WO2018179157A1 - Substrate processing device, heater unit, and semiconductor device manufacturing method - Google Patents

Substrate processing device, heater unit, and semiconductor device manufacturing method Download PDF

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Publication number
WO2018179157A1
WO2018179157A1 PCT/JP2017/012974 JP2017012974W WO2018179157A1 WO 2018179157 A1 WO2018179157 A1 WO 2018179157A1 JP 2017012974 W JP2017012974 W JP 2017012974W WO 2018179157 A1 WO2018179157 A1 WO 2018179157A1
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WO
WIPO (PCT)
Prior art keywords
side wall
reaction tube
heater
temperature
substrate processing
Prior art date
Application number
PCT/JP2017/012974
Other languages
French (fr)
Japanese (ja)
Inventor
野内　英博
稲田　哲明
立野　秀人
裕也 宮西
Original Assignee
株式会社Ｋｏｋｕｓａｉ Ｅｌｅｃｔｒｉｃ
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社Ｋｏｋｕｓａｉ Ｅｌｅｃｔｒｉｃ filed Critical 株式会社Ｋｏｋｕｓａｉ Ｅｌｅｃｔｒｉｃ
Priority to CN201780088409.5A priority Critical patent/CN110419095A/en
Priority to JP2019508441A priority patent/JP6730513B2/en
Priority to PCT/JP2017/012974 priority patent/WO2018179157A1/en
Priority to SG11201907981YA priority patent/SG11201907981YA/en
Publication of WO2018179157A1 publication Critical patent/WO2018179157A1/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering

Definitions

  • the present invention relates to a substrate processing apparatus, a heater unit, and a method for manufacturing a semiconductor device.
  • a liquid source containing hydrogen peroxide (H 2 O 2 ) is vaporized to generate a vaporized gas as a process gas, and this vaporized gas is applied to the substrate in the process chamber.
  • substrate processing including a supplying step is performed (see, for example, Patent Documents 1 and 2).
  • One of the objects of the present invention is to provide a technique capable of performing heating so as to prevent local deviation in the temperature of members forming the processing chamber.
  • a reaction tube that accommodates a substrate, a lid that closes a furnace port formed in the reaction tube, a heater provided on an outer periphery of a side wall near the furnace port of the reaction tube, A plurality of temperature sensors configured to measure temperatures at a plurality of positions different from each other in the circumferential direction of the side wall on the side wall near the furnace port of the reaction tube, and the measured values of the plurality of temperature sensors, respectively.
  • a control unit configured to control the heater.
  • FIG. 1 It is a schematic block diagram of the vertical processing furnace of the substrate processing apparatus used suitably by one Embodiment of this invention, and is a figure which shows a processing furnace part with a longitudinal cross-sectional view. It is a schematic block diagram which shows the furnace port periphery structure of the reaction tube of the substrate processing apparatus used suitably by one Embodiment of this invention, and is a figure which shows a furnace port periphery by a horizontal sectional view.
  • A is a longitudinal cross-sectional view which shows the structure of one form of a heater unit, and the structure of the periphery of the said heater unit.
  • (B) is the longitudinal cross-sectional view of the heater unit in the dashed-dotted line seen from the direction A shown to (a).
  • (A) is a longitudinal cross-sectional view which shows the structure of the other form of a heater unit, and the structure of the periphery of the said heater unit.
  • (B) is the longitudinal cross-sectional view of the heater unit in the dashed-dotted line seen from the direction A shown to (a).
  • (A) is a longitudinal cross-sectional view which shows the structure of the other form of a heater unit, and the structure of the periphery of a heater unit.
  • (B) is the longitudinal cross-sectional view of the heater unit in the dashed-dotted line seen from the direction A shown to (a).
  • the longitudinal cross-sectional view which shows the structure of a soaking
  • the longitudinal cross-sectional view of the heater unit which shows the attachment structure of the side wall temperature sensor attached to a heater unit.
  • the flowchart which shows an example of a substrate processing process.
  • the schematic block diagram which shows the position of the temperature monitoring points A-N in an Example.
  • the schematic block diagram which shows the structure of a comparative example, and the position of temperature monitoring point AN.
  • the graph which shows the measurement result of the temperature in the temperature monitor points A-N in each of an Example and a comparative example.
  • the processing furnace 202 includes a reaction tube 203.
  • the reaction tube 203 is made of a heat resistant material such as quartz (SiO 2 ) or silicon carbide (SiC), and is configured as a cylindrical member having a furnace port (opening) at the lower end.
  • a processing chamber 201 is formed in the cylindrical hollow portion of the reaction tube 203.
  • the processing chamber 201 includes a wafer storage area A (hereinafter referred to as area A) as a first area for storing a wafer 200 as a substrate, and a furnace port peripheral area as a second area provided below the area A in the vertical direction. B (hereinafter referred to as region B) is provided inside.
  • a seal cap 219 is provided as a lid that can airtightly close the lower end opening of the reaction tube 203.
  • a rotation mechanism 267 is installed below the seal cap 219.
  • the seal cap 219 is formed in a disc shape, and is configured such that an upper surface base portion 219a constituting the upper surface side and a lower surface base portion 219b constituting the lower surface side are laminated.
  • the upper surface base portion 219a is made of a nonmetallic member such as quartz, and has a thickness of about 10 to 20 mm.
  • the lower surface base portion 219b is made of a metal member such as SUS.
  • a rotation shaft 255 of the rotation mechanism 267 passes through the seal cap 219 and is connected to the boat 217.
  • the rotation mechanism 267 is configured to rotate the wafer 200 by rotating the boat 217.
  • a bearing portion 219s of the rotating shaft 255 provided on the rotating shaft 255 is configured as a fluid seal such as a magnetic seal.
  • the seal cap 219 is raised and lowered in the vertical direction by a boat elevator 115 installed below the reaction tube 203.
  • the boat elevator 115 is configured as a transfer mechanism that loads and unloads (transfers) the boat 217, that is, the wafer 200 into and out of the processing chamber 201 by moving the seal cap 219 up and down.
  • the boat 217 as a substrate support is configured to support a plurality of, for example, 25 to 200, wafers 200 in a multi-stage manner by aligning them vertically in a horizontal posture and with their centers aligned. It is configured to arrange at intervals.
  • the boat 217 is made of a heat-resistant material such as quartz or SiC, and includes a top plate 217a and a bottom plate 217b above and below.
  • the heat insulator 218 supported in a multi-stage at a lower position of the boat 217 is made of a heat resistant material such as quartz or SiC, and is configured to suppress heat conduction between the region A and the region B. .
  • the heat insulator 218 can also be considered as a part of the components of the boat 217.
  • a heater 207 as a first heating unit and a heater 208 as a second heating unit are provided outside the reaction tube 203. Electric power is supplied from the heater power supply unit 210 to the heaters 207 and 208.
  • the heater 207 is vertically installed so as to surround the area A.
  • the heater 207 is controlled so as to heat the wafer 200 accommodated in the region A to a predetermined temperature in a substrate processing step to be described later.
  • the heater 208 is provided vertically below the heater 207 so as to surround the region B.
  • the heater 208 includes a plurality of heater units (heater units 208a to 208d) arranged (divided) in the outer peripheral direction of the reaction tube 203.
  • the heater 208 is controlled to maintain the temperature of the side wall around the furnace port of the reaction tube 203 and the temperature of the piping at predetermined temperatures in the substrate processing step described later.
  • the side wall around the furnace port of the reaction tube 203 is simply referred to as a furnace port side wall.
  • a temperature sensor protective tube 263 a that penetrates the side wall of the reaction tube 203 from the outside to the inside and extends along the inner wall of the reaction tube 203 is provided.
  • a temperature sensor 263 as a temperature detection unit is inserted from the outside of the reaction tube 203 and provided in the temperature sensor protection tube 263a. Based on the temperature information detected by the temperature sensor 263, the output of the heater 207 is adjusted.
  • the temperature sensor 263 is mainly composed of a thermocouple. A plurality of temperature sensors 263 and temperature sensor protective tubes 263a may be provided.
  • a gas supply pipe 232 a for supplying vaporized gas into the processing chamber 201 is connected to the side wall of the reaction pipe 203.
