Apparatus and method for controlling atmospheres in heat treating of metals

• US 20060263256A1
• Filed: 03/29/2006
• Published: 11/23/2006
• Est. Priority Date: 05/17/2005
• Status: Abandoned Application

• Current Assignee: Nitrex Metal, Inc. (Canada)
• Original Assignee: Nitrex Metal, Inc. (Canada)
• Inventors: Korwin, Michel J., Koshel, Dimitri
• Application Number:
  US11/391,348
• Publication Number:
  US 20060263256A1
• Time in Patent Office: Days
• US Class Current: 422/83
• CPC Class Codes: C23C 8/06 using gases C23C8/36 takes precedence
• CPC Class Codes: G01N 21/0303 Optical path conditioning in cuvettes, e.g. windows; adapted optical elements or systems; path modifying or adjustment G01N21/031 - G01N21/15 take precedence
• CPC Class Codes: G01N 21/0332 with temperature control control of temperature G05D23/00; cryostats F17C3/08
• CPC Class Codes: G01N 21/05 Flow-through cuvettes G01N21/09 takes precedence; handling fluid samples G01N1/10
• CPC Class Codes: G01N 21/3504 for analysing gases, e.g. multi-gas analysis

Abstract

The present invention relates to an absorption gas analyzer for measuring a concentration of at least a component gas in a sample gas. The absorption gas analyzer comprises a main absorption cell for containing the sample gas for measurement therein. At least a narrow band emitter emits electromagnetic radiation in at least a predetermined narrow wavelength band which is transmitted through the main absorption cell. A reflecting device is disposed for reflecting the electromagnetic radiation after transmission through the main absorption cell such that the electromagnetic radiation is transmitted again therethrough. At least a detector detect the electromagnetic radiation and provide at least an intensity signal in dependence upon the concentration of the at least a component gas. The absorption gas analyzer enables simultaneous determination of concentration of a plurality of individual component gases with a high level of accuracy.

Claims

1. An absorption gas analyzer for measuring a concentration of at least a component gas in a sample gas comprising:

a main absorption cell for containing the sample gas at a predetermined temperature and a predetermined pressure for measurement therein;

at least an electromagnetic radiation source for providing electromagnetic radiation in at least a predetermined narrow wavelength band, the predetermined narrow wavelength band being within a wavelength range of a predetermined absorption band of each of the at least a component gas, the electromagnetic radiation for being transmitted through the main absorption cell;

a reflecting device disposed for reflecting the electromagnetic radiation after transmission through the main absorption cell such that the electromagnetic radiation is transmitted again therethrough; and

,

at least a detector for detecting the electromagnetic radiation after the second transmission through the main absorption cell and for providing at least an intensity signal in dependence upon the concentration of the at least a component gas, the at least a detector being placed at a predetermined distance from the reflecting device with the predetermined distance including a predetermined defocusing distance.

2. An absorption gas analyzer as defined in claim 1 wherein the at least an electromagnetic radiation source comprises at least a narrow band emitter absent a filter.

3. An absorption gas analyzer as defined in claim 2 wherein the at least a narrow band emitter is one of a LED and a Laser Diode.

4. An absorption gas analyzer as defined in claim 3 wherein the at least a narrow band emitter is a pulsed emitter.

5. An absorption gas analyzer as defined in claim 4 wherein the pulsed emitter is capable of operating in a quasi-continuous mode.

6. An absorption gas analyzer as defined in claim 3 wherein at least one of the at least a detector is sensitive in a wavelength range comprising at least a predetermined narrow wavelength band.

7. An absorption gas analyzer as defined in claim 3 wherein the at least a narrow band has a bandwidth between 1 nm and 150 nm.

8. An absorption gas analyzer as defined in claim 7 wherein the electromagnetic radiation is emitted in a wavelength range of infrared radiation.

9. An absorption gas analyzer as defined in claim 2 comprising a reference emitter for emitting a reference electromagnetic radiation in a wavelength band outside absorption bands of the sample gas, the electromagnetic radiation for being transmitted through the main absorption cell, reflected at the reflecting device, and transmitted again therethrough.

10. An absorption gas analyzer as defined in claim 9 comprising a reference detector for detecting the reference electromagnetic radiation.

11. An absorption gas analyzer as defined in claim 2 wherein a window of the main absorption cell facing the at least a detector comprises a sloped surface, the surface being sloped such that backscattered electromagnetic radiation is substantially prevented from impinging onto the at least a detector.

12. An absorption gas analyzer as defined in claim 11 comprising a primary reference detector for detecting a portion of the electromagnetic radiation prior transmission through the main absorption cell.

13. An absorption gas analyzer as defined in claim 2 comprising at least an emitter/detector temperature control device in thermal communication with the at least an emitter and the at least a detector.

14. An absorption gas analyzer as defined in claim 13 wherein the emitter/detector temperature control device comprises a thermoelectric cooler.

15. An absorption gas analyzer as defined in claim 2 comprising a main absorption cell temperature control device covering at least a portion of an outside surface of the body of the main absorption cell.

