Calorimeter

Patent metadata

Field	Value
Publication number	US-12523625-B2
Application number	US-202118034096-A
Country	US
Kind code	B2
Filing date	Oct 20, 2021
Priority date	Oct 30, 2020
Publication date	Jan 13, 2026
Grant date	Jan 13, 2026

Abstract

Provided herein is technology relating to calorimetry and particularly, but not exclusively, to apparatuses, methods, and systems for making high-resolution thermodynamic measurements of reactions between gas phase reactants and nanomaterials. For example, the technology can provide thermodynamic measurements with a high heat flow resolution and long term stability at a wide range of temperatures and reaction pressures. The technology is used, for example, to study the thermodynamics of surface reactions and phase transformations in nanomaterials.

First claim

We claim:

1 . A calorimetry system comprising:
i) a calorimetry apparatus comprising:
a capillary comprising a sample holder capsule;
an inner thermal shield encapsulating the capillary and in thermal communication with the capillary; and
an outer thermal shield encapsulating the inner thermal shield and thermally isolated from an environment; and
ii) a gas handling unit configured to provide a gas phase reactant to the sample holder capsule,
wherein said gas handling unit comprises:
a gas handling unit capillary tube coupled to the calorimetry apparatus capillary; and
a prechamber configured to hold and provide the gas phase reactant to the gas handling unit capillary tube.

2 . The calorimetry system of claim 1 , wherein said apparatus has a heat flow resolution of less than 3 μW/√Hz.

3 . The calorimetry system of claim 1 , wherein said apparatus operates over a temperature range of 20° C. to 300° C.

4 . The calorimetry system of claim 1 , wherein said sample holder capsule comprises the gas phase reactant.

5 . The calorimetry system of claim 1 , wherein said sample holder capsule comprises a solid phase reactant.

6 . The calorimetry system of claim 5 , wherein said solid phase reactant has a mass of 1-10 mg.

7 . The calorimetry system of claim 5 , wherein said solid phase reactant comprises a nanomaterial.

8 . A method of measuring a heat transfer for a chemical reaction, said method comprising:
providing the calorimetry system of claim 1 ; reacting a solid phase reactant with the gas phase reactant in said sample holder capsule; and recording a heat transfer measurement of heat produced by reacting said solid phase reactant with said gas phase reactant.

9 . The method of claim 8 , further comprising providing said gas phase reactant using said gas handling unit.

10 . The method of claim 8 , wherein said heat transfer measurement has a resolution of less than 3 μW/√Hz.

11 . The method of claim 8 , further comprising removing gas from a volume enclosed by said outer thermal shield or enclosed by said gas handling unit to provide a pressure of less than 10, 9, 8, 7, 6, or 5 μTorr.

12 . The method of claim 8 , further comprising heating the outer thermal shield.

13 . The method of claim 8 , wherein said solid phase reactant has a mass of 1-10 mg.

14 . The method of claim 8 , wherein said solid phase reactant comprises a nanomaterial.

15 . The method of claim 8 , wherein recording the heat transfer measurement comprises using a thermistor ultrasonically soldered to said capillary.

16 . The method of claim 8 , further comprising quantifying a mass of said gas phase reactant.

17 . The method of claim 8 , further comprising quantifying a mass of said gas phase reactant that reacts with said solid phase reactant to form a product.

Assignees

• Univ Michigan Regents
• Google Llc

Inventors

• Meyhofer Edgar
• Reddy Pramod
• Fork David
• Lim Ju Won
• Reihani Amin

Classifications

• G01N25/20

  by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity (calorimeters per se G01K) · CPC title

• G01N25/4886

  concerning the circulation of the sample · CPC title

• G01N25/486

  Sample holders · CPC title

• G01N25/4826

  concerning the heating or cooling arrangements (heating apparatus for chemical or physical laboratory apparatus in general B01L7/00) · CPC title

• G01K17/04

  Calorimeters using compensation methods {, i.e. where the absorbed or released quantity of heat to be measured is compensated by a measured quantity of heating or cooling} · CPC title