  • the gas supply pipe 232a penetrates the side wall in the vicinity of the furnace port of the reaction tube 203 (that is, around the region B) from the outside to the inside, and extends to the vicinity of the upper end along the inner wall of the reaction tube 203.
  • the gas supply port 232p is configured. Note that a plurality of gas supply pipes 232a having different heights may be provided, and the vaporized gas may be supplied into the processing chamber 201 from the gas supply ports provided at the respective upper ends.
  • the gas supply pipe 232a is provided with a gas generator 250a, a mass flow controller (MFC) 241a that is a flow rate controller (flow rate control unit), and a valve 243a that is an on-off valve in order from the upstream side.
  • the gas generator 250a is connected to a liquid supply pipe that supplies hydrogen peroxide as a liquid source, a carrier gas supply pipe that supplies a carrier gas used to vaporize the liquid, and the like.
  • the hydrogen peroxide solution is an aqueous solution obtained by dissolving hydrogen peroxide (H 2 O 2 ), which is liquid at room temperature, in water (H 2 O) as a solvent.
  • the gas generator 250a generates vaporized gas by, for example, heating the hydrogen peroxide solution to a predetermined temperature (vaporization temperature) and vaporizing or misting it.
  • the vaporized gas contains gaseous or mist-like H 2 O 2 and water vapor (H 2 O gas) at predetermined concentrations.
  • H 2 O 2 contained in the vaporized gas is a kind of active oxygen, is unstable and easily releases O, generates OH radicals, and acts as an oxidizing agent (O source) having a very strong oxidizing power. To do.
  • the gas supply pipe 232a, the MFC 241a, and the valve 243a constitute a vaporized gas supply system.
  • An exhaust pipe 231 for exhausting the atmosphere in the processing chamber 201 is connected to the side wall of the reaction tube 203 near the furnace port (around the furnace port).
  • a vacuum pump 246 as an exhaust device is connected to the exhaust pipe 231 via a pressure sensor 245 as a pressure detector for detecting the pressure in the processing chamber 201 and an APC valve 244 as a pressure regulator.
  • the APC valve 244 can perform evacuation and evacuation stop in the processing chamber 201 by opening and closing the valve while the vacuum pump 246 is activated, and further, with the vacuum pump 246 activated,
  • the pressure in the processing chamber 201 can be adjusted by adjusting the valve opening based on the pressure information detected by the pressure sensor 245.
  • An exhaust system is mainly configured by the exhaust pipe 231, the APC valve 244, and the pressure sensor 245.
  • the vacuum pump 246 may be included in the exhaust system.
  • the heater 208 is mainly configured as follows to prevent these local low-temperature regions and high-temperature regions from occurring.
  • the heater unit 208 a is a portion of the side wall of the furnace port portion where the pipes such as the gas supply pipe 232 a, the temperature sensor protection pipe 263 a, and the exhaust pipe 231 are not connected (hereinafter referred to as “flat part”).
  • a unit arranged to heat a region (sometimes referred to as a “region”).
  • two heater units 208a (208a and 208a ′) are provided.
  • the heater unit 208b includes a peripheral portion of a portion where the gas supply pipe 232a is connected on the side wall of the furnace port, and a peripheral portion of the connection portion exposed outside the reaction tube 203 of the gas supply pipe 232a.
  • the heater unit 208c includes a peripheral portion of a portion where the temperature sensor protective tube 263a is connected on the side wall of the furnace port portion, and a peripheral portion of a connected portion which is exposed outside the reaction tube 203 of the temperature sensor protective tube 263a. , And a unit arranged to heat. That is, the heater unit 208c is configured to heat both the side wall of the reaction tube 203 and the temperature sensor protection tube 263a.
  • the heater unit 208d is a unit arranged to heat a peripheral portion of a connection portion with the reaction tube 203 in the exhaust pipe 231.
  • peripheral part of the location where the piping such as the gas supply pipe 232a, the temperature sensor protection pipe 263a, the exhaust pipe 231 and the like is connected is collectively referred to as a “projection part region” hereinafter. There is.
  • each of the heater units 208a to 208c can include a side wall temperature sensor (303a, 303b) that measures the outer peripheral surface temperature of the furnace port side wall. At least a plurality of side wall temperature sensors are provided at positions spaced apart in the outer circumferential direction. By controlling the heater 208 based on the temperatures respectively measured by the plurality of side wall temperature sensors, the temperature of the side wall of the reaction tube 203 can be heated to be uniform in the outer circumferential direction. Note that at least two or more side wall temperature sensors may be provided in the heater 208, and all of the heater units 208a to 208c do not have to include the side wall temperature sensor.
  • each of the heater units 208b to 208d can include a gas supply pipe temperature sensor 304b and an exhaust pipe temperature sensor 304d for measuring the temperature around the pipe such as the gas supply pipe 232a. ing.
  • the heater 208 By controlling the heater 208 based on the temperatures measured by the temperature sensors around these pipes, the pipes connected to the reaction tube 203 are individually heated, and the temperature of the side wall of the reaction tube 203 is more increased in the outer circumferential direction. It can be heated to be precisely uniform.
  • the heater units 208a to 208d are connected to the heater power supply unit 210, and the heater power supply unit 210 is configured to supply power to the heater units 208a to 208c. Further, the plurality of side wall temperature sensors are connected to a controller 121 as a control unit to be described later, and the controller 121 supplies power to the heater units 208a to 208d via the heater power supply unit 210 based on the measured temperature. Are configured to be controlled individually. By individually controlling the temperature of each of the plurality of heater units arranged in the outer peripheral direction of the reaction tube 203, it becomes easy to uniformly heat the furnace port side wall in the circumferential direction. Each of the heater units 208a to 208d may include an individual heater power supply unit and may be configured to be controlled by the controller 121.
  • the heater unit 208a is disposed along the outer periphery of the side wall of the furnace port. More specifically, the heater unit 208 a is placed on a flange that forms the lower end of the reaction tube 203 via an O-ring protection part 273. In addition, a partition portion 308 formed of SUS or the like is provided between the heater unit 208a and the heater 207, and in order to suppress heat influence from the heater 207 and heat escape from the heater unit 208a. Material 307 is filled.
  • the seal cap 219 has relatively few protruding structures such as the gas supply pipe 232a around the furnace port of the reaction tube 203. Therefore, it is relatively easy to heat the seal cap 219 evenly with the cap 209.
  • an O-ring 220a is provided as a seal member that contacts the lower end of the reaction tube 203. Further, an O-ring 220b as a seal member that comes into contact with the lower surface of the upper surface base portion 219a is provided on the upper surface of the lower surface base portion 219b.
  • the refrigerant flow path 274 provided in the O-ring protection part 273 and the refrigerant flow path 270 provided in the lower surface base 219b are respectively set so that the O-ring 220a and the O-ring 220b are not heated to a predetermined temperature or higher. It is configured to cool.
  • the heater unit 208a includes a heating wire 301a, a heating wire storage unit 305 integrally formed in a block shape for storing the heating wire 301a, and a heater cover 306 provided so as to surround the heating wire storage unit 305.
  • the side wall temperature sensor 303a which measures the outer peripheral surface temperature of the furnace port part side wall arrange
  • the exothermic wire 301a is formed of a spiral (spring-like) Kanthal wire or the like, and is provided at a position facing the outer periphery of the reaction tube 203 along the circumferential direction of the outer periphery.
  • the heating wire 301a is composed of one or a plurality of parallel heating wires. In order to heat the side wall of the reaction tube 203 evenly in the height direction, it is preferable to use a plurality of parallel heating lines.
  • the heating wire 301a is composed of four Kanthal wires arranged in parallel to each other.
  • the heating line 301a is constituted by a plurality of independent heating lines, but four parallel heating lines are formed by folding a single Kanthal line a plurality of times. You can also.
  • the heating wire 301a it is particularly preferable to use a wire having a characteristic that the peak wavelength of the heat rays radiated when generating heat at around 80 to 100 ° C. is around 5 to 10 ⁇ m (for example, Kanthal wire). These wavelengths are easily absorbed by quartz and are suitable for efficiently heating structures such as the reaction tube 203 and the gas supply tube 232a formed of quartz. The same applies to heating lines 301b, 302b, and 302d described later.