16. An absorption gas analyzer as defined in claim 15 comprising:

an inlet and an outlet in fluid communication with the main absorption cell, the inlet for being in fluid communication with a processing apparatus for receiving a sample gas therefrom; and

,

a pressure control device in communication with at least one of the inlet and the outlet.

17. An absorption gas analyzer as defined in claim 16 wherein the inlet and the outlet are disposed at a first end of the main absorption cell.

18. An absorption gas analyzer as defined in claim 17 comprising:

a conduit disposed inside the main absorption cell, the conduit being in fluid communication with the inlet and having at least an opening at a second opposite end of the main absorption cell.

19. An absorption gas analyzer as defined in claim 18 wherein the conduit is disposed in a spiraling fashion.

20. An absorption gas analyzer as defined in claim 16 comprising a processor in signal communication with the at least a detector for receiving data indicative of the at least an intensity signal for determining a concentration of the at least a component gas in dependence thereupon.

21. An absorption gas analyzer as defined in claim 20 comprising a gas inflow control communication link for providing control communication between the processor and a gas inflow controller of the processing apparatus.

22. An absorption gas analyzer for measuring a concentration of at least a component gas in a sample gas comprising:

a main absorption cell for containing the sample gas at a predetermined temperature and a predetermined pressure for measurement therein;

at least an electromagnetic radiation source for providing electromagnetic radiation in at least a predetermined narrow wavelength band, the predetermined narrow wavelength band being within a wavelength range of a predetermined absorption band of the at least a component gas, the electromagnetic radiation for being transmitted through the main absorption cell;

an interfering gas cell containing an interfering gas comprising an absorption band which is partially overlapping the wavelength band of one of the at least a narrow band emitter;

a reflecting device disposed for reflecting the electromagnetic radiation after transmission through the main absorption cell such that the electromagnetic radiation is transmitted again therethrough; and

,

at least a detector for detecting the electromagnetic radiation after the second transmission through the main absorption cell and for providing at least an intensity signal in dependence upon the concentration of the at least a component gas.

23. An absorption gas analyzer as defined in claim 22 wherein the interfering gas cell is interposed between at least the one of the at least an emitter and the main absorption cell.

24. An absorption gas analyzer as defined in claim 22 wherein the interfering gas cell is interposed between the main absorption cell and the reflecting device.

25. An absorption gas analyzer as defined in claim 22 wherein the at least an electromagnetic radiation source comprises at least a narrow band emitter absent a filter.

26. An absorption gas analyzer as defined in claim 25 comprising:

an interfering gas reference emitter for emitting electromagnetic radiation in a wavelength band outside absorption bands of the sample gas, the interfering gas reference emitter being disposed such that its electromagnetic radiation is transmitted through the main absorption cell without passing through the interfering gas cell; and

,

an interfering gas reference detector for detecting the electromagnetic radiation of the interfering gas reference emitter after passing through the main absorption cell and for providing an interfering gas reference intensity signal in dependence thereupon.

27. An absorption gas analyzer as defined in claim 26 comprising a component gas cell containing a component gas having an absorption band which is overlapping the wavelength band of the one of the at least an emitter.

28. A method for measuring a concentration of at least a component gas in a sample gas representative of an atmosphere in a processing apparatus comprising:

a) providing in a main absorption cell the sample gas at a predetermined temperature and a predetermined pressure for measurement therein;

b) transmitting electromagnetic radiation through the main absorption cell, the electromagnetic radiation being provided from at least an electromagnetic radiation source in at least a predetermined narrow wavelength band within a wavelength range of a predetermined absorption band of the at least a component gas;

c) reflecting the electromagnetic radiation using a reflecting device;

d) transmitting the reflected electromagnetic radiation through the main absorption cell; and

,

e) detecting the electromagnetic radiation after the second transmission through the main absorption cell at a predetermined distance from the reflecting device with the predetermined distance including a predetermined defocusing distance and providing at least an intensity signal in dependence upon the concentration of the at least a component gas.

29. A method for measuring a concentration of at least a component gas as defined in claim 28 wherein the electromagnetic radiation is emitted from at least a narrow band emitter absent a filter.

30. A method for measuring a concentration of at least a component gas as defined in claim 29 wherein a) to e) are performed simultaneously for the at least a component gas.

31. A method for measuring a concentration of at least a component gas as defined in claim 29 wherein a) to e) are performed successively for each of the at least a component gas.

32. A method for measuring a concentration of at least a component gas as defined in claim 29 comprising:

f) determining a concentration of the at least a component gas in dependence upon the at least an intensity signal.

33. A method for measuring a concentration of at least a component gas as defined in claim 32 comprising;

g) determining at least a potential with respect to the at least a component gas based on the determined concentration of the at least a component gas.

34. A method for measuring a concentration of at least a component gas as defined in claim 33 comprising:

h) comparing the at least a determined potential with at least a predetermined potential value to produce at least a comparison result and if at least one of the comparison results is not within predetermined limits providing a control signal for adjusting the concentration of the at least one component gas of the atmosphere in the processing apparatus.

