Monitoring technology

• US 4,798,954 A
• Filed: 02/03/1987
• Issued: 01/17/1989
• Est. Priority Date: 02/03/1987
• Status: Expired due to Term

• Current Assignee: Foster-Miller Incorporated (Thermo Fisher Scientific Incorporated)
• Original Assignee: Foster-Miller Incorporated (Thermo Fisher Scientific Incorporated)
• Inventors: Stevenson, William A.
• Primary Examiner(s): Howell, Janice A.
• Assistant Examiner(s): Hannaher, Constantine
• Application Number:
  US07/010,306
• Time in Patent Office: 714 Days
• Field of Search: 250/341, 250/340, 250/339, 250/227, 350/96.29, 374/53, 374/131
• US Class Current: 250/341.7
• CPC Class Codes: G01N 2021/3595 using FTIR
• CPC Class Codes: G01N 2021/432 comprising optical fibres
• CPC Class Codes: G01N 21/552 Attenuated total reflection
• CPC Class Codes: G01N 2201/08 Optical fibres; light guides

Abstract

A process for infrared spectroscopic monitoring of insitu compositional changes in a polymeric material comprises the steps of providing an elongated infrared radiation transmitting fiber that has a transmission portion and a sensor portion, embedding the sensor portion in the polymeric material to be monitored, subjecting the polymeric material to a processing sequence, applying a beam of infrared radiation to the fiber for transmission through the transmitting portion to the sensor portion for modification as a function of properties of the polymeric material, monitoring the modified infrared radiation spectra as the polymeric material is being subjected to the processing sequence to obtain kinetic data on changes in the polymeric material during the processing sequence, and adjusting the processing sequence as a function of the kinetic data provided by the modified infrared radiation spectra information.

Claims

1. An infrared spectroscopy system for monitoring the processing of a polymeric material comprising

a source of infrared radiation for generating a beam of infrared radiation,

infrared spectrum analyzing means,

an infrared radiation transmission fiber that has a transmission portion and a sensor portion adapted to be embedded in the polymeric material to be monitored, and

means for coupling said transmission fiber to said source to transmit a beam of infrared radiation through said fiber to said sensor portion and for coupling said fiber to said infrared spectrum analyzing means for analyzing the resulting spectra as said polymeric material is processed to provide kinetic information on the processing of said polymeric material.

2. The system of claim 1 wherein said source is of the Michelson interferometer type.

3. The system of claim 1 wherein said spectrum analyzing means is of the Fourier transform type.

4. The system of claim 1 wherein the material of said fiber is selected from the class consisting of chalcogenide glass such as arsenic sulfide or arsenic germanium selenide, heavy metal fluoride glass, such a mixture of zirconium, barium, lanthanum and aluminum fluorides, and polycrystalline or single crystal materials such as thallium bromoiodide or cesium iodide.

5. The system of claim 1 wherein said sensor fiber has a diameter of at least about one hundred micrometers and a refractive index greater than 1.7.

6. The system of claim 1 wherein said sensor-transmitter fiber has a length of at least about two meters with a clad transmission portion and an unclad sensor portion, both of which are adapted to be embedded in the polymer material to be monitored.

7. The system of claim 6 wherein said fiber has a diameter of at least about one hundred micrometers, a refractive index greater than 1.7 and an overall transmission loss of less than 5 dB per meter over an 1800-750 wavenumber bandwidth and said sensor portion of said fiber has a length that is less than about five percent of the overall length of said fiber.

8. The system of claim 7 wherein the material of said fiber is selected from the class consisting of chalcogenide glass such as arsenic sulfide or arsenic germanium selenide, heavy metal fluoride glass, such as a mixture of zirconium, barium, lanthanum and aluminum fluorides, and polycrystalline or single crystal materials such as thallium bromoiodide or cesium iodide.

9. The system of claim 1 wherein said sensor-transmitter fiber has an overall transmission loss of less than 5 dB per meter over an 1800-750 wavenumber bandwidth.

