IP Library Granted Patent US 11,963,446
Granted Patent B2
US 11,963,446 · App. 16/712,629 · Granted Apr 16, 2024

Methods for making high-temperature thermocouples

Inventors: Richard S. Skifton (Idaho Falls, ID); Alma J. Palmer (Idaho Falls, ID); Kurt Davis (Idaho Falls, ID); Joshua Daw (Idaho Falls, ID); Pattrick Calderoni (Idaho Falls, ID)
Assignee: Battelle Energy Alliance, LLC
H10N10/01C21D9/52G01K15/005G01R19/03H01B13/0016H10N10/17H10N10/854
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Quick Facts
Patent No.
US 11,963,446
App. No.
16/712,629
Granted
Apr 16, 2024
Kind
B2
Abstract

Methods of manufacturing thermocouples having a first thermoelement wire comprises a molybdenum-lanthanum based material and a second thermoelement wire comprises a phosphorus-doped niobium, may involve exposing a first thermoelement wire and a second thermoelement wire to a temperature in a range extending from about 50° C. to about 60° C. above an intended operational temperature of the first and second thermoelement wires and until a rate of change of a normalized voltage output of the first thermoelement wire and the second thermoelement wire is about 0.001 normalized Volts per hour or less.

Claims (30)

1. A method of manufacturing a thermocouple, comprising:

exposing a thermocouple junction comprising a first thermoelement wire and a second thermoelement wire to a temperature in a range extending from 50° C. to 60° C. above an intended operational temperature of the first and second thermoelement wires and until a rate of change of a normalized voltage output of the first thermoelement wire and the second thermoelement wire is 0.001 normalized Volts per hour or less than 0.001 normalized Volts per hour, wherein the first thermoelement wire comprises a molybdenum-lanthanum based material and the second thermoelement wire comprises a phosphorus-doped niobium.

2. The method of claim 1 , wherein exposing the thermocouple junction comprising first thermoelement wire and the second thermoelement wire to the temperature comprises exposing the thermocouple junction comprising the first and second thermoelement wires to a temperature of 1650° C.

3. The method of claim 1 , wherein exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature comprises subjecting a portion of each of the first thermoelement wire and the second thermoelement wire to a thermal gradient of at least 60° C. during operation of the thermocouple junction.

4. The method of claim 1 , wherein exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature comprises exposing an entire length of the first thermoelement wire and the second thermoelement wire to the temperature.

5. The method of claim 1 , further comprising:

disposing the first thermoelement wire and the second thermoelement wire in respective apertures of an electrically insulating material;

swaging a metallic tube on the first thermoelement wire and the second thermoelement wire to form the thermocouple junction therebetween; and

disposing the first thermoelement wire, the second thermoelement wire, and the thermocouple junction in a sheath.

6. The method of claim 5 , wherein exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature further comprises exposing the thermocouple junction comprising the first thermoelement wire, the second thermoelement wire, and the sheath to the temperature.

7. The method of claim 1 , further comprising selecting the first thermoelement wire comprising between 0.5 percent by weight and 1.0 percent by weight of lanthanum oxide and between 98.95 percent by weight and 99.45 percent by weight molybdenum.

8. The method of claim 1 , further comprising selecting the second thermoelement wire comprising between 99.5 percent by weight and 99.8 percent by weight niobium and between 490 parts-per-million and 1,000 parts-per-million phosphorus.

9. The method of claim 1 , wherein exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature until the rate of change of the normalized voltage output of the first thermoelement wire and the second thermoelement wire is 0.001 normalized Volts per hour or less than 0.001 normalized Volts per hour comprises exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature until the rate of change of the normalized voltage output of the first thermoelement wire and the second thermoelement wire is between 0.001 normalized Volts per hour and 0.0001 normalized Volts per hour.

10. The method of claim 1 , wherein exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature until the rate of change of the normalized voltage output of the first thermoelement wire and the second thermoelement wire is 0.001 normalized Volts per hour or less than 0.001 normalized Volts per hour comprises exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature for a duration in a range extending from 4 hours to 6 hours.

