Patent Publication Number: US-7723685-B2

Title: Monitoring system comprising infrared thermopile detector

Description:
CROSS REFERENCE TO RELATED APPLICATIONS 
   This is a continuation of U.S. patent application Ser. No. 11/555,094 filed on Oct. 31, 2006, and subsequently issued as U.S. Pat. No. 7,351,976 on Apr. 1, 2008, which is a continuation of U.S. patent application Ser. No. 10/668,489 filed on Sep. 23, 2003 and subsequently issued as U.S. Pat. No. 7,129,519, which is a continuation-in-part of U.S. patent application Ser. No. 10/623,244 filed on Jul. 18, 2003 and subsequently issued as U.S. Pat. No. 7,011,614, which is a divisional of U.S. patent application Ser No. 10/140,848 filed on May 8, 2002 and subsequently issued as U.S. Pat. No. 6,617,175. Each of the foregoing patents and patent applications is hereby incorporated by reference as if set forth fully herein. 

   FIELD OF THE INVENTION 
   This invention relates to infrared thermopile monitoring systems for semiconductor process monitoring and control. 
   DESCRIPTION OF THE RELATED ART 
   Most infrared energy-absorbing molecules absorb infrared radiation at discrete energy levels, so that when a gas, liquid or solid composition is exposed to infrared (IR) radiation of a broad wavelength range, the infrared energy-absorbing component(s) of that composition will absorb a portion of the IR light at very specific wavelengths. This phenomenon enables infrared-based detection, by comparing energy spectra of various known compositions with and without specific IR-absorbing component(s), to obtain an absorption profile or pattern that can be used to detect the presence of specific IR-absorbing component(s) in an unknown composition. Additionally, the concentration of the IR-absorbing component(s) in the composition directly correlates to the amount of IR light that is absorbed by such component(s), and can be determined based thereon. 
   Conventional IR gas analyzers depend on grating techniques or prisms to break IR radiation into its individual wavelengths (see  FIGS. 1A and 1B , showing split IR lights of wavelength λ 1  and λ 2 ). The IR radiation of individual wavelengths would then be introduced into a gas cell by means of a moveable slit aperture and the IR radiation of the selected wavelength passing through the gas cell would be detected. Such dispersive IR analyzers used electronic processing means to correlate the slit aperture position with the IR energy level and the signal from the detector, and produce energy versus absorbance relations. 
   The principal drawbacks of the above-described dispersive spectrometers are the loss of radiation intensity due to multiple reflection and refraction, the risk of total system failure due to misalignment of the movable parts, the cost and complexity of the spectrometer apparatus due to the number of optical components (e.g., mirrors, lens, and prism), and the space requirement for accommodating the numerous optical components used. 
   Fourier transform IR (FT-IR) spectrometers, like dispersive spectrometers, also use broad energy IR sources. The originally generated IR beam is split into two beams and an interference pattern is created by sending one of the two beams in and out-of-phase, using a movable mirror. A laser beam is used to monitor the location of the movable mirror at all times. After the dual beam is sent to a sample, a sensor component of the spectrometer device receives the convoluted infrared wave pattern together with the laser-positioning beam. That information is then sent to a computer and deconvoluted using a Fourier transform algorithm. The energy versus mirror displacement data is thereby converted into energy versus absorbance relationships. Such FT-IR spectrometers suffer from similar drawbacks as described hereinabove for the conventional dispersive spectrometers. 
   It is therefore an object of the present invention to provide an IR photometer system that minimizes the loss of radiation intensity during transmission of the IR radiation. 
   It is another object of the present invention to provide an IR photometer system that is simple and robust, which is less vulnerable to misalignment. 
   It is still another object of the present invention to provide a scrubber system for abating semiconductor process effluent, which is capable of analyzing composition of the incoming effluent and responsively modifying the operational mode accordingly. 
   Other objects and advantages of the invention will be more fully apparent from the ensuing disclosure and appended claims. 