10. A process for infrared spectroscopic monitoring of insitu compositional changes in a polymeric material comprising the steps of

providing an elongated infrared radiation transmitting fiber that has a transmission portion and a sensor portion,

embedding said sensor portion in the polymeric material to be monitored,

subjecting said polymeric material to a processing sequence,

applying a beam of infrared radiation to said fiber for transmission through said transmitting portion to said sensor portion for modification as a function of properties of the polymeric material, and

monitoring the modified infrared radiation spectra as said polymeric material is being subjected to said processing sequence to obtain kinetic data on changes in the polymeric material during the processing sequence.

11. The process of claim 10 and further including the step of adjusting the processing sequence as a function of the kinetic data provided by said modified infrared radiation spectra information.

12. The process of claim 10 wherein a polymer-fiber matrix is being monitored, said polymer-fiber matrix including alternating layers of fibers and polymer resins, and the sensor portions of a plurality of said infrared radiation transmitting fibers are embedded in spaced relation in said polymer resin layers.

13. The process of claim 12 wherein said polymeric material being monitored is selected from the class consisting of epoxies and polyimides.

14. The process of claim 13 wherein the material of said infrared radiation transmitting fibers is selected from the class consisting of chalcogenide glass such as arsenic sulfide or arsenic germanium selenide, heavy metal fluoride glass, such a mixture of zirconium, barium, lanthanum and aluminum fluorides, and polycrystalline or single crystal materials such as thallium bromoiodide or cesium iodide.

15. A elongated infrared radiation transmitting process monitoring fiber for use in the process of claim 10, said fiber having a transmission portion and a sensor portion, said fiber having a length of at least about one meter and said sensor portion having a length that is less than about five percent of the overall length of said fiber.

16. The fiber of claim 15 wherein said fiber has an overall transmission loss of less than 5 dB per meter over an 1800-750 wavenumber bandwidth, a diameter of at least about one hundred micrometers, a refractive index greater than 1.7, said sensor portion is unclad, and said transmission portion is clad.

17. The fiber of claim 16 wherein the material of said fiber is selected from the class consisting of chalcogenide glass such as arsenic sulfide or arsenic germanium selenide, heavy metal fluoride glass, such a mixture of zirconium, barium, lanthanum and aluminum fluorides, and polycrystalline or single crystal materials such as thallium bromoiodide or cesium iodide.

18. A system for insitu infrared spectroscopic monitoring of a polymer-fiber matrix to provide kinetic information during the curing of the polymeric constituent of said polymeric fiber matrix, said polymer-fiber matrix including alternating layers of fibers and polymer resins, comprising

a plurality of infrared radiation transmitting fibers, each said fiber having a transmission portion and a sensor portion, the sensor portions of said fibers being adapted to be embedded in spaced relation in said layers of polymer resin,

a source of infrared radiation for generating a beam of infrared radiation,

means for coupling said transmitting fibers to said source to transmit infrared radiation through said fibers to said sensor portions,

infrared spectrum analyzing means, and

means for coupling said fibers to said infrared spectrum analyzing means for analyzing the resulting infrared spectra as said polymer resin constituents are being cured to provide kinetic information on the curing of said polymer resins.

19. The system of claim 18 wherein each said infrared radiation transmitting fiber has a diameter of at least about one hundred micrometers and a length of at least about one meter, each said transmission portion is clad and each said sensor portion is unclad, each said sensor portion has a length that is less than about five percent of the overall length of its fiber.

20. The system of claim 19 wherein the material of said infrared radiation transmitting fibers is selected from the class consisting of chalcogenide glass such as arsenic sulfide or arsenic germanium selenide, heavy metal fluoride glass, such a mixture of zirconium, barium, lanthanum and aluminum fluorides, and polycrystalline or single crystal materials such as thallium bromoiodide or cesium iodide;

said polymer-fiber matrix includes fiber of material such as graphite or boron and polymers of materials such as epoxies or polyimides;

each said infrared radiation transmitting fiber has a refractory index greater than 1.7 and an overall transmission loss of less than 5 dB per meter over an 1800-750 wavenumber bandwidth; and

further including autoclave type containment structure for receiving said polymer-fiber matrix during cure, said containment structure including gland structure through said transmission portions of said fibers are connected to said infrared radiation source and said infrared spectrum analyzer means.