  • the heating wire storage portion 305 is formed of a low thermal conductivity material (thermal conductivity is 0.3 W / m ⁇ K or less) such as a porous industrial alumina board, and between the heating wires constituting the heating wire 301a. Temperature interference is suppressed. That is, the heating wire storage unit 305 functions as a separation member that prevents temperature interference between the heating wires.
  • a low thermal conductivity material thermal conductivity is 0.3 W / m ⁇ K or less
  • the heat generation amount of the heat generation lines arranged at the upper and lower ends among the plurality of heat generation lines arranged in parallel is larger than the heat generation amount of the other heat generation lines sandwiched between those heat generation lines.
  • the heating wire 301a By configuring the heating wire 301a to be large, the side wall of the reaction tube 203 is heated evenly in the height direction. More specifically, the thickness of the heating lines arranged at the upper and lower ends is configured to be thinner than the thickness of other heating lines sandwiched between the heating lines. Thereby, the electric resistance value of each heating wire is made different so that the heating value is made different for the same supply current amount.
  • the electric power supplied from the heater power supply unit 210 to the heating wire 301a is controlled by the controller 121 mainly based on the measured temperature of the side wall temperature sensor 303a.
  • the supplied power can be controlled based on the measured temperature of the side wall temperature sensor provided in another heater unit.
  • the supplied power can be controlled based on both the measured temperature of the sidewall temperature sensor 303a and the measured temperature of the other sidewall temperature sensor.
  • Heat unit 208b The configuration of the heater unit 208b and its periphery will be described in detail below with reference to FIGS. 4 (a) and 4 (b). Similarly to the heater unit 208a, the heater unit 208b is disposed along the outer periphery of the side wall of the furnace port. Among the specific configurations, the same components as those of the heater unit 208a and its surroundings are denoted by the same reference numerals in FIGS. 4A and 4B, and description thereof is omitted.
  • the heater unit 208b includes a heating line 301b and a heating line 302b, a heating line storage unit 305 that stores the heating lines 301a and 302b, and a gas supply pipe temperature sensor 304b as a pipe temperature sensor that measures the temperature in the vicinity of the gas supply pipe 232a.
  • a gas supply pipe temperature sensor 304b as a pipe temperature sensor that measures the temperature in the vicinity of the gas supply pipe 232a.
  • the side wall temperature sensor 303b which measures the outer peripheral surface temperature of a furnace port part side wall can be provided similarly to the heater unit 208a.
  • the gas supply pipe temperature sensor 304b may directly measure the temperature of the gas supply pipe 232a itself as long as the temperature state of the gas supply pipe 232a in the vicinity of the side wall of the reaction tube 203 can be grasped.
  • the heating wire 301b is provided along the circumferential direction of the outer periphery at a position facing the outer periphery of the reaction tube 203, and has the same configuration as the heating wire 301a. However, unlike the heating wire 301a, the heating wire 301b is disposed only at a position that avoids the position where the gas supply pipe 232a is disposed.
  • the heating wire 302b is composed of one or a plurality of heating wires arranged in the vicinity of the gas supply pipe 232a and arranged along the extending direction of the gas supply pipe 232a (parallel to the extending direction).
  • these heating lines are arranged so as to surround the gas supply pipe 232a.
  • only the exothermic wire 301b heats only the portion immediately adjacent to the side wall of the reaction tube 203 among the gas supply tube 232a protruding from the side wall of the reaction tube 203, and sufficiently heats the gas supply tube 232a in the extending direction. Is difficult. Therefore, heat escape from the side wall of the reaction tube 203 to the gas supply tube 232a cannot be prevented.
  • the heating wire 302b since the heating wire 302b is arranged in parallel to the gas supply pipe 232a, the gas supply pipe 232a can be heated uniformly in the extending direction.
  • the gas supply pipe temperature measurement sensor 304b is inserted into the heating wire storage unit 305 in parallel to the gas supply pipe 232a. It is preferable that the heating lines 302b are spaced apart from each other by a uniform distance.
  • the heating wire storage unit 305 is configured as an integrally formed member (storage block) that stores the heating wire 301b and the heating wire 302b, and suppresses temperature interference between the heating wire 301b and the heating wire 302b.
  • the temperatures (supply power) of the heating wire 301b and the heating wire 302b are individually controlled by the control unit, and the side wall of the reaction tube 203 and the gas supply tube 232a are individually heated.
  • independent and precise heating control can be easily performed on the side wall of the reaction tube 203 and the gas supply tube 232a.
  • the power supply from the heater power supply unit 210 to the heating wire 301b and the heating wire 302b is individually controlled by the controller 121.
  • the controller 121 controls the power supplied to the heating wire 301b via the heater power supply unit 210 mainly based on the measured temperature of the side wall temperature sensor 303b.
  • the controller 121 controls the power supplied to the heating wire 302b through the heater power supply unit 210 mainly based on the measured temperature of the gas supply pipe temperature sensor 304b.
  • the power supplied to at least one of the heating wire 301b and the heating wire 302b can be controlled based on both the measured temperature of the side wall temperature sensor 303b and the measured temperature of the gas supply pipe temperature sensor 204b.
  • one gas supply pipe 232a is connected to the protruding region on the side wall of the reaction tube 203 in which the heater unit 208b is disposed.
  • a modification in which a plurality of gas supply pipes are connected to the projecting region where one heater unit heater is disposed is conceivable.
  • 5A and 5B show the configuration of the heater unit 208b-1 and its surroundings in this modification. Among the specific configurations, the same components as those of the heater unit 208b and its surroundings are denoted by the same reference numerals in FIGS. 5A and 5B, and description thereof is omitted.
  • the heater unit 208b-1 is provided with one or a plurality of heating wires 302b for each of the plurality of gas supply pipes 232a.
  • the heating wire 302b is arranged in parallel to the gas supply pipe 232a, so that the gas supply pipe is heated evenly even when the interval between the gas supply pipes is narrow. Can do.
  • the heat generation lines 302b are arranged between the adjacent gas supply pipes 232a so that the plurality of gas supply pipes are heated by one heat generation line. Can do.
  • the gas supply pipe temperature measurement sensor 304b is provided for at least one of the plurality of gas supply pipes 232a, but may be provided for each of the plurality of gas supply pipes 232a.
  • Heat unit 208c The configuration of the heater unit 208c and its periphery is the same as that of the heater unit 208b.
  • the heater unit 208b heats the connection location of the gas supply pipe 232a, whereas the heater unit 208c differs only in heating the connection location of the temperature sensor protection pipe 263a.
  • Heat unit 208d Similarly to the heater units 208a to 208c, the heater unit 208d is disposed along the outer periphery of the side wall of the furnace port. The configuration of the heater unit 208d and its periphery will be described in detail below with reference to FIG.
  • the heater unit 208d includes a heating wire 302d, a storage member 305a that stores the heating wire 302d, storage members 305b and 305c that do not store the heating wire 302d, and an exhaust pipe 231 between the outer periphery of the exhaust pipe 231 and the heating wire 302d.
  • a soaking sheet 320 is provided so as to cover it.
  • an exhaust pipe temperature sensor 304d similarly to the gas supply pipe temperature sensor 304b in the heater unit 208b, an exhaust pipe temperature sensor 304d as a pipe temperature sensor for measuring the temperature in the vicinity of the exhaust pipe 231 can be provided.
  • the heating line 302d is configured by a plurality of heating lines arranged in the vicinity of the exhaust pipe 231 and in parallel with the exhaust pipe 231 similarly to the heating line 302b.
  • the heating wire 302d may not be disposed so as to surround the entire outer peripheral surface of the exhaust pipe 231. Therefore, the heater unit 208d is arranged so that at least one of these heat generation lines extends along only a part of the outer peripheral surface of the exhaust pipe 231 and is not disposed at a position along the remaining outer peripheral surface where the heat generation lines cannot be arranged. .
  • the storage members 305a to 305c are made of a low thermal conductivity material, similar to the heating wire storage portion 305. In addition, the storage members 305a to 305c are divided to facilitate attachment to the exhaust pipe 231.
