Infrared spectrophotometer accelerated corrosion-erosion analysis system

• US 5,793,042 A
• Filed: 09/30/1996
• Issued: 08/11/1998
• Est. Priority Date: 09/30/1996
• Status: Expired due to Fees

• Current Assignee: Quick, Nathaniel R.
• Original Assignee: Quick, Nathaniel R.
• Inventors: Quick, Nathaniel R.
• Primary Examiner(s): Tokar, Michael J.
• Assistant Examiner(s): HANIG, RICHARD E
• Application Number:
  US08/721,747
• Time in Patent Office: 680 Days
• Field of Search: 250/339.08, 250/339.07, 250/339.06, 250/341.1, 250/341.6, 356/346, 356/244
• US Class Current: 250/339.08
• CPC Class Codes: G01J 3/453 by correlation of the amplitudes

Abstract

A preferred embedment of the system and a method are provided utilizing Fourier Transform Infrared Spectrophotometer (FITR) for examination and analysis of materials on a real-time basis in a chamber at elevated temperatures with corrosive-erosive gaseous environments that cause accelerated material deterioration. The apparatus is capable on a real-time basis of examining and analyzing a wide variety of materials subjected to accelerated deterioration events missed by prior art systems and methods. Empirical data of accelerated corrosion-erosion events are also acquired and stored for subsequent computer analysis of recorded absorbed and reflected vibrational frequencies detected. The system utilizes preselected adjustable grazing angles of an incident beam of the infrared beam impinging upon a material sample during the observation and analysis processes to enhance the data to be collected. The system provides feed back laser signals for alignment adjustment for the selectable grazing angles.

Claims

1. A method for monitoring and analyzing in real-time the corrosive-erosive effects on materials introduced into a chamber at elevated temperatures in the presence of hostile gaseous atmosphere to simulate the accelerated life and deterioration of the materials for life assessment studies, the method comprising the steps of:

a. providing a fourier transform infrared spectrophotometer and laser control system for generating and transmitting infrared and laser beams to a chamber, for systematized collection and processing of detected infrared spectrum data and laser feed-back signals, and further for transmission of the systematized infrared spectrum data to acquisition, storage and monitoring systems;

b. providing acquisition, storage and monitoring devices that examine and analyze detected infrared spectra data on a continuous real-time basis indicative of the accelerated life effects on said material sample within said chamber and still utilized for after-test analysis of recorded and stored infrared spectra data;

c. providing a chamber equipped with an input environmentally resistant window for transmission of a infrared light and laser light beam into the chamber and an output environmentally resistant window for transmission of exiting infrared and laser light, the chamber being further equipped with an input port and valve and an output port and valve for introducing gases into the chamber and the removal therefrom, respectively, the chamber still further being equipped for receiving a material sample support platform, a material sample and energizing electrical power to said support platform;

d. providing a material sample as the target for receiving continuous impinging incident infrared and laser beams thereby producing exiting reflecting infrared beam spectra data from said material sample indicative of surface and sub-surface conditions and other material species thereof on the an ongoing and real-time basis;

e. supplying one or more gases from gas sources to the input port of said chamber, and drawing a vacuum or removal of said gases with a vacuum or removal device through the output port of said chamber;

f. supplying energizing electrical power to said sample support platform having an environmentally resistant electrical element incorporated therein for providing elevated temperatures to said chamber and material sample, providing electrical means for angular orientational adjustment of the material sample support platform along the path of the said infrared and laser beams;

g. providing a first moveable transmission mirror between said fourier transform infrared spectrometer control system and said chamber and a second moveable transmission mirror on said output window side of said chamber, both moveable mirrors being disposed along the paths of infrared and laser beams, further providing a first and second fixed transmission and reflective mirrors beyond said second moveable transmission mirror along the path of the infrared and laser beams, still further providing a detector device disposed in spaced apart relationship to said second fixed transmission and reflective mirror for receiving reflected infrared and laser signals to said fourier transform infrared spectrometer control system for systematization data collection and processing;

