Capabilities

Capabilities
The Kostecki lab contains infrared, Raman, and XPS spectrometers with air-free measurement and mapping capability, AFM and optical microscopes, gloveboxes for air-free electrode preparation and cell assembly and potentiostats for cell testing. Group members also access shared LBL capabilities at the Molecular Foundry and conduct synchrotron x-ray work at the ALS.

Raman Spectroscopy

Our confocal Renishaw Qontor Raman system is equipped with 488nm and 633nm excitation lasers, a mapping stage capable of 100 nm spatial resolution, and autofocus with 16nm vertical precision. It also has a light-tight enclosure with feed-throughs for operando cell characterization. Some of our research using Raman is shown on our Raman research page.

Raman PhotographRaman Map of graphite signal overlaid on microscope image of composite cathode

 

 

 

 

 

 

Infrared Spectroscopy (FTIR)

Three spectrometers are available:

  1. A Shimadzu IR-tracer FTIR spectrometer housed in a nitrogen-filled environmental chamber for air-free measurements. It is equipped with an ATR attachment with Ga/Se, Si, Diamond/ZnSe crystals allowing for measurement of a large range of solids and liquids, and an optional transmissInfrared spectrometer and microscopeion measurement module.
  2. A Thermo-Fisher Nicolet 6700 or 4700 spectrometer equipped with a Nicolet Nexus 870 IR microscope (right). This versatile setup allows several different types of measurements:
    (a) Transmission measurements using a high resolution HgCdTe detector. The sample chamber can be filled with inert gas of choice.
    (b) IR Microscopy can be used to determine the microscale chemical distribution on the surface of a sample. The IR microscope can also be equipped with a reflectance attachment.
    (c) ATR measurements; coupling with an IR compatible electrochemical cell enables direct probing of electrode interfaces.

Thermo Electron Nicolet 5700 spectrometer (measures FTIR as well as UV-vis), coupled with an integrating sphere accessory. Additional accessories include a liquid flow cell, diamond horizontal ATR crystal, and grazing angle reflectance attachment.

 

X-ray Photoelectron Spectroscopy (XPS)

Photograph of XPS toolOur PHI 5400 XPS system is equipped with both an Al Kα and a Mg Kα source, which provide photons with 1486.6 eV and 1254.6 eV energy respectively. A mechanism for transfer of air sensitive materials from various glove boxes directly into the measurement system is available. Developing additional XPS capabilities for operando measurements is part of our ongoing research.

 

 

 

photograph of atomic force microscope

 

Atomic Force Microscopy (AFM)

Our Agilent (currently Keysight) AFM features a highly modular microscope and scanner. The AFM has two types of scanners: one for large scan area (90µm X 90µm) scanning and another one for high resolution (9µm X 9µm) scanning. It also has a variety of accessories such as an environment-control closure and a fluid operation sample stage which are suited for electrochemical applications.

 

Infrared Nanospectroscopy

near field infrared schematicphotograph of near field infrared system

Infrared nanospectroscopy is a unique tool available in the Kostecki lab. It combines atomic force microscopy (AFM) with infrared spectroscopy. Infrared light is focussed to the AFM tip, which locally amplifies the electric field of the incident beam. This enables infrared spectroscopy at a lateral and depth resolution on the order of the tip radius, i.e. ~10 nm. This greatly exceeds the normal diffraction limit for infrared light, and provides a unique nanoscale chemical mapping capability. The system is equipped with 3 tunable QCLs for IR nanoscopy and a broadband laser for nano-FTIR, and is housed in an environmental chamber to enable air-free experiments. The development of this technique is part of our ongoing research.

 

Spectral Ellipsometryphotograph of spectral ellipsometer

Spectral ellipsometry measures the ratio and phase shift between s- and p-polarized light upon reflection from a sample surface, as a function of wavelength. It is a fast, non-destructive technique for determining film thicknesses (1-1000 nm) and compositions particularly of flat, transparent films with planar interfaces.

 

Tools for Water Research

  1. Wescor 5600XR vapor pressure osmometer.This instrument measures the dew point temperature depression of a solution in vapor equilibrium in a closed chamber; it is more suitable than a freezing point depression measurement for viscous and concentrated samples, and does not require modification of the sample as it is performed at 25 °C.
  2. Solar simulator (Newport, 94081A)
  3. Forward Osmosis set up: acrylic cross-flow cell (Sterlitech Corporation). The cell consists of two symmetric channels for the feed and draw solutions separated by a thin film composite membrane with an effective area of 30 cm2. Feed and draw solutions are pumped using a peristaltic pump.
  4. Three custom built electrochemical work stations for electrode (flow and static) testing with influent and effluent pH and conductivity monitoring.

 

Splat Quencher and Arc-Melt Furnacephotograph of splat quencher

Our splat quencher (shown right) is a unique tool in the energy storage field. It is capable of melting reactive alloys with a maximum melting temperature of 2500°C via levitation melting. Subsequently, the molten droplet is rapidly cooled (with cooling rates up to 106 K/sec) by being splatted between two copper pistons to form amorphous metallic glasses. The instrument has a loading capacity of 80-200 mg, and produces a splat with a thickness of 20-100 µm and a diameter of 10-30mm.

Our arc-melt furnace (Materials Research Furnaces Inc.) has a single arc with a maximum operating temperature of 3500°C in an inert environment. The instrument is well-suited for intermetallic alloys synthesis for electrochemical energy storage applications. It is used to prepare the feedstock material for the splat quencher.

 

Gloveboxes and Potentiostats

We have four VAC gloveboxes for Li ion battery work dedicated to electrolyte and electrode preparation and cell assembly and testing. Multiple bio-logic potentiostats are available for cell testing, and feed-throughs are available to test cells inside a glovebox if needed. A range of different electrochemical cells, as well as the resources to construct custom cells for specific experiments, are available.

photograph of lab, showing multiple glove boxes

 

Berkeley Lab User Facilities

Molecular Foundry: foundry.lbl.gov

Advanced Light Source (ALS): als.lbl.gov