  • the soaking sheet 320 conducts heat from the heating wire 302d disposed along only a part of the outer peripheral surface of the exhaust pipe 231 to the entire outer peripheral surface, and uniformly heats the outer peripheral surface of the exhaust pipe 231. It is provided as follows.
  • the soaking sheet 320 is made of an insulating material 321 made of a material such as alumina cloth, a high heat conductive material 322 made of a material such as an aluminum sheet, and a material such as a carbon sheet.
  • the structured cushioning material 323 is laminated and disposed.
  • the high heat conductive material 322 is disposed on the side close to the heating wire 302d, and conducts the heat of the heating wire 302d evenly in the entire outer circumferential direction of the exhaust pipe 231.
  • the cushion material 323 is disposed on the side close to the exhaust pipe 231, and causes the soaking sheet 320 to adhere to the outer peripheral surface of the exhaust pipe 231.
  • the thickness of the soaking sheet 320 is about 3 to 5 mm.
  • the soaking sheet 320 By providing the soaking sheet 320, local high temperature portions are suppressed from being generated on the outer peripheral surface of the exhaust pipe 231 facing the heating line 302d, and on the outer peripheral surface of the exhaust pipe 231 where the heating line 302d is not disposed. Generation of a local low temperature part can be suppressed.
  • the electric power supplied from the heater power supply unit 210 to the heating wire 302d is controlled by the controller 121 mainly based on the measured temperature of the exhaust pipe temperature sensor or the side wall temperature sensor provided in another heater unit.
  • the tip part which is the temperature measurement sensor part of the side wall temperature sensor 303a is in contact with the furnace port part side wall by the structure shown in FIG.
  • a fixing member 309 is fixed to the heater cover 306, and a spring 310, which is an elastic member, is provided between the protruding portion of the side wall temperature sensor 303a and the fixing member 309.
  • the spring 310 is configured to press the side wall temperature sensor 303a against the side wall of the reaction tube 203 with the fixing member 309 as a fulcrum.
  • the side wall temperature sensor 303b is also installed with a similar structure.
  • the flat region on the side wall of the reaction tube 203 where the heater unit 208a is installed is likely to be hotter than the projecting region where the heater units 208b, 208c and 208d are installed, and conversely, the projecting region is a flat region.
  • the temperature tends to be lower than that. This is because heat escape from the protruding portion such as the gas supply pipe 232a hardly occurs in the flat portion region, and the area in which the heating lines 301b and 301c are arranged in the protruding portion region is uniform. The reason is that it is difficult to heat properly.
  • the side wall temperature sensor 303a is provided in the heater unit 208a that heats the longest flat portion region
  • the side wall temperature sensor 303a ′ is provided in the heater unit 208a ′ disposed at a position facing the heater 208a
  • the protruding portion region is provided.
  • a side wall temperature sensor 303b is provided in the heater unit 208b ′ for heating the heater.
  • the side wall temperature sensors are arranged at these positions with heater control points at positions separated from each other in the outer peripheral direction of the reaction tube 203, the temperature of the side wall of the reaction tube 203 is determined based on the temperature measured at each position.
  • the heater units 208a to 208d can be individually controlled so as to be uniform in the outer circumferential direction.
  • the target temperature value (first target temperature) measured by the side wall temperature sensors 303a and 303a ′ for measuring the temperature of the flat portion region that is likely to become high is as follows. It is preferable to set the temperature lower than the target value (second target temperature) of the temperature measured by the side wall temperature sensor 303b that measures the temperature of the protruding region that tends to be low. This makes it easy to control the heater 208 so that the temperature of the side wall of the reaction tube 203 is uniform in the outer circumferential direction.
  • the heater units 208a and 208a ′ are mainly arranged so that the temperature measured by the side wall temperature sensors 303a and 303a ′ that measure the temperature of the flat region does not exceed a predetermined temperature (for example, a first upper limit temperature described later). By controlling, it becomes easy to prevent a local high temperature region from being generated on the side wall around the furnace port.
  • a predetermined temperature for example, a first upper limit temperature described later.
  • the heater unit 208b ′ controls the heater unit 208b ′ so that the temperature measured by the side wall temperature sensor 303b that measures the temperature of the protruding region does not become lower than a predetermined temperature (for example, a first lower limit temperature described later), It becomes easy to prevent a local low temperature region from occurring on the side wall around the furnace port.
  • a predetermined temperature for example, a first lower limit temperature described later
  • the heater 208 it is possible to more easily control the heater 208 so that the temperature of the side wall of the reaction tube 203 falls within a predetermined temperature range (for example, the first lower limit temperature or higher and the first upper limit temperature or lower) in the outer peripheral direction. .
  • a predetermined temperature range for example, the first lower limit temperature or higher and the first upper limit temperature or lower
  • three sidewall temperature sensors are provided.
  • at least one sidewall temperature sensor is provided for each of the flat region where the heater unit 208a is disposed and the protruding region where the heater units 208b to 208d are disposed.
  • the above-described effects can be obtained.
  • the heater units 208a to 208d are connected to each other by a structure in which crank-shaped end faces are combined as shown in FIG.
  • the outer peripheral surfaces of the connection portions of the heater units 208a to 208d are covered (covered) with a protective cover 330 made of a material such as SUS.
  • the controller 121 as a control unit is configured as a computer including a CPU 121a, a RAM 121b, a storage device 121c, and an I / O port 121d.
  • the RAM 121b, the storage device 121c, and the I / O port 121d are configured to exchange data with the CPU 121a via the internal bus 121e.
  • An input / output device 122 configured as a touch panel or the like is connected to the controller 121.
  • the storage device 121c is configured by a flash memory, an HDD, or the like.
  • a control program that controls the operation of the substrate processing apparatus, a process recipe that describes the procedure and conditions of the substrate processing described later, and the like are stored in a readable manner.
  • the process recipe is a combination of functions so that a predetermined result can be obtained by causing the controller 121 to execute each procedure described later, and functions as a program.
  • the process recipe, the control program, and the like are collectively referred to simply as a program.
  • the process recipe is also simply called a recipe.
  • program When the term “program” is used in this specification, it may include only a recipe, only a control program, or both.
  • the RAM 121b is configured as a memory area that temporarily stores programs, data, and the like read by the CPU 121a.
  • the I / O port 121d includes the MFC 241a, the valve 243a, the gas generator 250a, the pressure sensor 245, the APC valve 244, the vacuum pump 246, the heater power supply unit 210, the temperature sensor 263, the side wall temperature sensors 303a and 303b, and the gas supply pipe.
  • the temperature sensor 304b, the exhaust pipe temperature sensor 304d, the rotation mechanism 267, the boat elevator 115, and the like are connected.
  • the CPU 121a is configured to read out and execute a control program from the storage device 121c and to read a recipe from the storage device 121c in response to an operation command input from the input / output device 122 or the like.
  • the CPU 121a performs a gas generation operation by the gas generator 250a, a gas flow rate adjustment operation by the MFC 241a, an opening / closing operation of the valve 243a, a pressure adjustment operation by the APC valve 244 based on the pressure sensor 245, and a vacuum in accordance with the contents of the read recipe.
  • the controller 121 installs the above-mentioned program stored in an external storage device (for example, a magnetic disk such as an HDD, an optical disk such as a CD, a magneto-optical disk such as an MO, or a semiconductor memory such as a USB memory) 123 in a computer.
  • an external storage device for example, a magnetic disk such as an HDD, an optical disk such as a CD, a magneto-optical disk such as an MO, or a semiconductor memory such as a USB memory
  • the storage device 121c and the external storage device 123 are configured as computer-readable recording media. Hereinafter, these are collectively referred to simply as a recording medium.
  • recording medium When the term “recording medium” is used in this specification, it may include only the storage device 121c alone, may include only the external storage device 123 alone, or may include both of them.
  • the program may be provided to the computer using a communication means such as the Internet or a dedicated line without using the external storage device 123.
  • a film having a silazane bond (—Si—N—) (polysilazane film) is formed on the surface of the substrate that is subjected to predetermined processing in the substrate processing step.
  • this film contains nitrogen (N) and hydrogen (H), and may further contain carbon (C) and other impurities.