h. illuminating said test sample within said chamber through said input transmission window with a dispersed infrared light and laser light beam, said beams passing through said first moveable mirror enroute to said chamber for impinging upon said test sample at selected grazing angles, said light beams thereafter being reflected therefrom and exited from said chamber through said output transmission window and thence through said second moveable mirror, and said first and second fixed mirrors to said detector device;

i. providing an infrared and laser sensitive detector device along the path of said infrared and laser beams useful with said fourier infrared transform spectrophotometer control system for detecting the exiting infrared light spectra of repetitive incidents of infrared light beam impinging upon the surface of said material sample and exited through the output beam transmission port of said chamber and providing a spectrum indication of the presence and extent of corrosive-erosive deterioration effects at the surfaces and sub-surfaces of said material sample and other surface species that may occurred thereon;

j. detecting and analyzing the exited infrared beam on a real-time basis providing an indication of the presence and extent of corrosive-erosive effects upon the surface and sub-surface of said test sample as a result of exposure to elevated temperature and gaseous environment within said chamber and

k. further providing laser means for processing feed-back laser signals for alignment adjustment of infrared transmission mirrors to selectable grazing angles for said impinging infrared beam as it strikes a target sample.

2. Method of claim 1, in which said characterization of the presence of chemical species upon a surface of said material sample after exposure to said broadband infrared light beam at elevated temperatures is identified by a wavenumber cm^-1.

3. An apparatus for monitoring and analyzing in real-time the corrosive-erosive status and effects on and the extent of change in the surface conditions and species of a material introduced into a chamber that is subjected to an impinging broadband frequency infrared light beam at elevated temperatures in the presence of hostile gaseous atmosphere in the chamber to simulate the accelerated life and deterioration thereof, the combination comprising:

a. a fourier transform infrared control system for providing and outputting continuous broadband infrared and laser light beams, utilized to impinge upon material samples under test and measurement, and collecting and systematizing detected reflected and absorbed infrared and laser light signals for examination and analysis;

b. a chamber having an X and Y axis and being disposed in spaced apart relationship to said fourier transform control system to receive the infrared and laser light beams outputted therefrom, and being equipped with an environmentally resistant input and output window for receiving incident infrared and laser light beams and for exiting reflected components thereof, respectively, and further being equipped with an input and output gas port, and still further being equipped and adapted for receiving and supporting a material sample, the surface which is to be the examined and spectroscopically analyzed for the presence and extent of chemical species and changes in the physical and chemical conditions thereof, and said material sample being disposed within said chamber to receive incoming infrared and laser light beams at selected incident grazing angles with respect to the X-axis of said chamber;

c. a pair of adjustable mirrors, a first mirror being disposed in spaced apart relationship between said fourier transform infrared control system and said chamber and a second mirror being disposed in spaced apart relationship to said output window of the chamber along a path of said exiting light beams, said pair of mirrors being equipped and adapted for separate monitoring and adjustment to achieve and maintain control of the path of the infrared and laser light beams into and out of the chamber;

d. a light detection and measuring means for receiving infrared and laser light exited through the output window of the chamber and generating signals proportional to the detected light and providing an indication of the surface condition of a material sample subjected to said infrared light beam;

e. a pair of fixed mirrors disposed in space apart relationship with said second adjustable mirror along said infrared light beam after passing therethrough, said second fixed mirror also being disposed in spaced apart relationship to said light detection means for transmitting reflected infrared and laser light thereto;

f. an analyzer system connected to said fourier transform control system for receiving collected and systematized signals for analyzing signals proportional to the detected light and providing and indication of the presence of chemical species present upon the material sample and of the changes in the material sample due to corrosive-erosive effects;

g. a gas source connected to the input port of said chamber and a gas removal source connected to the output port of said chamber to cause the measurement of the material sample to occur in a selected hostile gaseous environment;

h. an electrical heat source connected to a material support platform disposed within said chamber to cause the measurement of the material sample to occur at selected elevated temperatures; and

i. a laser means for processing feed-back laser signals for alignment adjustment of infrared transmission mirrors to selectable grazing angles for said impinging infrared beam as it strikes a target sample.