11. The method of claim 1 , wherein exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature comprises exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to a temperature between 50° C. and greater than a maximum intended operating temperature of the thermocouple.

12. The method of claim 1 , wherein exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to the temperature in the range extending from 50° C. to 60° C. above the intended operational temperature of the first and second thermoelement wires comprises exposing the thermocouple junction comprising the first thermoelement wire and the second thermoelement wire to a temperature in a range extending from 1150° C. to 1650° C.

13. A method of heat-treating a thermocouple, comprising:

measuring an output voltage of a thermocouple while exposing a first thermoelement wire and a second thermoelement wire to a temperature between 50° C. to 60° C. above a predetermined operational temperature of the first and second thermoelement wires; and

maintaining the first thermoelement wire and the second thermoelement wire exposed to the temperature until a rate of change of a normalized voltage output of the first thermoelement wire and the second thermoelement wire is between 0.001 normalized Volts per hour and 0.0001 normalized Volts per hour.

14. The method of claim 13 , wherein exposing the first thermoelement wire and the second thermoelement wire to the temperature comprises exposing the first and second thermoelement wires to a temperature of 1650° C.

15. The method of claim 13 , further comprising:

disposing the first thermoelement wire and the second thermoelement wire in respective apertures of an electrically insulating material;

swaging a metallic tube on the first thermoelement wire and the second thermoelement wire to form a thermocouple junction therebetween; and

disposing the first thermoelement wire, the second thermoelement wire, and the thermocouple junction in a sheath.

16. The method of claim 13 , wherein exposing the first thermoelement wire and the second thermoelement wire to the temperature until the rate of change of the normalized voltage output of the first thermoelement wire and the second thermoelement wire is between 0.001 normalized Volts per hour and 0.0001 normalized Volts per hour comprises exposing the first thermoelement wire and the second thermoelement wire to the temperature for a duration in a range extending from 4 hours to 6 hours.

17. The method of claim 13 , wherein exposing the first thermoelement wire and the second thermoelement wire to the temperature comprises exposing the first thermoelement wire and the second thermoelement wire to a temperature between 50° C. and 60° C. greater than a maximum intended operating temperature of the thermocouple.

18. The method of claim 13 , wherein measuring the output voltage of the thermocouple while exposing the first thermoelement wire and the second thermoelement wire to the temperature between 50° C. to 60° C. above the predetermined operational temperature of the first and second thermoelement wires comprises measuring the output voltage of the thermocouple while exposing the first thermoelement wire and the second thermoelement wire to a temperature between 1150° C. and 1650° C.

19. A thermocouple subjected to a method of heat treating, the method comprising:

exposing a thermocouple junction comprising a first thermoelement wire and a second thermoelement wire to a temperature in a range extending from 50° C. to 60° C. above an intended operational temperature of the first and second thermoelement wires and until a rate of change of a normalized voltage output of the first thermoelement wire and the second thermoelement wire is 0.001 normalized Volts per hour or less than 0.001 normalized Volts per hour, wherein the first thermoelement wire comprises a molybdenum-lanthanum based material and the second thermoelement wire comprises a phosphorus-doped niobium.

20. The thermocouple of claim 19 , wherein exposing the thermocouple element junction comprising the first thermoelement wire and the second thermoelement wire to the temperature in the range extending from 50° C. to 60° C. above the intended operational temperature of the first and second thermoelement wires comprises exposing the thermocouple element junction the first thermoelement wire and the second thermoelement wire to a temperature in a range extending from 1150° C. to 1650° C.

Assignments (2)
CONFIRMATORY LICENSE Recorded Apr 27, 2020
From: BATTELLE ENERGY ALLIANCE/IDAHO NAT'L LAB
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 052505/0914 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 12, 2019
From: SKIFTON, RICHARD S.; PALMER, ALMA J.; DAW, JOSHUA; CALDERONI, PATTRICK; DAVIS, KURT
To: BATTELLE ENERGY ALLIANCE, LLC
Reel/Frame 051269/0535 →
Continuity (2)
Provisional Application 62779354 · Dec 13, 2018
Related Publication 20200194652A1 · Jun 18, 2020