Method for measuring the coefficient of heat conductivity of a sample

• US 5,711,604 A
• Filed: 11/03/1995
• Issued: 01/27/1998
• Est. Priority Date: 12/14/1993
• Status: Expired due to Term

• Current Assignee: SII Nano Technology Inc. (Hitachi, Ltd.)
• Original Assignee: Seiko Instruments Incorporated (Seiko Group)
• Inventors: Nakamura, Nobutaka
• Primary Examiner(s): GUTIERREZ, DIEGO F
• Application Number:
  US08/552,548
• Time in Patent Office: 816 Days
• Field of Search: 374/44, 374/10, 374/12, 374/16, 374/31, 374/11
• US Class Current: 374/44
• CPC Class Codes: G01N 25/18 by investigating thermal conductivity by calorimetry G01N25/20; by measuring change of resistance of an electrically-heated body G01N27/18
• CPC Class Codes: G01N 25/4866 by using a differential method

Abstract

A method for measuring the coefficient of thermal conductivity of a solid sample material by: heating a meltable calibration sample having good thermal conductivity to its melting temperature by raising the temperature of an analyzer at a controlled rate and causing heat to flow through a path having a thermal resistance to the calibration sample, the heating being performed one time with the solid sample material interposed in the path so that heat flows through the path and through the solid sample material, and one time with the solid sample material removed so that heat flows only through the path; deriving thermal analysis curves each representing a relation between heat flow to the calibration sample and the controlled rate at which the analyzer temperature is raised, during melting of the calibration sample in respective performances of the heating step; and determining the coefficient of thermal conductivity of the solid sample material based on the solid sample material thickness and a characteristic of the thermal analysis curves at the melting temperature of the calibration sample.

Claims

1. A method for measuring the coefficient of thermal conductivity of a solid sample martial having a known thickness and having a thermal resistance, said method comprising:

heating a meltable calibration sample having good thermal conductivity to its melting temperature in a sample station of a thermal analyzer by raising the temperature of the analyzer at a controlled rate and causing heat to flow to the calibration sample through a path having a thermal resistance, said heating step being performed one time with the solid sample material interposed in the path so that heat flows through the path and through the solid sample material, and one time with the solid sample material removed so that heat flows only through the path;

deriving thermal analysis curves each representing a relation between heat flow to the calibration sample and the controlled rate at which the analyzer temperature is raised, over a temperature range which contains the melting temperature of the calibration sample during respective performances of the heating step; and

determining the coefficient of thermal conductivity of the solid sample material based on the solid sample material thickness and a characteristic of the thermal analysis curves at the melting temperature of the calibration sample.

2. A method as defined in claim 1 wherein the thermal analyzer is a differential thermal analyzer or a differential scanning calorimeter for observing heat flows to and from a sample in relation to a standard sample which does not undergo a thermal transformation.

3. A method as defined in claim 2 wherein the sample station includes a container made of aluminum, silver, or stainless steel, and the calibration sample is housed within the container.

4. A method as defined in claim 2 wherein the characteristic of the thermal analysis curves which is used to determine the coefficient of thermal conductivity is the maximum absolute value of the slope of each curve at the start of melting of the calibration sample.

5. A method as defined in claim 4 wherein the coefficient k, of thermal conductivity is determined by calculating the equation ##EQU2## where:

t is the thickness of the sample material;

P is the absolute value of the rate of change of the thermal analysis curve at the melting temperature of the calibration sample and with the solid sample material;

Q is the absolute value of the rate of change of the thermal analysis curve at melting temperature of the calibration sample and without the solid sample material interposed in the path;

A is an effective surface area associated with the solid sample material; and

B is the controlled rate at which the temperature is raised in the sample station.

6. A method for measuring the coefficient of thermal conductivity of a solid sample material having a known thickness and having a thermal resistance, said method comprising:

placing the solid sample material and a meltable calibration sample having good thermal conductivity in a heat flow path having a thermal resistance in a sample station of a thermal analyzer;

heating the meltable calibration sample to its melting temperature in the sample station by raising the temperature of the analyzer at a controlled rate and causing heat to flow to the calibration sample and the solid sample material through the heat flow path;

deriving a thermal analysis curve representing a relation between heat flow to the calibration sample and the controlled rate at which the analyzer temperature is raised, over a temperature range which contains the melting temperature of the calibration sample during the heating step;

comparing the thermal analysis curve derived in said deriving step with a thermal analysis curve produced by raising the temperature of the analyzer at a controlled rate and causing heat to flow to the calibration sample through the heat flow path, with the solid sample material removed from the flow path; and

determining the coefficient of thermal conductivity of the solid sample material based on the solid sample material thickness and a characteristic of the thermal analysis curves at the melting temperature of the calibration sample.