Accelerated Rate Calorimetry

Instrument Modes

  • Heat-search mode: Initially, the heating elements in the adiabatic chamber heats the sample a little, stops, and let the sensors search for self-heatup. If the self-heatup is above a prespecified value, the cycle stops, and we go in to adiabatic mode.
  • Adiabatic mode: The self-heatup is measured.
    • Events: Self-heatup initializing temp, Venting temp (for cells), accelerated heat output and uncontrolled heat output (thermal runway)
      • Separator meltdown: Endotherm reaction displayed by small lowering of heat generation.
  • Usual specifics:
    • Instrument: EV+ARC from Thermal Hazard Technologies.
      • Videocamera, Window, two cable connections, pressure sensor, and gas release.
      • Chamber: 40cm diameter, 44cm depth. Sealed by Si-gasket and 40kg lid with magnet lock released at 1bar overpressure.
      • Program: ARC-ES v6.3.2
    • Heat rate:
      • Heated to \(60^\circ\)C, thereafter \(5^\circ\)C steps in the searching phase.
      • Wait time was 50 minutes, and search time is determined by software.
      • With self-heat rate above\(0.2^\circ\)C/min, it eneters adiabatic mode.
      • Measured until \(250^\circ\)C or until heat rate is below \(0.2^\circ\)C/min

Source: M.Sc. degree of Torleif Lian (FFI)

Sample holder

  • Should be described in detail.
  • Will absorb heat from the experiment: Lower temp rise than expected
  • Heat lost by sample container can be explaied by the \(\varphi\)-factor:
    • \(\varphi = 1 + \frac{m_b c_b}{m_s c_s}\)
    • m = mass, c = heat cap, b = bomb, s = sample
    • Ideally: It should be close to that of a full lithium cell

Analytics

  • Lowered heat-rate may not be because of a break between two exotherms, but rather an endoterm. This can be indicated by pressure increase at the temperature where the endotherm is: Why would there be a pressure increase if there is no reaction?