Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/32—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by electrical effects other than those provided for in group B01D61/00
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B08—CLEANING
  • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
  • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
  • B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
  • C30B25/02—Epitaxial-layer growth
  • C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
  • C30B29/02—Elements
  • C30B29/06—Silicon
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
  • H01J37/32357—Generation remote from the workpiece, e.g. down-stream
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/32431—Constructional details of the reactor
  • H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
  • H01J37/32816—Pressure
  • H01J37/32834—Exhausting
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/32917—Plasma diagnostics
  • H01J37/32935—Monitoring and controlling tubes by information coming from the object and/or discharge
  • H01J37/32963—End-point detection
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
  • B01D2259/818—Employing electrical discharges or the generation of a plasma
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/32—Processing objects by plasma generation
  • H01J2237/33—Processing objects by plasma generation characterised by the type of processing
  • H01J2237/335—Cleaning

Definitions

• aspects of the present disclosure generally relate to a methods and apparatuses for cleaning exhaust systems, such as exhaust systems used with process chambers for the formation of epitaxial silicon.
• Epitaxial silicon is deposited in process chambers using silicon- containing precursor gases. After a predetermined number of deposition cycles in the process chamber, the process chamber is cleaned using a chlorine-containing gas. Chloride radicals from the chlorine-containing gas react with silicon to form chlorosilane, which is exhausted from the process chamber.
• the chlorosilane is a flammable material which deposits on internal surfaces of the exhaust system, and must be periodically removed. Cleaning times to remove the chlorosilane can range from half a day to up to a month, depending on the extent of removal required. Additionally, the chlorosilane may react with oxygen in the ambient environment upon disassembly of the exhaust system, thus forming chlorosiloxane, which is a contact explosive. The formation of chlorosiloxane further extends the time required for cleaning and maintenance due to the extra precautions which are taken by personnel.
• a processing system comprises a process chamber; and an exhaust system coupled to the process chamber.
• the exhaust system comprises a remote plasma source for supplying an ionized cleaning gas to the exhaust system downstream of the process chamber; and one or more sensors for measuring the temperature of the exhaust system at one or more locations of the exhaust system.
• a processing system comprises a process chamber; and an exhaust system coupled to the process chamber.
• the exhaust system comprises a remote plasma source for supplying an ionized cleaning gas to the exhaust system downstream of the process chamber; one or more sensors downstream of the remote plasma source for measuring the temperature of the exhaust system at one or more locations of the exhaust system; an endpoint detection system downstream of the one or more sensors; and a vacuum pump downstream of the endpoint detection system.
• a process for cleaning an exhaust system comprises introducing one or more ionized gases to the exhaust system downstream of a process chamber; monitoring the temperature within the exhaust system; and adjusting the flow rate of the one or more ionized gases based on the monitored temperature.
• Figure 1 is a schematic illustration of a processing system 100, according to one aspect of the disclosure.
• Figure 2 is a graph illustrating temperature response of an exhaust system during cleaning cycles.
• Figure 3 illustrates internal views of sections of the exhaust system after cleaning according to aspects described herein.
• aspects of the present disclosure generally relate to a methods and apparatuses for cleaning exhaust systems, such as exhaust systems used with process chambers for the formation of epitaxial silicon.
• the exhaust system includes a remote plasma source for supplying ionized gas through the exhaust system, and one or more temperature sensors positioned downstream of the remote plasma source. It is to be noted that the use of methods and apparatuses described herein are contemplated for other processes, such as etching, or the deposition of materials other than epitaxial silicon.
• FIG. 1 is a schematic illustration of a processing system 100, according to one aspect of the disclosure.
• the processing system 100 includes a process chamber 101 , such as an epitaxial deposition reactor, coupled to an exhaust system 102.
• the exhaust system 102 is coupled to a vacuum pump 103 at a downstream end thereof to facilitate flow of effluent to a scrubber 122 located downstream of the exhaust system 102.