   SUMMARY OF THE INVENTION 
   In one aspect, the present invention relates to a system for treatment of an effluent material, said system comprising: an inlet conduit arranged to receive the effluent material from an upstream processing unit; a sampling region for the effluent material in flow communication with the inlet conduit, the sampling region defining a radiation transmission path; an infrared radiation source constructed and arranged to emit infrared radiation into the sampling region; and a thermopile detector constructed and arranged to receive at least a portion of the infrared radiation following passage thereof through the sampling region, and arranged to responsively generate an output signal correlative of at least one of (i) effluent material composition and (ii) concentration of an abatable component of the effluent material within the sampling region; and a control element arranged to receive the output signal from the thermopile detector and arranged to adjust an effluent treatment media flow based on the received output signal to maintain effluent material and/or abatable component discharge below a predetermined level. 
   In another aspect, the present invention relates to a method of generating an output signal indicative of presence or concentration of a desired component of a material, said method comprising emitting infrared radiation generated by an infrared radiation source into a sampling region defining a radiation transmission path and a material flow path, receiving at least a portion of said emitted infrared radiation with a thermopile detector, generating the output signal from said thermopile detector indicative of the presence or concentration of the desired component of said material in the sampling region, wherein the method is further characterized by any of the following: (a) flowing a gas through at least one gas introduction element between the infrared radiation source and the thermopile detector; (b) transmitting the infrared radiation along a transmission path that comprises an inner surface characterized by a roughness in a range of from about 0.012 μm Ra to about 1.80 μm Ra; and (c) heating at least a portion of said radiation transmission path with a heating element that is distinct from the infrared radiation source. 
   In one embodiment, infrared (IR) radiation in a system according to the present invention is transmitted along a transmission path that is substantially linear, while both the infrared radiation source and the thermopile detector are aligned along the transmission path of said infrared radiation. The linear transmission path for the IR radiation minimizes reflection and refraction of such IR radiation and therefore significantly reduces loss of radiation intensity during transmission. Such linear transmission path is made available by the integration of the thermopile detector, which comprises one or more radiation filters for selectively transmitting the IR radiation of a specific wavelength, therefore eliminating the requirements for monochromating the IR radiation through splitting and grating that are essential to the conventional dispersive and FT-IR spectrometers. 
   The loss of IR radiation intensity can also be reduced, either independent from or in addition to the use of linear transmission path, by providing a transmission path with inner surface that is sufficient smooth and/or reflective, which minimizes absorption and dissipation of the IR radiation by such inner surface of the transmission path. Specifically, such inner surface of the transmission path is characterized by a roughness in a range of from about 0.012 μm Ra to about 1.80 μm Ra, preferably from about 0.10 μm Ra to about 0.80 μm Ra, and more preferably from about 0.10 μm Ra to about 0.20 μm Ra. Such inner surface may further be characterized by a reflectivity in a range of from about 70% to about 99%, preferably from about 92% to about 97%. 
   “Ra” as used herein refers to the average differences between peaks and valleys of a surface finish. 
   When the material is subjected to IR radiation in the sampling region is a process gas, such material may comprise particles or be susceptible to particle formation, resulting in deposition of particles around the IR radiation source or the thermopile detector, which may in turn significantly reduce the amount of IR radiation transmitted therethrough or completely block the transmission path. 
   Various embodiments of the present invention can be arranged and constructed to utilize a purge gas for purging the interfacial spaces between the sampling region containing the process gas and the IR radiation source as well as between the sampling region and the thermopile detector. Such purge gas can be passed through porous media into the interfacial spaces, to form a purge gas flow that moves any particle deposits away from the IR radiation source and the thermopile detector into the sampling region. Alternatively, particle deposit may be reduced by providing external thermal energy for heating at least a portion of the IR transmission path, so as to create a thermal gradient or heat flux that hinders the particle access to the internal surface of the transmission path. 
   A semiconductor process system according to one embodiment of the present invention may comprise a scrubber unit for abating a semiconductor process effluent from an upstream process unit, with a sampling region arranged near the inlet of such scrubber unit, so as to enable analysis of the effluent before its entry into such the scrubber unit, thereby enabling the scrubber unit to be responsively operated according the composition of the process gas. 