  • the polysilazane film formed on the wafer 200 is modified (oxidized) by supplying a vaporized gas containing H 2 O 2 under a relatively low temperature condition.
  • a plurality of wafers 200 having a polysilazane film formed on the surface are loaded into a boat 217. Thereafter, as shown in FIG. 1, the boat 217 that supports the plurality of wafers 200 is lifted by the boat elevator 115 and carried into the processing chamber 201. In this state, the seal cap 219 is in a state of sealing the lower end of the reaction tube 203 via the O-ring 220a.
  • the inside of the processing chamber 201 is evacuated by the vacuum pump 246 so that the space in which the wafer 200 exists, that is, the space where the wafer 200 exists becomes a predetermined pressure (reforming pressure). Further, the reaction tube 203, the wafer 200 accommodated in the processing chamber 201, the seal cap 219, and the like are heated by the heaters 207 and 208 and the cap heater 209.
  • the state of energization from the heater power supply unit 210 to the heater 207 is feedback controlled based on the temperature information detected by the temperature sensor 263 so that the wafer 200 accommodated in the region A has a predetermined temperature.
  • the side wall of the furnace port portion of the reaction tube 203 is detected.
  • the temperature and the temperature of the gas supply pipe 232a, the temperature sensor protection pipe 263a, and the exhaust pipe 231 are each set to a predetermined temperature (or a predetermined temperature distribution). The state of energization is feedback controlled.
  • the feedback control of the heaters 207 and 208 is continuously performed at least until the processing on the wafer 200 is completed. Further, the rotation of the wafer 200 by the rotation mechanism 267 is started. The operation of the vacuum pump 246 and the heating and rotation of the wafer 200 are continuously performed at least until the processing on the wafer 200 is completed.
  • valve 243a is closed and the supply of the vaporized gas into the processing chamber 201 is stopped.
  • Examples of the processing conditions for the reforming step include the following. H 2 O 2 concentration of liquid raw material: 20 to 40%, preferably 25 to 35% Liquid raw material vaporization conditions: Heated to 120 to 200 ° C. at approximately atmospheric pressure Reforming pressure: 700 to 1000 hPa (any of atmospheric pressure, slightly reduced pressure, and slightly increased pressure) Wafer 200 temperature: 70 to 110 ° C., preferably 70 to 80 ° C.
  • the vaporized gas supplied into the processing chamber 201 is liquefied in the processing chamber 201, and the liquid thus generated can stay around the furnace port (such as the upper surface of the seal cap 219).
  • the furnace port such as the upper surface of the seal cap 219.
  • the gas supply pipe 232a in the processing chamber 201, the temperature sensor protection pipe 263a, and the like a local low temperature region may be generated as described above, and the locally generated low temperature region is contacted. By doing so, the vaporized gas tends to re-liquefy.
  • the heater 208 configured as described above, the side wall of the furnace port of the reaction tube 203 and the like are heated evenly, and a local low temperature region is prevented from being generated.
  • temperature control is performed so that a region below a predetermined temperature (first lower limit temperature) does not occur on the side wall and the like around the furnace port.
  • the lower limit temperature varies depending on conditions such as the concentration of vaporized gas, but is, for example, 80 ° C. or higher under the above-described processing conditions.
  • the liquid generated by re-liquefaction of the vaporized gas tends to be in a state where H 2 O 2 is concentrated to a high concentration, that is, a high concentration H 2 O 2 solution. Further, the retained high concentration H 2 O 2 liquid tends to change to a state in which H 2 O 2 is further concentrated to a higher concentration.
  • the high-concentration H 2 O 2 liquid is very reactive and has a strong corrosive action, which may cause serious damage to the furnace port member.
  • H 2 O 2 is O 2 gas and the H 2 O gas contained in the high concentration H 2 O 2 solution
  • the explosive decomposition reaction means that a liquid containing H 2 O 2 is rapidly decomposed into oxygen gas (O 2 ) and water vapor (H 2 O) and expands to explode, burn, or close to these. It is to cause a phenomenon.
  • An explosive decomposition reaction can occur when the H 2 O 2 liquid exceeds a certain temperature (explosion critical temperature) at a certain H 2 O 2 liquid concentration and pressure. Therefore, the high concentration H 2 O 2 liquid retained by reliquefaction must be maintained so as not to exceed the explosion critical temperature.
  • the explosion critical temperature varies depending on the concentration of H 2 O 2 in the high-concentration H 2 O 2 liquid, and specifically decreases as the concentration of H 2 O 2 increases.
  • the lowering of the explosion critical temperature becomes the lower limit when the concentration of the high concentration H 2 O 2 liquid reaches 100%. Therefore, when the treatment pressure is atmospheric pressure, the temperature of the high concentration H 2 O 2 liquid is maintained at a temperature lower than 112 ° C., which is the explosion critical temperature when the concentration is 100%. Occurrence can be reliably avoided.
  • the side wall and the like of the furnace port of the reaction tube 203 are evenly heated to prevent the occurrence of a local high temperature region.
  • temperature control is performed so that a region exceeding a predetermined temperature (first upper limit temperature) does not occur on the side wall around the furnace port. I do.
  • the first upper limit temperature is 112 ° C. or lower when the processing pressure is atmospheric pressure.
  • the present embodiment is applied when performing temperature control in a temperature region (that is, a temperature region of 120 ° C. or lower, more preferably 100 ° C. or lower) in which the influence of heat transfer by heat conduction is larger than that of heat transfer by radiation.
  • a temperature region that is, a temperature region of 120 ° C. or lower, more preferably 100 ° C. or lower
  • temperature controllability can be improved.
  • the heating control by the cap heater 209 can be maintained within the temperature range so that the temperature controllability by the heater 208 can be maintained.
  • the heater 207 is controlled to heat the wafer 200 to a temperature higher than the above-described reforming temperature. By maintaining this temperature, the wafer 200 and the inside of the processing chamber 201 are gently dried.
  • the seal cap 219 is lowered by the boat elevator 115 and the lower end of the reaction tube 203 is opened. Then, the processed wafer 200 is unloaded from the lower end of the reaction tube 203 to the outside of the reaction tube 203.
  • Example An example of the present embodiment and a comparative example will be described below.
  • the temperature of the heater 208 in this embodiment was controlled, and the temperatures at the temperature monitoring points A to N shown in FIG. 12 were measured.
  • Monitor points A to H are points on the upper surface base 219a
  • monitor points I to N are points on the outer peripheral surface of the side wall around the furnace port.
  • temperature control is performed by a heater having the following configuration in place of the heater 208 of the present embodiment, and temperature monitoring points A, B, E, F, I, K, L are performed in the same manner as in the examples.
  • N were measured.
  • the control was performed by setting the target temperature at the monitor points A to H to 80 to 112 ° C.
  • the substrate processing apparatus in the comparative example includes a heater 400 that heats the side wall around the furnace port, and a jacket heater 401 that heats the protruding portion such as the gas supply pipe 232a.
  • the heater 400 does not include the side wall temperature sensor 303a of this embodiment, and is configured to perform temperature control only by the heater output.
  • the jacket heater 401 is installed so as to be wound around each protrusion such as the gas supply pipe 232a, and is mainly provided for the purpose of heating only the protrusion.
  • FIG. 14 shows the measurement results of the temperatures at the monitor points A to N in the example and the comparative example.
  • the occurrence of a local high temperature region was particularly noticeable particularly at the monitor points A and I having a large distance from the protruding portion.
  • the result exceeded 112 ° C. as the first upper limit temperature.
  • processing procedure and processing conditions at this time can be the same processing procedure and processing conditions as in the above-described embodiment, for example.

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Abstract

Provided is a substrate processing device provided with: a reaction tube in which a substrate is housed; a lid portion for closing a furnace opening formed in the reaction tube; a heater disposed on the outer periphery of a side wall in the vicinity of the furnace opening of the reaction tube; a plurality of temperature sensors respectively configured to measure the temperatures at a plurality of mutually different positions in the circumferential direction of the side wall in the vicinity of the furnace opening of the reaction tube; and a control unit configured to control the heater on the basis of respective measurement values according to the plurality of temperature sensors. In this way, heating is performed so as to prevent the development of local deviations in the temperatures of members of which a processing chamber is formed.

