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Title: Modulation calorimetry in diamond anvil cells. II. Joule-heating design and prototypes

Abstract

Here, Part I shows that quantitative measurements of heat capacity are theoretically possible inside diamond anvil cells via high-frequency Joule heating (100 kHz–10 MHz), opening up the possibility of new methods to detect and characterize transformations at high-pressure such as the glass transitions, melting, magnetic orderings, and the onset of superconductivity. Here, we test the possibility outlined in Part I, using prototypes and detailed numerical models. First, a coupled electrical-thermal numerical model shows that specific heat of metals inside diamond cells can be measured directly using ~1 MHz frequency, with <10% accuracy. Second, we test physical models of high-pressure experiments, i.e., diamond-cell mock-ups. Metal foils of 2–6 μm-thickness are clamped between glass insulation inside diamond anvil cells. Fitting data from 10 Hz to ~30 kHz, we infer the specific heat capacities of Fe, Pt, and Ni with ±20%–30% accuracy. The electrical test equipment generates -80 dBc spurious harmonics, which overwhelm the thermally induced harmonics at higher frequencies, disallowing the high precision expected from numerical models. An alternative Joule-heating calorimetry experiment, on the other hand, does allow absolute measurements with < 10% accuracy, despite the -80 dBc spurious harmonics: the measurement of thermal effusivity, $$ \sqrt{ρck}$$ (ρ, c, and k being density, specific heat, and thermal conductivity), of the insulation surrounding a thin-film heater. Using a ~50 nm-thick Pt heater surrounded by glass and 10 Hz–300 kHz frequency, we measure thermal effusivity with ±6% accuracy inside the sample chamber of a diamond anvil cell.

Authors:
 [1];  [1]; ORCiD logo [2];  [2]
  1. Carnegie Inst. for Science, Washington, DC (United States). Geophysical Lab.
  2. Univ. of California, Berkeley, CA (United States)
Publication Date:
Research Org.:
Carnegie Inst. of Washington, Washington, DC (United States)
Sponsoring Org.:
USDOE National Nuclear Security Administration (NNSA)
OSTI Identifier:
1535306
Alternate Identifier(s):
OSTI ID: 1361810
Grant/Contract Number:  
NA0002006; CDAC
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Applied Physics
Additional Journal Information:
Journal Volume: 121; Journal Issue: 14; Journal ID: ISSN 0021-8979
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
42 ENGINEERING; Physics; Thin films; Diamond anvil cells; Thermodynamic states and processes; Thermodynamic properties; Calorimetry; Thermal conductivity; Bridge circuit; Signal generators; Numerical methods; Harmonic distortion

Citation Formats

Geballe, Zachary M., Struzhkin, Viktor V., Townley, Andrew, and Jeanloz, Raymond. Modulation calorimetry in diamond anvil cells. II. Joule-heating design and prototypes. United States: N. p., 2017. Web. doi:10.1063/1.4979850.
Geballe, Zachary M., Struzhkin, Viktor V., Townley, Andrew, & Jeanloz, Raymond. Modulation calorimetry in diamond anvil cells. II. Joule-heating design and prototypes. United States. https://doi.org/10.1063/1.4979850
Geballe, Zachary M., Struzhkin, Viktor V., Townley, Andrew, and Jeanloz, Raymond. Mon . "Modulation calorimetry in diamond anvil cells. II. Joule-heating design and prototypes". United States. https://doi.org/10.1063/1.4979850. https://www.osti.gov/servlets/purl/1535306.
@article{osti_1535306,
title = {Modulation calorimetry in diamond anvil cells. II. Joule-heating design and prototypes},
author = {Geballe, Zachary M. and Struzhkin, Viktor V. and Townley, Andrew and Jeanloz, Raymond},
abstractNote = {Here, Part I shows that quantitative measurements of heat capacity are theoretically possible inside diamond anvil cells via high-frequency Joule heating (100 kHz–10 MHz), opening up the possibility of new methods to detect and characterize transformations at high-pressure such as the glass transitions, melting, magnetic orderings, and the onset of superconductivity. Here, we test the possibility outlined in Part I, using prototypes and detailed numerical models. First, a coupled electrical-thermal numerical model shows that specific heat of metals inside diamond cells can be measured directly using ~1 MHz frequency, with <10% accuracy. Second, we test physical models of high-pressure experiments, i.e., diamond-cell mock-ups. Metal foils of 2–6 μm-thickness are clamped between glass insulation inside diamond anvil cells. Fitting data from 10 Hz to ~30 kHz, we infer the specific heat capacities of Fe, Pt, and Ni with ±20%–30% accuracy. The electrical test equipment generates -80 dBc spurious harmonics, which overwhelm the thermally induced harmonics at higher frequencies, disallowing the high precision expected from numerical models. An alternative Joule-heating calorimetry experiment, on the other hand, does allow absolute measurements with < 10% accuracy, despite the -80 dBc spurious harmonics: the measurement of thermal effusivity, $ \sqrt{ρck}$ (ρ, c, and k being density, specific heat, and thermal conductivity), of the insulation surrounding a thin-film heater. Using a ~50 nm-thick Pt heater surrounded by glass and 10 Hz–300 kHz frequency, we measure thermal effusivity with ±6% accuracy inside the sample chamber of a diamond anvil cell.},
doi = {10.1063/1.4979850},
journal = {Journal of Applied Physics},
number = 14,
volume = 121,
place = {United States},
year = {Mon Apr 10 00:00:00 EDT 2017},
month = {Mon Apr 10 00:00:00 EDT 2017}
}

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