   Other aspects, features and embodiments of the invention will be more fully apparent from the ensuing disclosure and appended claims. 

   
     BRIEF DESCRIPTION OF THE DRAWINGS 
       FIGS. 1A and 1B  show conventional monochromator systems for splitting and grating IR radiation. 
       FIG. 2  is a schematic view of a semiconductor process system comprising a linear transmission path for IR radiation, according to one embodiment of the present invention. 
       FIG. 3  is a schematic view of a semiconductor process system comprising a scrubber unit having an IR radiation source and a thermopile detector constructed and arranged for analyzing an incoming process effluent near the inlet of such scrubber unit, according to one embodiment of the present invention. 
       FIG. 4  is a time-concentration plot of tetraethyloxysilane (TEOS) and silicon tetrafluoride (SiF 4 ) as measured for the process effluent from an upstream plasma enhanced chemical vapor deposition chamber that is operated according to alternative deposition and cleaning cycles. 
       FIG. 5  is a graph showing the IR signal responses measured for a first transmission path having non-electropolished inner surface, a second transmission path having moderately electropolished inner surface, and a third transmission path having highly electropolished inner surface, at various IR wavelengths. 
       FIGS. 6 and 7  are perspective views of semiconductor process systems comprising purge gas inlets for introducing a purge gas to remove particles from the interfacial spaces between the sampling region and the IR source as well as between the sampling region and the thermopile detector. 
       FIG. 8  is a perspective view of semiconductor process system comprising purge gas inlets for forming a sheath of purge gas around the particle-containing process effluent in the sampling region. 
   

   DETAILED DESCRIPTION OF THE INVENTION, AND PREFERRED EMBODIMENTS THEREOF 
   The present invention provides infrared thermopile detector systems useful for semiconductor process monitoring and control. U.S. patent application Ser. No. 10/140,848 filed on May 8, 2002 in the name of Jose I. Arno, and issued as U.S. Pat. No. 6,617,175 on Sep. 9, 2003, is incorporated herein by reference in its entirety for all purposes. 
   As used herein, the term “semiconductor process” is intended to be broadly construed to include any and all processing and unit operations involved in the manufacture of semiconductor products, as well as all operations involving treatment or processing of materials used in or produced by a semiconductor manufacturing facility, as well as all operations carried out in connection with the semiconductor manufacturing facility not involving active manufacturing (examples include conditioning of process equipment, purging of chemical delivery lines in preparation for operation, etch cleaning of process tool chambers, abatement of toxic or hazardous gases from effluents produced by the semiconductor manufacturing facility, etc.). 
   The thermopile-based infrared monitoring system of the invention comprises an infrared (IR) radiation source, a sampling region for exposing a material of interest (e.g., a process gas) to IR radiation, and a thermopile detector for analyzing the IR radiation as transmitted through the material of interest. The sampling region in the broad practice of the invention may comprise any suitable compartment, passageway or chamber, in which the material to be analyzed is subjected to passage of IR light therethrough for the purpose of using its IR absorbance-determined output to generate control signal(s) for process monitoring and control. The thermopile detector generates small voltages when exposed to IR light (or heat in the IR spectral regime). The output signal of the thermopile detector is proportional to the incident radiation on the detector. 
   Thermopile detectors employed in the preferred practice of the present invention may have a multiple array of elements in each detector unit. For instance, in a dual element detector, one of the thermopile detector elements is used as a reference, sensing IR light in a range in which substantially no absorption occurs (e.g., wavelength of 4.00±0.02 μm). The second thermopile detector element is coated with a filter that senses IR energy in the spectral range of interest (such spectral range depending on the particular material to be monitored). Comparison of the differences in the voltages generated by the reference thermopile detector element and those generated by the thermopile detector active element(s) provides a concentration measurement. Detectors with up to 4 thermopile detector element arrays are commercially available. For example, in a 4-element detector unit, one detector element is employed as a reference and the remaining 3 detector elements are utilized for measurements in different spectral regions. 