• the exhaust system 102 may include an endpoint detection system 104 coupled thereto via bellows 105.
• the exhaust system 102 and the bellows 105 may be disposed upstream of the vacuum pump 103 to facilitate determination of the endpoint of a cleaning operation.
• a remote plasma source (RPS) 106 is coupled to the exhaust system 102 to ionize cleaning, purge, carrier, or other process gases, and to provide the ionized gases to the exhaust system 102.
• a first gas supply source 107 may be coupled to the RPS 106 to provide an inert or non- reactive gas, such as argon, therethrough to the exhaust system 102.
• a second gas supply source 108 may be coupled to the RPS 106 to provide a cleaning gas, such as NF 3 , therethrough to the exhaust system 102.
• Other contemplated cleaning gases include NF 2 H, CHF 3 , CF 4 , and the like. It is to be noted that other cleaning gases and other non-reactive gases are contemplated.
• the ionized gases facilitate removal of accumulated deposits from the interior of the exhaust system 102, thus reducing or eliminating the need for disassembly of the exhaust system 102 for cleaning.
• the exhaust system 102 includes a first isolation valve 109 which prevents the backflow of exhaust gases into the process chamber 101 .
• the process chamber 101 may be separated from the vacuum pump 103 by a wall 120.
• the RPS 106 is coupled to the exhaust system 102 downstream of the first isolation valve 109 via a gas passage 1 10.
• the gas passage 1 10 includes a second isolation valve 1 1 1 disposed therein for controlling gas flow therethrough, and thus, for controlling gas flow from the RPS 106 to the exhaust system 102.
• the isolation valves 109 and 1 1 1 may be controlled by a controller (not shown).
• the exhaust system 102 also includes one or more sensors 1 12a- 1 12g (seven are shown) for sensing temperature.
• a first temperature sensor 1 12a disposed downstream of the isolation valves 109 and 1 1 1 , and upstream of a pressure control valve 1 13.
• the remaining sensors 1 12b-1 12g are positioned downstream of the pressure control valve 1 13 and upstream of the bellows 105.
• the sensors 1 12a-1 12g facilitate monitoring of the exhaust temperature at different locations of the exhaust system 102.
• the sensors 1 12a-1 12g are positioned at locations in the exhaust system 102 susceptible to increased deposition of effluent material. For example, valves, elbows, T-fittings, and the like are susceptible to increase deposition of material.
• the sensors 1 12a-1 12g may be thermocouples. In one example, temperature sensors 1 12e and 1 12f are located below a floor 121. [0017] The temperature sensors 1 12a-1 12g facilitate monitoring of a cleaning operation within the exhaust system 102. The reaction of fluoride radicals from a cleaning gas with chlorosilane deposits is exothermic. Thus, the extent of reaction can be generally qualified through temperature measurements. For example, endpoint detection of the cleaning operation may be monitored by tracking the temperature within the exhaust system 102.
• An elevated temperature at the sensor 1 12a-1 12g indicates reaction of cleaning gas with deposited material, while a temperature approximately equal to or approaching ambient temperature (or the temperature of the cleaning gas exiting the RPS 106) indicates a substantially completed cleaning operation due to complete reaction/removal of deposited material.
• the sensors 1 12a-1 12g may be utilized to facilitate monitoring and control of the cleaning operation.
• the sensors 1 12a-1 12g may monitor temperature in order to prevent runaway exothermic reactions within the exhaust system.
• a signal may be relayed to a controller.
• the controller may adjust the flow rate (and/or stop the flow rate) of cleaning gas exiting the RPS 106.
• a decrease in the amount of cleaning gas limits the extent of reaction in the exhaust system 102, thus maintaining temperatures at desirable levels.
• each sensor 1 12a-1 12g may be programmed to the same or different temperatures limits.