35. A method for measuring a concentration of at least a component gas as defined in claim 34 comprising:

i) repeating a) to h) until each of the comparison results is within predetermined limits.

36. A method for measuring a concentration of at least a component gas as defined in claim 35 comprising:

j) repeating a) to i) at predetermined time instances.

37. A method for measuring a concentration of at least a component gas as defined in claim 33 comprising:

receiving a hydrogen sensor signal indicative of a concentration of hydrogen in the atmosphere for determining a potential of at least a component gas.

38. A method for measuring a concentration of at least a component gas as defined in claim 32 comprising:

determining at least a transfer function for use in determining the concentration of at least a component gas.

39. A method for measuring a concentration of at least a component gas as defined in claim 32 comprising:

providing non absorbent gas in the main absorption cell;

performing b) to d);

detecting the electromagnetic radiation after the second transmission through the main absorption cell and providing at least a calibration intensity signal for correcting subsequent concentration measurements in dependence thereupon.

40. A method for measuring a concentration of at least a component gas as defined in claim 32 comprising:

transmitting reference electromagnetic radiation in a wavelength band outside absorption bands of the sample gas through the main absorption cell;

reflecting the reference electromagnetic radiation;

transmitting the reflected reference electromagnetic radiation through the main absorption cell;

detecting the reference electromagnetic radiation after the second transmission through the main absorption cell and providing a reference intensity signal in dependence upon the concentration of the at least a component gas; and

,

determining the concentration of the at least a component gas in dependence upon the at least an intensity signal and the reference intensity signal.

41. A method for measuring a concentration of at least a component gas as defined in claim 32 comprising:

detecting reflected electromagnetic radiation prior transmission through the main absorption cell and providing a primary reference intensity signal in dependence thereupon.

42. A method for measuring a concentration of at least a component gas as defined in claim 41 comprising:

determining the concentration of the at least a component gas in dependence upon the at least an intensity signal and the primary reference intensity signal.

43. A method for measuring a concentration of at least a component gas as defined in claim 41 comprising:

controlling intensity of the electromagnetic radiation emitted from the at least a narrow band emitter based on the primary reference intensity signal.

44. A method for measuring a concentration of at least a component gas as defined in claim 41 comprising:

controlling temperature of the at least a narrow band emitter based on the primary reference intensity signal.

45. A method for measuring a concentration of at least a component gas as defined in claim 44 comprising:

controlling temperature of the at least a detector based on the primary reference intensity signal.

46. A method for measuring a concentration of at least a component gas as defined in claim 32 comprising:

transmitting electromagnetic radiation of one of the at least a predetermined narrow wavelength band through an interfering gas cell containing an interfering gas comprising an absorption band which is partially overlapping the one wavelength band;

emitting interfering gas reference electromagnetic radiation in a wavelength band outside absorption bands of the sample gas through the main absorption cell;

detecting the interfering gas reference electromagnetic radiation after passing through the main absorption cell and providing an interfering gas reference intensity signal in dependence thereupon; and

,

determining the concentration of the component gas corresponding to the one wavelength band in dependence upon the corresponding intensity signal and the interfering gas reference intensity signal.

47. A system for controlling composition of a heat treating atmosphere comprising:

a main absorption cell for containing the sample gas at a predetermined temperature and a predetermined pressure for measurement therein;

an inlet and an outlet in fluid communication with the main absorption cell, the inlet for being in fluid communication with a heat treating apparatus for receiving a sample gas representative of the heat treating atmosphere therefrom;

at least an electromagnetic radiation source for providing electromagnetic radiation in at least a predetermined narrow wavelength band, the predetermined narrow wavelength band being within a wavelength range of a predetermined absorption band of each of at least a component gas in the sample gas, the electromagnetic radiation for being transmitted through the main absorption cell;

a reflecting device disposed for reflecting the electromagnetic radiation after transmission through the main absorption cell such that the electromagnetic radiation is transmitted again therethrough;

at least a detector for detecting the electromagnetic radiation after the second transmission through the main absorption cell and for providing at least an intensity signal in dependence upon the concentration of the at least a component gas;

a processor in signal communication with the at least a detector for determining at least a heat treating potential in dependence upon data indicative of the at least an intensity signal and for providing a gas inflow control signal in dependence upon the at least a heat treating potential; and

,

a gas inflow control communication link for providing the gas inflow control signal to a gas inflow controller of the heat treating apparatus.

48. A system for controlling composition of a heat treating atmosphere as defined in claim 47 wherein the at least an electromagnetic radiation source comprises at least a narrow band emitter absent a filter.

49. A system for controlling composition of a heat treating atmosphere as defined in claim 48 comprising:

a hydrogen sensor communication link connected to the processor for receiving a hydrogen sensor signal indicative of a concentration of hydrogen in the heat treating atmosphere.

50. A system for controlling composition of a heat treating atmosphere as defined in claim 48 comprising:

a pressure control device in communication with at least one of the inlet and the outlet.

51. A system for controlling composition of a heat treating atmosphere as defined in claim 50 comprising:

a main absorption cell temperature control device covering at least a portion of an outside surface of the body of the main absorption cell.