Description

基板処理装置、ヒータユニットおよび半導体装置の製造方法Substrate processing apparatus, heater unit, and semiconductor device manufacturing method
　本発明は、基板処理装置、ヒータユニットおよび半導体装置の製造方法に関する。 The present invention relates to a substrate processing apparatus, a heater unit, and a method for manufacturing a semiconductor device.
　半導体装置の製造工程の一工程として、過酸化水素（Ｈ２Ｏ２）を含む液体原料を気化させて処理ガスとしての気化ガスを生成する工程と、処理室内の基板に対してこの気化ガスを供給する工程と、を含む基板処理が行われることがある（例えば特許文献１，２参照）。 As a process of manufacturing the semiconductor device, a liquid source containing hydrogen peroxide (H 2 O 2 ) is vaporized to generate a vaporized gas as a process gas, and this vaporized gas is applied to the substrate in the process chamber. In some cases, substrate processing including a supplying step is performed (see, for example, Patent Documents 1 and 2).
国際公開第２０１４／０６９８２６号International Publication No. 2014/069826 国際公開第２０１３／０７０３４３号International Publication No. 2013/070343
　上述の基板処理を行うと、条件によっては、処理室内へ供給された気化ガスが処理室内において冷やされて液化したり、液化で生じた液体が加熱されて急激な反応を起こしたりする。このような現象は、処理室を形成する部材の温度が不均一になることによって局所的な低温領域や高温領域が生じることにより起こる場合がある。本発明の目的の一つは、処理室を形成する部材の温度に局所的な偏りが生じることを防止するように加熱を行うことが可能な技術を提供することにある。 When the above-described substrate processing is performed, depending on conditions, the vaporized gas supplied into the processing chamber is cooled and liquefied in the processing chamber, or the liquid generated by the liquefaction is heated to cause a rapid reaction. Such a phenomenon may occur when a local low temperature region or a high temperature region is generated due to non-uniform temperatures of members forming the processing chamber. One of the objects of the present invention is to provide a technique capable of performing heating so as to prevent local deviation in the temperature of members forming the processing chamber.
　本発明の一態様によれば、基板を収容する反応管と、前記反応管に形成された炉口を閉塞する蓋部と、前記反応管の炉口近傍の側壁の外周に設けられたヒータと、前記反応管の炉口近傍の側壁における、前記側壁の周方向において互いに異なる複数の位置の温度をそれぞれ測定するよう構成された複数の温度センサと、前記複数の温度センサのそれぞれの測定値に基づいて、前記ヒータを制御するよう構成された制御部と、を備える基板処理装置が提供される。 According to one aspect of the present invention, a reaction tube that accommodates a substrate, a lid that closes a furnace port formed in the reaction tube, a heater provided on an outer periphery of a side wall near the furnace port of the reaction tube, A plurality of temperature sensors configured to measure temperatures at a plurality of positions different from each other in the circumferential direction of the side wall on the side wall near the furnace port of the reaction tube, and the measured values of the plurality of temperature sensors, respectively. And a control unit configured to control the heater.
本発明の一実施形態で好適に用いられる基板処理装置の縦型処理炉の概略構成図であり、処理炉部分を縦断面図で示す図。It is a schematic block diagram of the vertical processing furnace of the substrate processing apparatus used suitably by one Embodiment of this invention, and is a figure which shows a processing furnace part with a longitudinal cross-sectional view. 本発明の一実施形態で好適に用いられる基板処理装置の反応管の炉口周辺構造を示す概略構成図であり、炉口周辺を水平断面図で示す図。It is a schematic block diagram which shows the furnace port periphery structure of the reaction tube of the substrate processing apparatus used suitably by one Embodiment of this invention, and is a figure which shows a furnace port periphery by a horizontal sectional view. （ａ）は、ヒータユニットの一形態の構成、及び当該ヒータユニットの周辺の構成を示す縦断面図。（ｂ）は、（ａ）に示す方向Ａから見た、一点鎖線におけるヒータユニットの縦断面図。(A) is a longitudinal cross-sectional view which shows the structure of one form of a heater unit, and the structure of the periphery of the said heater unit. (B) is the longitudinal cross-sectional view of the heater unit in the dashed-dotted line seen from the direction A shown to (a). （ａ）は、ヒータユニットの他の形態の構成、及び当該ヒータユニットの周辺の構成を示す縦断面図。（ｂ）は、（ａ）に示す方向Ａから見た、一点鎖線におけるヒータユニットの縦断面図。(A) is a longitudinal cross-sectional view which shows the structure of the other form of a heater unit, and the structure of the periphery of the said heater unit. (B) is the longitudinal cross-sectional view of the heater unit in the dashed-dotted line seen from the direction A shown to (a). （ａ）は、ヒータユニットの他の形態の構成、及びヒータユニットの周辺の構成を示す縦断面図。（ｂ）は、（ａ）に示す方向Ａから見た、一点鎖線におけるヒータユニットの縦断面図。(A) is a longitudinal cross-sectional view which shows the structure of the other form of a heater unit, and the structure of the periphery of a heater unit. (B) is the longitudinal cross-sectional view of the heater unit in the dashed-dotted line seen from the direction A shown to (a). ヒータユニットの他の形態の構成を示す概略構成図であり、排気管の延伸方向に垂直な面を断面とした縦断面図。It is a schematic block diagram which shows the structure of the other form of a heater unit, and is the longitudinal cross-sectional view which made the surface perpendicular | vertical to the extending | stretching direction of an exhaust pipe into a cross section. 均熱シートの構成を示す縦断面図。The longitudinal cross-sectional view which shows the structure of a soaking | uniform-heating sheet | seat. ヒータユニットに取り付けられる側壁温度センサの取り付け構造を示すヒータユニットの縦断面図。The longitudinal cross-sectional view of the heater unit which shows the attachment structure of the side wall temperature sensor attached to a heater unit. ヒータユニット間の接続構造を説明する概略構成図。The schematic block diagram explaining the connection structure between heater units. 本発明の一実施形態で好適に用いられる基板処理装置のコントローラの概略構成図であり、コントローラの制御系をブロック図で示す図。It is a schematic block diagram of the controller of the substrate processing apparatus used suitably by one Embodiment of this invention, and is a figure which shows the control system of a controller with a block diagram. 基板処理工程の一例を示すフロー図。The flowchart which shows an example of a substrate processing process. 実施例における温度モニタ点Ａ～Ｎの位置を示す概略構成図。The schematic block diagram which shows the position of the temperature monitoring points A-N in an Example. 比較例の構成と、温度モニタ点Ａ～Ｎの位置を示す概略構成図。The schematic block diagram which shows the structure of a comparative example, and the position of temperature monitoring point AN. 実施例と比較例それぞれにおける温度モニタ点Ａ～Ｎにおける温度の測定結果を示すグラフ。The graph which shows the measurement result of the temperature in the temperature monitor points A-N in each of an Example and a comparative example.
＜本発明の一実施形態＞
　以下、本発明の一実施形態について、図１～図２を用いて説明する。 <One Embodiment of the Present Invention>
Hereinafter, an embodiment of the present invention will be described with reference to FIGS.
（１）基板処理装置の構成
　図１に示すように、処理炉２０２は反応管２０３を備えている。反応管２０３は、例えば石英（ＳｉＯ２）や炭化シリコン（ＳｉＣ）等の耐熱性材料からなり、下端に炉口（開口）を有する円筒部材として構成されている。反応管２０３の筒中空部には、処理室２０１が形成される。処理室２０１は、基板としてのウエハ２００を収容する第１領域としてのウエハ収容領域Ａ（以下、領域Ａ）、および、領域Ａの鉛直方向下方に設けられた第２領域としての炉口周辺領域Ｂ（以下、領域Ｂ）を、内部に備えている。 (1) Configuration of Substrate Processing Apparatus As shown in FIG. 1, the processing furnace 202 includes a reaction tube 203. The reaction tube 203 is made of a heat resistant material such as quartz (SiO 2 ) or silicon carbide (SiC), and is configured as a cylindrical member having a furnace port (opening) at the lower end. A processing chamber 201 is formed in the cylindrical hollow portion of the reaction tube 203. The processing chamber 201 includes a wafer storage area A (hereinafter referred to as area A) as a first area for storing a wafer 200 as a substrate, and a furnace port peripheral area as a second area provided below the area A in the vertical direction. B (hereinafter referred to as region B) is provided inside.