• the pressure control valve 1 13 may be temperature-sensitive, and thus, sensors 1 12a and 1 12b adjacent the pressure control valve 1 13 may be limited to a relatively lower temperature, such as about 70 degrees Celsius to about 80 degrees Celsius.
• Sensors 1 12c-1 12g may be positioned adjacent components such as T-fitting or elbows, which are less temperature sensitive.
• the feedback signal for sensors 1 12c-1 12g may be set at a relatively higher temperature, such as about 1 10 degrees Celsius to about 130 degrees Celsius.
• the controller may respond based on the readings of more than one of the temperature sensors 1 12a-1 12g. For example, if only one of the temperature sensors 1 12a-1 12g records a high temperature, the controller may be configured not to respond until one or more additional temperature sensors 1 12a-1 12g records a high temperature.
• each sensor 1 12a-1 12g may include two-tiered limits. For example, when a first limit is reached, a signal may be relayed to reduce the flow of a cleaning gas. When a second, higher, limit is reached, a flow of the cleaning gas may be completely halted to quench any reactions in the exhaust system 102. It is contemplated that the sensors 1 12a-1 12g may be coupled to any suitable relay or communication link to facilitate transfer of information or control of gas flow. In one example, snap switches and/or interlock switches may be utilized to control gas flow within the exhaust system 102. The snap switches and/or interlock switches may be positioned adjacent to or coupled to a respective sensor 1 12a-1 12g.
• the controller may be configured to respond when a rate of temperature rise in one or more of the sensors 1 12a-1 12g is above a limit.
• the controller may sample temperature readings from the sensors 1 12a-1 12g according to a set interval, compare successive readings of the sensors 1 12a-1 12g to determine a temperature change, and compare the temperature change to a limit, which may be the same for all sensors 1 12a-1 12g or different for any or all of the sensors 1 12a-1 12g.
• the controller may then adjust flow of cleaning gas if any or all temperature changes are above their respective limits.
• a cleaning operation may be performed in the exhaust system after a predetermined interval, such as processing a specific number of substrates in the process chamber 101 .
• the isolation valve 109 is closed to prevent backflow of cleaning gas into the process chamber.
• the pressure within the process chamber 101 may be monitored to ensure that the isolation valve is not leaking and thus not undesirably allow cleaning gas to enter the process chamber.
• the second isolation valve 1 1 1 is opened to allow gas ionized by the RPS 106 to travel through the exhaust system 102, and additionally, the pressure control valve 1 13 is set to a position that gives a pressure suitable for striking a plasma, for example, about 0.5 torr to about 1 .5 torr.
• Argon is then allowed to flow through the RPS 106 at a flow rate within a range of about 500 standard cubic centimeters per minute (seem) to about 3000 seem.
• a plasma is then ignited in the RPS 106 and allowed to stabilize, for example, for about 5 seconds to about 10 seconds.
• a cleaning gas such as NF 3 is provided to the RPS 106 at flow rate within a range of 100 seem to about 500 seem, and is allowed to flow through the exhaust system 102 to remove accumulated material from within the exhaust system 102.
• a control system coupled to one or more sensors 1 12a-1 12g monitors the exhaust component temperature. If the exhaust components reach a predetermined threshold, the flow of cleaning gas is reduced or halted to allow the exhaust system 102 to cool. Once the temperature cools to a predetermined set point, the cleaning gas flow is resumed or elevated. The process may be repeated until the exhaust system 102 is sufficiently cleaned. Continued monitoring of the temperature facilities identification of cleaning endpoint. As the temperature of the components approaches ambient temperature, cleaning endpoint is indicated. Alternatively, clean process endpoint detection may be determined using the endpoint detection system 104, which may be, for example, a nondispersive infrared sensor.
• temperature within the exhaust system may be controlled using a variable flow ratio of carrier gas to cleaning gas.
• argon and NF 3 may be ionized in the RPS 106 using a flow ratio of about 2: 1 to about 4: 1 when initiating a cleaning operation.
