabo Mazerustar KK250S planetary mixer: The mixer produces ideal slurry for fabricating battery electrodes.

Kurabo Mazerustar KK250S planetary mixer

 

Kinematica Polytron™ Model PT 10-35 GT-D Homogenizer: Powerful and versatile benchtop homogenizer; Completely homogenizes samples from 0.1 to 4000mL; Powerful 1200W motor provides quiet and reproducible results.

Homemade High-Precision Casting Kits: High-precision casting kits are used for coating electrodes. The thickness of coating varies from 120 μm to 5 μm with different blades.

MTI Pouch Cell Fabrication Facility (located at UK’s Center for Applied Energy Research):

  • UL Standard 1200°C Split Tube Furnace with Vacuum Flanges & Quartz Tube 80mm O.D
  • Bench-Top Planetary Ball Mill with four Nylon Jars (500mL) & Lock Clamps
  • 2 Liter Tri-Shaft Planetary Vacuum Mixer with Vacuum Pump and Water Chiller
  • Compact Tape Casting Film Coater with Dryer, Vacuum Chuck & Adjustable Film Applicator
  • 4" Electric Hot Rolling Press / Calender up to 100°C with Variable Speed
  • Pouch Cell Case/Cup Forming Machine for Aluminum-Laminated Films with Die
  • Semi-Automatic Die Cutter for Pouch Cell electrode Sheet
  • Desk-Top 800W Ultrasonic Metal Welder ( Tabbing ) with Touch-Screen Digital Controller
  • UL Standard 53L 250°C Vacuum Oven (16x13x14" ) with Programmable Controller
  • Semi-Automatic Stacking Machine for Pouch Cell
  • Compact Heating Sealer for Sealing Laminated Aluminum Case of Pouch Cells
  • Glove Box with H2O & O2 Purification System and Openable Front Window
  • Bottletop Electrolyte Digital Dispenser with 32oz Boston Round Glass Bottle
  • Electrolyte Diffusion & Degassing Chamber for Professional Li-on Battery Research
  • Compact Vacuum Sealer for Preparing Pouch Cell
  • 8 Channel Battery Analyzer (0.1-10mA, up to 5V) Adjustable Cell Holders Laptop & Software

Maccor Series 4000 Automated Test System with 48 channels (located at UK’s Center for Applied Energy Research): Electrochemical tests of  batteries, electrochemical capacitors, and fuel cells.

Model AL200-DP Microwave Gas Plasma System by Plasmatech, Inc: Deposition of coatings and surface modification of materials.

Gas Plasma System (plasmatech, inc.)

 

Atomic Layer Deposition System by Cambridge NanoTech Inc: 3D conformal nano-meter thick coatings of oxides, nitrides, and fluorides. The system has been used to deposit coatings on electrodes for improved performance and durability.

Several e-beam and Magnetron Sputtering Deposition Systems: Shared facilities for making thin film and nanostructures.

Box furnace 30400 Thermolyne Furnace, 1200°C

Tube furnace OTF-1500X-GSL 1200°C

Tube furnace OTF-1500X-GSL 1200°C

Nano Indenter G200 by Agilent Technologies Inc with an electrochemical cell for in situ mechanical property measurements in controlled environments. The nanoindenter is situated inside a glovebox filled with argon gas. Nanoindentation measurements can be conducted between room temperature and 100oC.

G200 inside a glovebox

Enviornmental Nanoindentation:

  1. A method used to measure mechanical properties such as elastic modulus and hardness at a microscopic level.
  2. Housed in an argon-filled glovebox which enables indentation on air and moisture sensitive samples.

 

Environmental Nanoindentation: Liquid Indentation

  • Use electrolyte resistant epoxy to mount sample.
  • Soak sample in electrolyte and add a few drops of electrolyte to immerse the sample.
  • Indenter stayed immersed in electrolyte during indentation.
  • Able to obtain the mechanical properties in a more realistic environment. 

 

 

NanoTest Vantage by Micro Materials Ltd capable of nanoindentation (both quasi-static and dynamic), nano-impact and fatigue, nano-scratch and wear, and nano-fretting measurements at ambient and high temperatures up to 650oC.

NanoTest Vantage: Nano-Indentation

 

 

TA Instruments AR-1000 controlled stress rheometer: Viscosity measurements

TA Instruments HR-2 Discovery Hybrid Rheometer System

TA Instruments HR-2 Discovery Hybrid Rheometer System

 

Brookfield Viscometers

X- ray diffraction: A Siemens D500 XRD system and a Siemens D5000 XRD system for determining the crystal structure, grain size, and residual stresses in materials. A modified coin cell has been designed, built, and tested for in situ XRD of electrode materials for battery research.

SEM (Scanning Electron Microscope)-Hitachi 3200S with Environmental Chamber: In addition to the standard capabilities of an SEM the Hitachi 3600 has a spatial resolution of 3.5 nm, variable pressure working environment (up to 2 Torr), digital image processing capability, a specimen current and induced current amplifier system, an independent solid state backscattered electron detection system, an independent cathodoluminescence detection system, dual signal imaging, and an energy dispersive X-ray spectrometer (EDS) system (≥atomic No. 4).

SEM-Hitachi S900 Field Emission SEM: The Hitachi S900 is an "in-lens" system which can image at very high resolution (0.5 nm). The specimens are placed inside the objective lens to maximize resolution and minimize aberrations, thus resulting in extremely high quality imaging.

JEOL 2000FX Transmission Electron Microscope (TEM): The JEOL 2000X is equipped with EDS and scanning transmission electron microscopy (STEM) and can be used for lattice imaging.

JEOL 2010F (TEM): The JEOL 2010F is capable of achieving high resolution lattice imaging. The instrument can also be operated in scanning mode (STEM), and has chemical measurement options such as electron energy loss spectroscopy (EELS), and EDS. Analytical TEM can be performed with this instrument.

Digital Instruments Atomic Force Microscope (AFM): Operated with a Nanoscope IIIa Multiprobe scanning microscope, this AFM runs in either contact or tapping mode.

Micro-Computer Tomography: SCANCO MEDICAL µCT 40 to determine the structure of 3D specimens.

Thermo Scientific K-Alpha X-ray Photoelectron Spectrometer (XPS) system: surface composition and chemical analysis

Thermo Scientific K-Alpha XPS system

AFM: Bruker Dimension icon GB 115

AFM technique examples:

  • Peakforce Tapping Mode, tapping mode, contact mode (topography)
  • Peakforce Quantitative Nanomechanics (PF-QNM) (local elastic modulus)
  • Peakforce Tunneling AFM (PF-TUNA) (local electronic conductivity)
  • Datacube TUNA: taking an array of IV curves
  • Kelvin Probe Force Microscopy (KPFM) (local work function and contact potential difference)

AFM: Quantitative NanoMechanical Mapping (QNM)

  • Contact mechanics at a smaller scale than nanoindentation (tip radius ~10 nm).
  • Allows for mapping of elastic modulus. Various regions of composite materials can be visualized if moduli are sufficiently different.


AFM: Peakforce QNM example: Elastic modulus of polyacrylic acid film


AFM: Peakforce TUNA example: Local electronic conductivity

 


AFM: AM-KPFM example: LLZO

 


Future work: Advanced AFM techniques