4. An apparatus for monitoring and analyzing in real-time the corrosive-erosive status and effects on and the extent of change in the surface conditions and species of a material introduced into a chamber that is subjected to an impinging broadband frequency infrared light beam at elevated temperatures in the presence of hostile gaseous/vapor, atmosphere in the chamber to simulate the accelerated life and deterioration thereof, the combination comprising:

a. a fourier transform infrared control system for providing and outputting continuous broadband infrared light beam, utilized to impinge upon material samples under test and measurement, and collecting and systematizing detected reflected and absorbed infrared light signals for examination and analysis;

b. a chamber having a Y-axis and being disposed in spaced apart relationship to said fourier transform control system to receive the infrared light beam outputted therefrom, and being equipped with an environmentally resistant combination input and output window for receiving incident infrared light beam and for existing reflected components thereof, and further being equipped with means for receiving and supporting a material sample, for examination and spectroscopic analysis for the presence and extent of chemical species and changes in the physical and chemical conditions thereof, and said material sample being disposed within said chamber to receive incoming infrared light beam at selected incident angles with respect to the Y-axis of said chamber;

c. a light detection and measuring means for receiving reflected infrared light exited through said output window of the chamber and generating signals proportional to the detected light and providing an indication of the surface condition of a material sample subjected to said infrared light beam;

d. an analyzer system connected to said fourier transform control system for receiving collected and systematized signals for analyzing signals proportional to the detected light and providing an indication of the presence of chemical species present upon the material sample and of the changes in the material sample due to corrosive-erosive effects;

e. a gas source connected to said chamber and a gas removal source connected to said chamber to provide a selected hostile gaseous environment therein; and

f. an electrical heat source connected to a material support platform disposed within said chamber to provide a selected elevated temperatures therein.

5. An apparatus of claim 4, in which said characterization of the presence of chemical species upon a surface of said material sample after exposure to said broadband infrared light beam at elevated temperatures is identified by a wavenumber cm^-1.

6. A method for monitoring and analyzing in real-time the corrosive-erosive status and effects on and the extent of change in the surface conditions and species of a material introduced into a chamber that is subjected to an impinging broadband frequency infrared light beam at elevated temperatures in the presence of hostile gaseous atmosphere in the chamber to simulate the accelerated life and deterioration thereof, the method comprising the step of:

a. providing a fourier transform infrared control system for generating and outputting a continuous broadband infrared light beam, utilized to impinge upon material samples under test and measurement, and collecting and systematizing detected reflected and absorbed infrared light signals for examination and analysis;

b. providing a chamber having an Y-axis to receive continuous broadband infrared light beams from said fourier transform control system transmitted through an environmentally resistant combination input and output window of said chamber for transmitting therethrough incident infrared light beam and for exiting therethrough reflected components thereof, and further providing means for receiving and supporting a material sample therein for exposure to said incident infrared light beam at selected incident angles with respect to the Y-axis of said chamber for examination and spectroscopic analysis for the presence and extent of chemical species and changes in the physical and chemical conditions thereof;

c. providing an infrared light beam detection and measuring means for receiving reflected infrared light beam exited through said output window of said chamber and generating signals proportional to the detected light beam so as to provide data indicating the surface condition of said material sample subjected to said infrared light beam;

d. providing an analyzer system connected to said fourier transform control system for receiving collected and systematized reflected infrared signals from said material sample to provide data, analysis and characterization of the presence of chemical species present upon said material sample and of the changes in said material sample due to corrosive-erosive effects;

e. providing a gas source and a gas removal device connected to said chamber to provide a selected hostile gaseous environment therein; and

f. proving an electrical heat source connected to a material sample support platform disposed within said chamber to provide a selected elevated temperatures therein.

7. Method of claim 6, in which said characterization of the presence of chemical species upon a surface of said material sample after exposure to said broadband infrared light beam at elevated temperatures is identified by a wavenumber cm^-1.

8. Method of claim 6, in which said characterization of the presence of chemical species upon a surface of said material sample after exposure to said broadband infrared light beam at elevated temperatures is identified by a wavenumber cm^-1.