logo 1.png

  Structure and Microstructure Study Platform

This platform is dedicated to the characterization of (micro-)structure, morphology, ionic mobility, thermal phase properties, and thermal stability of the material constituents of energy storage/conversion/saving devices. Users of this platform's techniques will have the ability to establish structure-property-electrochemical performance relationships and orient the synthesis of materials and processing conditions.

 

Hyphenated Thermogravimetric Analyser - Infrared Spectroscopy - Gas Chromatography/Mass Spectrometry  System 
(TGA-IR-GCMS)

TGA (TGA 8000) - IR spectrophotometer (Spectrum Two) - GC (Clarus 690)/MS (Clarus SQ 8 S), PerkinElmer

This system consists of four instruments: a thermogravimetric analyzer (TGA), an infrared spectrophotometer (IR), a gas chromatograph (GC), and a mass spectrometer (MS) hyphenated by two transfer lines. This TGA-IR-GC/MS system allows a user to vaporize or decompose a sample by heating, measure its mass loss, and simultaneously analyze the chemical composition of the sample. The transfer lines are heated at 270˚C to avoid condensation of the evolved gas.

The TGA can operate at temperatures ranging from room temperature to 1100˚C under flowing nitrogen, argon or helium. The mass spectrometer is used (with the help of the NIST MS Search Program) to identify the composition of the evolved gas. The gas chromatograph can be used to resolve each component through the column and better distinguish a sample’s chemical composition by the MS. The IR data (obtained in a continuous mode by a specified rate) can be coupled to the TGA and/or GC/MS results to confirm the chemical identity determined by the mass spectra library.

 

To learn more about evolved gas analysis and the possibilities offered by this technique as well, click here.

 

The TGA module can be booked as a stand-alone instrument for routine thermogravitational analyzes (see below).  

Hyphenatedjpg
 

Thermogravimetric Analyser
(TGA)

TGA 8000, PerkinElmer

On this TGA, an optical null ultra-microbalance, isolated in a temperature-compensated balance chamber, ensures stability and provides the capability of measuring the smallest weight changes. With its two integrated mass-flow controllers, it is possible to purge the furnace (sample) and the balance with distinct gases. The sample purge gases offered are helium, argon and nitrogen. Its low mass and forced-air cooling allow it to cool quickly for fast sample turnaround.

Our TGA permits the analysis of volatile and humidity/air-sensitive samples through the Accupick accessory. The accessory has a needle that is attached to a stem fixed under the balance system of the TGA. When the autosampler is raised, the needle punctures the cover of the Accupik pan (made of aluminum). The pan capacity is about 30µL and is suitable to liquid and solid samples.

 

The specification list of the instrument is available here.

TGA 8000.jpg
 

Mercury Intrusion Porosimetry Analyser

AutoPore V, Micromeritics

Mercury porosimetry provides a wide range of information, e.g. pore size distribution, total pore volume or porosity, skeletal and apparent density, and specific surface area of a sample. The AutoPore V provides measurements of pore radii from several hundreds of microns down to 3 nm, covering the size range of the materials and electrodes commonly used in electrochemical systems but also in broad range of other systems, from  aerospace materials to medical implants. The available pressure range span from 0.2 psia to 60 kpsia, with a controlled pressure increase as fine as 0.05 psi. The sub-microliter (better than 0.1 µL) measurement of intrusion/extrusion volumes permits the characterization of tighter samples and high-quality characterization data.

The specification list of the instrument is available here.

20210604_094113-1.jpg
 

Differential Scanning Calorimeter
(DSC)

DSC 6000, PerkinElmer

 

The DSC 6000 is a heat-flux DSC that permits the direct calorimetric measurement, characterization, and analysis of thermal properties of materials. The Intracooler module permits thermal analyses between -65°C to 650°C and allows a wide range of heating and cooling rates. Capable of complex temperature programming and sensitive to minimal variations of heat flux for advanced thermodynamics study, this instrument is also available for routine measurements to be carried out.

The specification list of the instrument is available here.

DSC 6000.jpg

Microwave Plasma Atomic Emission Spectroscopy

(MP-AES)

4210 MP-AES, Agilent

 

The Agilent MP-AES is a compact, bench-top microwave plasma-atomic emission spectrometer based on a robust, nitrogen plasma. It is suitable for elemental determinations using a solid-state CCD detector. With its microwave plasma source, this MP-EAS provides superior detection limits
to flame atomic adsorption (AA) spectroscopy and similar to what it is achievable with ICP-MS. 
This instrument will principally be used to quantify the metallic content in battery electrolytes, but can be accessed to analyze elemental content in a very diverse array of samples ranging from food and agriculture to environmental, geochemical and petrochemical applications. 

 
 

X-Ray Diffractometer for In Situ & In Operando Measurements 
(ISIO-XRD)

Empyrean, Malvern Panalytical

This XRD has the unique ability to measure different sample types, i.e., powders, thin films, nanomaterials, solid objects, on a single instrument. The diffractometer comes with an optimized configuration: reflection and transmission modes, soft X-rays (Co tube) for fluorescing elements like Fe, Co, Mn, which are found in most battery electrode materials, and more deeply penetrating hard X-rays (Mo and Ag) for pair distribution function (PDF) measurements, computed tomography and ISIO-XRD analysis of electrochemical cells in transmission mode. Appropriate optics and a CdTe based sensor, with 100% efficiency even for hard X-rays, reduces the measurement time or improve the quality of the data collected. A high-temperature chamber for X-ray diffraction studies in different atmospheres is available for in-situ investigations of chemical reactions, phase transitions or ISIO electrochemical studies on all solid-state batteries (ASSBs) as function of temperature.

 

The XRD is hosted in the X-Ray Diffraction Laboratory of Université de Montréal. Please contact Prof. Mickaël Dollé or Thiery Marris (X-Ray Diffraction Lab) for your inquiries on the instrument. 

20201126_145634_edited_edited.jpg

(external site)

 

In Situ Solid-State NMR
(ssNMR)

Add-ons to solid-state NMR spectrometers (400 MHz and 600 MHz), Bruker

We offer state-of-the-art, high-speed magic-angle spinning (MAS) probes (spin rate up to 67 kHz) that can be used for studying the structure and dynamics of materials. For dynamic studies, a special laser-based design, which heats only the sample holder (rotor), allows temperatures up to 700 K to be attained. Diffusion and imaging (MRI) capacities provide insights into the structural and dynamic properties of electrolytes, as well as on the local changes in solid phases. With this ssNMR setup, it is possible to probe local environment of Li and Na nuclei in battery materials. 

 

The ssNMR is hosted in the Regional Centre of NMR spectroscopy of Université de Montréal. Please contact Prof. Mickaël Dollé or Cédric Malveau (Centre of NMR spectroscopy) for your inquiries on the instrument.