   While the ensuing disclosure is directed to a process gas as the material being subjected to IR radiation, it will be recognized that the invention is applicable to a wide variety of materials, e.g., solids, fluids (liquids and gases), multiphase materials, multicomponent materials, supercritical media, etc. 
   The total loss of the IR radiation intensity (referred to herein as L Total ) is determined by both the loss of IR radiation intensity caused by transmission thereof (i.e., absorption by the transmission path and the optical components, referred to herein as L Path ) and the loss of IR radiation intensity due to absorption by the IR-absorbing material of interest (referred to herein as L Material ), according to the following equations:
 
 L   Total   =L   Path   +L   Material  
 
   The thermopile IR detector has a minimum requirement for the IR radiation intensity, in order to effectively detect such IR radiation. Therefore, when the intensity of the IR radiation generated by the IR source remains constant, the L Total  has to be maintained at a level that is equal to or smaller than a maximum limit L 0  in order to enable detection of the IR radiation by the thermopile IR detector. On the other hand, since the concentration of the IR-absorbing material of interest directly correlates to and is determined by L Material , maximization of L Material  will maximize the signal strength of the measurement, which is especially important for detection and analysis of low concentration IR-absorbing materials. 
   The present invention achieves the goal of maximizing L Material  while maintaining L Total  at or below a maximum limit L 0 , by reducing or minimizing L Path , according to the following methods: 
   When the IR radiation is transmitted through a substantially linear transmission path from the IR source to the thermopile detector, with minimum amount of reflection and refraction therebetween, the loss of radiation intensity is effectively reduced in comparison to that of a non-linear transmission path that requires multiple reflections and refractions of the IR radiation, as shown in  FIGS. 1A and 1B . 
   Therefore, the present invention constructs and arranges the IR radiation source, the sampling region, and the thermopile detector to provide a substantially linear transmission path for the IR light, as shown in  FIG. 2 . 
   Specifically, the system  1  comprises a sampling region  10 , preferably a gas sampling region having a gas inlet  12  and a gas outlet  14  and constitutes a part of a flow circuitry for flow of a process gas therethrough. 
   The IR radiation source  20  is positioned at one side of such gas sampling region  10 . Specifically, the IR radiation source  20  comprises an IR emitter  22  and a parabolic mirror  24 , for providing a parallel beam of IR light  2 , which is transmitted along a substantially linear transmission path through the gas sampling region  10 . 
   The thermopile detector  40  is positioned at the other side of such gas sampling region  10  for receiving and analyzing the transmitted IR light beam. The thermopile detector  40  comprises an IR detecting element  44  having one or more IR radiation band pass filters for selectively transmitting a portion of the IR radiation of a narrow wavelength range that encompasses the absorption wavelength that is characteristic to the IR-absorbing component(s) of interest in the process gas, so that the decrease in output signal generated by such thermopile is directly related to the amount of infrared absorption by the corresponding component(s) of interest. Preferably but not necessarily, the IR light beam is focused by a focusing lens  42  before entering the IR detecting element  44 . The thermopile detector unit as mentioned may further include a multiplicity of absorber areas, including reference (unfiltered) absorber and gas-filtered absorber regions, with the latter filters being gas-specific for sensing of the semiconductor gases or gas components of interest (e.g., arsine, phosphine, germane, stibine, distibine, silane, substituted silanes, chlorine, bromine, organometallic precursor vapor, etc.). 
   The gas sampling region  10  is separated from the IR radiation source  20  and the thermopile detector  40  by interfacial spaces  32  and  52 , which form parts of the IR transmission path. Preferably, the interfacial space  32  is connected to the IR radiation source  20  in a sealed manner, which comprises a weld connector  34  that is detachably and sealingly connected to the IR radiation source by a spacer  35  and O-rings  36 . Similarly, the interfacial space  52  is connected to the thermopile detector  40  in a sealed manner, which comprises a weld connector  54  that is detachably and sealingly connected to the IR radiation source by a spacer  55  and O-rings  56 . Such weld connector  34  and  54  both comprise IR transparent materials and therefore form a portion of the IR transmission path. 