• about 1 standard liter per minute (slm) of argon is provided to the RPS 106, while 250 seem of NF 3 are provided to the RPS.
• the flow rate of NF 3 may be increased until a 1 : 1 ratio of argon to NF 3 is reached, temperature permitting. The change in flow ratio allows a cleaning process to be expedited as safely allowed by process parameters.
• the flow of NF 3 gas may be pulsed according to a desired duty cycle. It is contemplated that pulsing the NF 3 gas may slow down the rate of temperature increase within the exhaust system 102. As another alternative, rather than decreasing or halting flow of the cleaning gas when a temperature threshold is reached, it is contemplated that the plasma in the RPS 106 may be extinguished. In such an aspect, the flow of cleaning gas may be allowed to continue flowing since cleaning gas is less reactive when not ionized by the RPS 106. Alternatively, flow of NF 3 gas may also be halted when plasma is extinguished.
• FIG. 2 is a graph illustrating temperature response of an exhaust system during cleaning cycles.
• the temperatures measured at each sensor 1 12b-1 12g e.g., sensors downstream of the pressure control valve 1 13 are shown).
• the relative spikes in temperature indicate an increase in temperature due to an exothermic reaction as ionized cleaning gas reacts with deposited material, and a decrease in temperature as the flow of cleaning gas is reduced or halted in response to reaching a threshold temperature.
• a threshold temperature of about 100 degrees Celsius is reached at sensor 1 12c at about 500 seconds, triggering a reduction in cleaning gas flow rate.
• the flow rate of cleaning gas is resumed when the temperature at the sensor 1 12c approaches 30 degrees Celsius. Subsequently, a threshold temperature of about 120 degrees is reached at sensor 1 12d, triggering a reduction in cleaning gas flow at around at 1 100 seconds. Similar peak events are illustrated around 1900 seconds 2500 seconds, 3200 seconds, 4000 seconds, 5000 seconds, and 6000 seconds. [0028] As noted above, the cycling of cleaning gas flow is continued until the exhaust system is sufficiently cleaned. The continued reduction in peak amplitude indicates a reduction in deposited material within the exhaust system, e.g., a reduction in reactant (for example, chlorosilane). As illustrated, at about 7000 seconds, the temperature within the exhaust system of all sensors approaches ambient temperature, indicating process endpoint.
• reactant for example, chlorosilane
• the exhaust system 102 may be purged to remove any cleaning gas or reacted by products from the exhaust system 102.
• the exhaust system 102 may be flushed using the carrier gas from the cleaning process, such as argon.
• the exhaust system 102 may be backfilled with nitrogen and flushed, while the isolation valves 109 and 1 1 1 are in the closed position.
• the exhaust system 102 may be backfilled and flushed multiple times, such as about 5-10 times.
• Figure 3 illustrates internal views of sections of the exhaust system after cleaning according to aspects described herein.
• Figure 3 illustrates internal views of the pressure control valve 1 13.
• aspects described herein sufficiently cleaned the pressure control valve 1 13, as no deposits are shown. The cleaning occurred without thermal damage to the pressure control valve 1 13.
• aspects described herein include safer and faster cleaning of exhaust systems. Aspects described herein may reduce cleaning times from up to one month to as little as 100 minutes or less. Additionally, the duration between timely and costly preventative maintenances may be extended. Moreover, aspects described herein reduce or eliminate the need to disassemble an exhaust system, which would otherwise expose chlorosilane to ambient oxygen and form chlorosiloxane. Even when disassembly is required, exposed components have much less chlorosilane present thereon after being cleaned in accordance with aspects of this disclosure. [0032] In one example, an exhaust system is cleaned in accordance with aspects described herein.
• hydrochloric acid which is outgassed as chlorosilane reacts with ambient oxygen
• ppm parts-per-million
• a conventional exhaust system which is disassembled for cleaning would likely exceed an HCI concentration of 5 ppm when exposed to the ambient environment.

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• 2017
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