　反応管２０３の下方には、反応管２０３の下端開口を気密に閉塞可能な蓋部としてのシールキャップ２１９が設けられている。シールキャップ２１９の下方には、回転機構２６７が設置されている。シールキャップ２１９は円盤状に形成されており、上面側を構成する上面ベース部２１９ａと、下面側を構成する下面ベース部２１９ｂとが積層するように構成されている。上面ベース部２１９ａは、例えば石英等の非金属部材により構成され、その厚さは１０～２０ｍｍ程度である。下面ベース部２１９ｂは、例えばＳＵＳ等の金属部材により構成されている。回転機構２６７の回転軸２５５は、シールキャップ２１９を貫通してボート２１７に接続されている。回転機構２６７は、ボート２１７を回転させることでウエハ２００を回転させるように構成されている。回転軸２５５に開設された回転軸２５５の軸受部２１９ｓは、磁気シール等の流体シールとして構成されている。シールキャップ２１９は、反応管２０３の下方に設置されたボートエレベータ１１５によって垂直方向に昇降させられる。ボートエレベータ１１５は、シールキャップ２１９を昇降させることで、ボート２１７すなわちウエハ２００を処理室２０１内外に搬入および搬出（搬送）する搬送機構として構成されている。 Below the reaction tube 203, a seal cap 219 is provided as a lid that can airtightly close the lower end opening of the reaction tube 203. A rotation mechanism 267 is installed below the seal cap 219. The seal cap 219 is formed in a disc shape, and is configured such that an upper surface base portion 219a constituting the upper surface side and a lower surface base portion 219b constituting the lower surface side are laminated. The upper surface base portion 219a is made of a nonmetallic member such as quartz, and has a thickness of about 10 to 20 mm. The lower surface base portion 219b is made of a metal member such as SUS. A rotation shaft 255 of the rotation mechanism 267 passes through the seal cap 219 and is connected to the boat 217. The rotation mechanism 267 is configured to rotate the wafer 200 by rotating the boat 217. A bearing portion 219s of the rotating shaft 255 provided on the rotating shaft 255 is configured as a fluid seal such as a magnetic seal. The seal cap 219 is raised and lowered in the vertical direction by a boat elevator 115 installed below the reaction tube 203. The boat elevator 115 is configured as a transfer mechanism that loads and unloads (transfers) the boat 217, that is, the wafer 200 into and out of the processing chamber 201 by moving the seal cap 219 up and down.
　基板支持具としてのボート２１７は、複数枚、例えば２５～２００枚のウエハ２００を、水平姿勢で、かつ、互いに中心を揃えた状態で垂直方向に整列させて多段に支持するように、すなわち、間隔を空けて配列させるように構成されている。ボート２１７は、例えば石英やＳｉＣ等の耐熱性材料からなり、上下に天板２１７ａ、底板２１７ｂを備えている。ボート２１７の下部に水平姿勢で多段に支持された断熱体２１８は、例えば石英やＳｉＣ等の耐熱性材料からなり、領域Ａと領域Ｂとの間の熱伝導を抑制するように構成されている。断熱体２１８をボート２１７の構成部材の一部と考えることもできる。 The boat 217 as a substrate support is configured to support a plurality of, for example, 25 to 200, wafers 200 in a multi-stage manner by aligning them vertically in a horizontal posture and with their centers aligned. It is configured to arrange at intervals. The boat 217 is made of a heat-resistant material such as quartz or SiC, and includes a top plate 217a and a bottom plate 217b above and below. The heat insulator 218 supported in a multi-stage at a lower position of the boat 217 is made of a heat resistant material such as quartz or SiC, and is configured to suppress heat conduction between the region A and the region B. . The heat insulator 218 can also be considered as a part of the components of the boat 217.
　反応管２０３の外側には、第１加熱部としてのヒータ２０７と、第２加熱部としてのヒータ２０８と、が設けられている。ヒータ２０７，２０８へは、ヒータ電源ユニット２１０から電力が供給される。 A heater 207 as a first heating unit and a heater 208 as a second heating unit are provided outside the reaction tube 203. Electric power is supplied from the heater power supply unit 210 to the heaters 207 and 208.
　ヒータ２０７は、領域Ａを囲うように垂直に据え付けられている。ヒータ２０７は、後述する基板処理工程において、領域Ａに収容されたウエハ２００を所定の温度に加熱するように制御される。 The heater 207 is vertically installed so as to surround the area A. The heater 207 is controlled so as to heat the wafer 200 accommodated in the region A to a predetermined temperature in a substrate processing step to be described later.
　ヒータ２０８は、領域Ｂを囲うようにヒータ２０７の鉛直方向下方に設けられている。ヒータ２０８は、反応管２０３の外周方向に配列（分割）された複数のヒータユニット（ヒータユニット２０８ａ～２０８ｄ）により構成されている。ヒータ２０８は、後述する基板処理工程において、特に反応管２０３の炉口周辺の側壁の温度や配管の温度をそれぞれ所定の温度に維持するよう制御される。なお以下では、反応管２０３の炉口周辺の側壁を、単に炉口部側壁と称する。 The heater 208 is provided vertically below the heater 207 so as to surround the region B. The heater 208 includes a plurality of heater units (heater units 208a to 208d) arranged (divided) in the outer peripheral direction of the reaction tube 203. The heater 208 is controlled to maintain the temperature of the side wall around the furnace port of the reaction tube 203 and the temperature of the piping at predetermined temperatures in the substrate processing step described later. Hereinafter, the side wall around the furnace port of the reaction tube 203 is simply referred to as a furnace port side wall.
　処理室２０１内には、反応管２０３の側壁を外側から内側に貫通するとともに、反応管２０３の内壁に沿って延伸する、温度センサ保護管２６３ａが設けられている。温度センサ保護管２６３ａの管内には、温度検出部としての温度センサ２６３が反応管２０３の外側から挿通されて設けられている。温度センサ２６３により検出された温度情報に基づいて、ヒータ２０７の出力が調整される。温度センサ２６３は主に熱電対により構成される。なお、温度センサ２６３及び温度センサ保護管２６３ａは複数設けてもよい。 In the processing chamber 201, a temperature sensor protective tube 263 a that penetrates the side wall of the reaction tube 203 from the outside to the inside and extends along the inner wall of the reaction tube 203 is provided. A temperature sensor 263 as a temperature detection unit is inserted from the outside of the reaction tube 203 and provided in the temperature sensor protection tube 263a. Based on the temperature information detected by the temperature sensor 263, the output of the heater 207 is adjusted. The temperature sensor 263 is mainly composed of a thermocouple. A plurality of temperature sensors 263 and temperature sensor protective tubes 263a may be provided.
　反応管２０３の側壁には、気化ガスを処理室２０１内に供給するガス供給管２３２ａが接続されている。ガス供給管２３２ａは、反応管２０３の炉口近傍（すなわち領域Ｂ周辺）の側壁を外側から内側に貫通して、反応管２０３の内壁に沿って上端近傍まで延伸しており、その先端は開口してガス供給ポート２３２ｐを構成している。なお、高さが互いに異なるガス供給管２３２ａを複数設けて、それぞれの上端に設けられたガス供給ポートから気化ガスを処理室２０１内に供給するように構成してもよい。ガス供給管２３２ａには、上流側から順に、ガス発生器２５０ａ、流量制御器（流量制御部）であるマスフローコントローラ（ＭＦＣ）２４１ａ、開閉弁であるバルブ２４３ａが設けられている。ガス発生器２５０ａには、液体原料としての過酸化水素水を供給する液体供給管や、液体を気化させるために用いるキャリアガスを供給するキャリアガス供給管等が接続されている。 A gas supply pipe 232 a for supplying vaporized gas into the processing chamber 201 is connected to the side wall of the reaction pipe 203. The gas supply pipe 232a penetrates the side wall in the vicinity of the furnace port of the reaction tube 203 (that is, around the region B) from the outside to the inside, and extends to the vicinity of the upper end along the inner wall of the reaction tube 203. Thus, the gas supply port 232p is configured. Note that a plurality of gas supply pipes 232a having different heights may be provided, and the vaporized gas may be supplied into the processing chamber 201 from the gas supply ports provided at the respective upper ends. The gas supply pipe 232a is provided with a gas generator 250a, a mass flow controller (MFC) 241a that is a flow rate controller (flow rate control unit), and a valve 243a that is an on-off valve in order from the upstream side. The gas generator 250a is connected to a liquid supply pipe that supplies hydrogen peroxide as a liquid source, a carrier gas supply pipe that supplies a carrier gas used to vaporize the liquid, and the like.