   The linear transmission path of the IR radiation reduces unnecessary loss of radiation intensity. In addition, connection between the IR source, the gas sampling region, and the thermopile detector is simple and robust, providing a sufficient small footprint and efficient resistance against misalignment. 
   Further, an integrated circuit board  62  may be positioned behind the thermopile detector  40 , for immediately receiving output signals from the thermopile detector  40 , so as to further reduce the footprint and minimize signal loss due to remote connections. 
   In one illustrative embodiment of the invention, the thermopile detector system is utilized as an abatement tool controller for an abatement unit for treating process effluent produced in a semiconductor manufacturing operation, or other industrial process. For such purpose, the thermopile detector system advantageously is installed at the inlet of the abatement unit, where the abatement apparatus receives the effluent to be treated. In such service, the thermopile detector system is used to sense whether or not an upstream tool that generates the effluent in active on-stream operation, is in an active operating mode, or alternatively whether or not the upstream tool is in a non-effluent-producing state, e.g., undergoing purging or cleaning. The thermopile detector unit, by way of specific example, is usefully employed as an abatement tool controller for an effluent scrubber, such as a wet/dry scrubber or a thermal scrubber, whereby the presence of the thermopile detector system transforms the scrubber into a “smart” scrubber and enhances the efficiency of the scrubber, allowing conservation of resources (lower consumables) to be achieved. 
     FIG. 3  shows a semiconductor process system  100  comprising a scrubber unit  140  having a gas inlet  142  and a gas outlet  144 . An IR source  120  and a thermopile detector  130  are provided at both sides of a gas sampling region  110  near the gas inlet  142  of such scrubber unit  140 , for analyzing the composition of the effluent flowed into the scrubber. The output signal generated by the thermopile detector  130  is forwarded through transmission line  152  to a microcontroller  150 . The microcontroller  150  is connected to the scrubbing medium sources  160  and responsively adjusts the amount of scrubbing media (preferably fuel, water, and chemical additives)  162 ,  164 , and  166  input according to the composition of the effluent as measured. 
   Various abatable components in the effluent, including but not limited to, tetraethyloxysilane, silane, silicon tetrafluoride, silicon-containing organic compounds, boranes, arsenic hydride, phosphine, hydrogen fluoride, fluorine, tungsten hexafluoride, hydrogen chloride, chlorine, titanium tetrachloride, perfluorocarbons, nitrous oxide, ammonium, hydrogen, oxygen, argon, and helium, may be analyzed by the thermopile detector system of the present invention. Additional sensors, such as temperature sensors, flow sensors, pressure transducers, ultraviolet spectrometers, mass spectrometers, and electrochemical sensors, may be provided for further measuring the flow rate, gas composition and concentration, pressure, and temperature of the effluent, so as to allow corresponding adjustment of the operational mode of the scrubber unit. 
   The IR thermopile detector system of the present invention may be used to analyze the effluent gas species emitted from a plasma enhanced chemical vapor deposition (PECVD) chamber, in which SiO 2  films are deposited using tetraethyloxysilane (TEOS) and which performs chamber cleaning by using SiF 4  after each deposition cycle. Therefore, during the deposition cycles, the IR detector system measures the real-time concentration of TEOS in the deposition effluent. During alternating cleaning cycles, the IR detector system measures the SiF 4  concentration. Measurements obtained by the IR detector system during the alternating deposition/cleaning cycles are provided in  FIG. 4 . The information collected by the IR photometer can be used to adjust the settings of the downstream scrubber unit for abatement of TEOS and SiF 4 . 
   For further reduce the IR radiation loss (L Path ) during the transmission, a transmission path with a smooth, reflective inner face is provided, which minimize the absorption and dissipation of IR radiation by the surface of such transmission path. 
   When such smooth, reflective transmission path is provided, longer path length can be provided for maximizing the absorption of IR radiation by the IR-absorbing components of interest (i.e., L Gas ), which is especially important for effectively measuring low concentration IR-absorbing components. 
   Preferably, such inner surface of the transmission path is characterized by a roughness in a range of from about 0.012 μm Ra to about 1.80 μm Ra, more preferably from about 0.10 μm Ra to about 0.80 μm Ra, and most preferably from about 0.10 μm Ra to about 0.20 μm Ra. Such inner surface may further be characterized by a reflectivity in a range of from about 70% to about 99%, preferably from about 92% to about 97%. Such smooth, reflective inner surface may be provided by electropolishing or super polishing techniques. 
     FIG. 5  shows the IR signal responses measured for a first transmission path having non-electropolished inner surface, a second transmission path having moderately electropolished inner surface, and a third transmission path having highly electropolished inner surface, at various IR wavelengths (Channel 2=3.88 μm, Channel 4=4.65 μm, and Channel 5=4.2 μm). The path length for each transmission path is the same, and the same IR source and thermopile detector are used. The measurement results indicate that the highly polished transmission path provides much stronger signal strength than that of the moderately polished and non-polished transmission paths. 
   Process gas that contains particles or is susceptible to particles formation may form particle deposits along the transmission path of the IR radiation, which will absorb the IR radiation and significantly reduces the radiation intensity of the IR radiation transmitted. 
   The present invention therefore provides a purge gas near the interfacial spaces between the gas sampling region and the IR source as well as between the gas sampling region and the thermopile detector. The purge gas flow provides a sufficient force to remove the particle deposits away from the IR source and the thermopile detector, so as to prevent such particles from interfering with the detection process. 
     FIG. 6  shows a gas sampling region  210  having an inlet  212  and an outlet  214  for flowing a particle-containing process gas  202  therethrough. An IR source  220  is positioned at one side of such gas sampling region  210  and is isolated therefrom by an interfacial space  232 , while a thermopile detector  240  is positioned at the other side of such gas sampling region  210  and is isolated therefrom by an interfacial space  252 . A purge gas  262  is introduced into such interfacial spaces  232  and  252  from a purge gas source (not shown), preferably through a porous media  264 , for forming a uniform flow of purge gas that moves away from the IR source  220  and the thermopile detector  240  toward the gas sampling region  210 . Such flow of purge gas further generates vacuum at the dead-end spaces near the IR source  220  and the thermopile detector  240 , so as to force the particle deposits out of such dead-end spaces and discharge same into the process gas flow in the gas sampling region  210 . 
   The purge gas may be introduced into the interfacial spaces  232  and  252  along a direction that is substantially parallel to the process gas flow, as shown in  FIG. 6 , which then flows through such interfacial spaces into the gas sampling region  210  in a direction that is substantially perpendicular to the process gas flow. 
     FIG. 7  shows an alternative embodiment of the present invention, in which the purge gas is introduced into the interfacial spaces  332  and  352  in a direction that is substantially perpendicular to the process gas flow and flows through such interfacial spaces along the same direction into to the gas sampling region  210 . 
   Further, the purge gas may be provided to form a gas sheath surrounding the process gas flow, so as to prevent particles from escaping from the gas sampling region. Specifically,  FIG. 8  shows a purge gas  362  that forms an annular sheath  466  around the particle-containing process gas flow. Such purge gas is flowed in a direction that is confluent with the process gas flow and is therefore discharged of the gas sampling region  410  together with the process gas. 
   Alternatively, external heating devices can be provided for heating at least a portion of the IR transmission path (including the IR transmission windows), so as to generate a thermal gradient or heat flux, which functions to prevent the particles from accessing and depositing on the internal surface of the IR transmission path. 
   Although the invention has been variously disclosed herein with reference to illustrative embodiments and features, it will be appreciated that the embodiments and features described hereinabove are not intended to limit the invention, and that other variations, modifications and other embodiments will suggest themselves to those of ordinary skill in the art. The invention therefore is to be broadly construed, consistent with the claims hereafter set forth.