　ここで過酸化水素水とは、常温で液体である過酸化水素（Ｈ２Ｏ２）を溶媒としての水（Ｈ２Ｏ）中に溶解させることで得られる水溶液のことである。ガス発生器２５０ａは、過酸化水素水を所定の温度（気化温度）に加熱する等し、これを気化或いはミスト化させることによって気化ガスを発生させる。気化ガス中には、ガス状或いはミスト状のＨ２Ｏ２および水蒸気（Ｈ２Ｏガス）がそれぞれ所定の濃度で含まれる。気化ガスに含まれるＨ２Ｏ２は、活性酸素の一種であり、不安定であってＯを放出しやすく、ＯＨラジカルを生成させ、非常に強い酸化力を持つ酸化剤（Ｏソース）として作用する。 Here, the hydrogen peroxide solution is an aqueous solution obtained by dissolving hydrogen peroxide (H 2 O 2 ), which is liquid at room temperature, in water (H 2 O) as a solvent. The gas generator 250a generates vaporized gas by, for example, heating the hydrogen peroxide solution to a predetermined temperature (vaporization temperature) and vaporizing or misting it. The vaporized gas contains gaseous or mist-like H 2 O 2 and water vapor (H 2 O gas) at predetermined concentrations. H 2 O 2 contained in the vaporized gas is a kind of active oxygen, is unstable and easily releases O, generates OH radicals, and acts as an oxidizing agent (O source) having a very strong oxidizing power. To do.
　主に、ガス供給管２３２ａ、ＭＦＣ２４１ａ、バルブ２４３ａにより、気化ガス供給系が構成される。 Mainly, the gas supply pipe 232a, the MFC 241a, and the valve 243a constitute a vaporized gas supply system.
　反応管２０３の炉口近傍（炉口周辺）の側壁には、処理室２０１内の雰囲気を排気する排気管２３１が接続されている。排気管２３１には、処理室２０１内の圧力を検出する圧力検出器としての圧力センサ２４５および圧力調整器としてのＡＰＣバルブ２４４を介して、排気装置としての真空ポンプ２４６が接続されている。ＡＰＣバルブ２４４は、真空ポンプ２４６を作動させた状態で弁を開閉することで、処理室２０１内の真空排気および真空排気停止を行うことができ、さらに、真空ポンプ２４６を作動させた状態で、圧力センサ２４５により検出された圧力情報に基づいて弁開度を調節することで、処理室２０１内の圧力を調整することができるように構成されている。主に、排気管２３１、ＡＰＣバルブ２４４、圧力センサ２４５により、排気系が構成される。真空ポンプ２４６を排気系に含めて考えてもよい。 An exhaust pipe 231 for exhausting the atmosphere in the processing chamber 201 is connected to the side wall of the reaction tube 203 near the furnace port (around the furnace port). A vacuum pump 246 as an exhaust device is connected to the exhaust pipe 231 via a pressure sensor 245 as a pressure detector for detecting the pressure in the processing chamber 201 and an APC valve 244 as a pressure regulator. The APC valve 244 can perform evacuation and evacuation stop in the processing chamber 201 by opening and closing the valve while the vacuum pump 246 is activated, and further, with the vacuum pump 246 activated, The pressure in the processing chamber 201 can be adjusted by adjusting the valve opening based on the pressure information detected by the pressure sensor 245. An exhaust system is mainly configured by the exhaust pipe 231, the APC valve 244, and the pressure sensor 245. The vacuum pump 246 may be included in the exhaust system.
　ここで、炉口部側壁では、ガス供給管２３２ａ、温度センサ保護管２６３ａ、排気管２３１等のように反応管２０３から外側に突出した部位（突出部）から熱逃げが発生したり、突出部が存在することによりヒータによる均一な加熱が困難であったりする。そのため、炉口部側壁や、処理室２０１内のガス供給管２３２ａや温度センサ保護管２６３ａ等に局所的な低温領域が生じることがある。また一方で、局所的な低温領域が生じないようにヒータの出力を上げることにより、反対に局所的な高温領域が生じることがある。本実施形態では、主にヒータ２０８を以下のように構成することにより、これらの局所的な低温領域や高温領域が生じることを防止する。 Here, on the side wall of the furnace port, heat escape occurs from a portion (protrusion) protruding outward from the reaction tube 203 such as the gas supply pipe 232a, the temperature sensor protection pipe 263a, the exhaust pipe 231 or the like. In some cases, uniform heating by a heater is difficult. Therefore, a local low temperature region may occur in the side wall of the furnace port, the gas supply pipe 232a in the processing chamber 201, the temperature sensor protection pipe 263a, or the like. On the other hand, when the output of the heater is increased so as not to generate a local low temperature region, a local high temperature region may be generated. In the present embodiment, the heater 208 is mainly configured as follows to prevent these local low-temperature regions and high-temperature regions from occurring.
（ヒータ２０８の構成）
　ヒータ２０８を構成するヒータユニット２０８ａ～２０８ｄのそれぞれの構成について説明する。 (Configuration of heater 208)
The configuration of each of the heater units 208a to 208d constituting the heater 208 will be described.
　図２に示されるように、ヒータユニット２０８ａは、炉口部側壁のうち、ガス供給管２３２ａ、温度センサ保護管２６３ａ、及び排気管２３１等の配管が接続されていない部分（以下、「平坦部領域」と称することがある）を加熱するよう配設されたユニットである。本実施形態では、ヒータユニット２０８ａが２個（２０８ａ及び２０８ａ´）設けられている。 As shown in FIG. 2, the heater unit 208 a is a portion of the side wall of the furnace port portion where the pipes such as the gas supply pipe 232 a, the temperature sensor protection pipe 263 a, and the exhaust pipe 231 are not connected (hereinafter referred to as “flat part”). A unit arranged to heat a region (sometimes referred to as a “region”). In the present embodiment, two heater units 208a (208a and 208a ′) are provided.
　ヒータユニット２０８ｂは、炉口部側壁のうちガス供給管２３２ａが接続されている箇所の周辺部分と、ガス供給管２３２ａのうち反応管２０３の外に露出している接続箇所の周辺部分と、を加熱するよう配設されたユニットである。すなわち、ヒータユニット２０８ｂは、反応管２０３の側壁とガス供給管２３２ａの両者を加熱するように構成されている。 The heater unit 208b includes a peripheral portion of a portion where the gas supply pipe 232a is connected on the side wall of the furnace port, and a peripheral portion of the connection portion exposed outside the reaction tube 203 of the gas supply pipe 232a. A unit arranged to heat. That is, the heater unit 208b is configured to heat both the side wall of the reaction tube 203 and the gas supply tube 232a.
　ヒータユニット２０８ｃは、炉口部側壁のうち温度センサ保護管２６３ａが接続されている箇所の周辺部分と、温度センサ保護管２６３ａのうち反応管２０３の外に露出している接続箇所の周辺部分と、を加熱するよう配設されたユニットである。すなわち、ヒータユニット２０８ｃは、反応管２０３の側壁と温度センサ保護管２６３ａの両者を加熱するように構成されている。 The heater unit 208c includes a peripheral portion of a portion where the temperature sensor protective tube 263a is connected on the side wall of the furnace port portion, and a peripheral portion of a connected portion which is exposed outside the reaction tube 203 of the temperature sensor protective tube 263a. , And a unit arranged to heat. That is, the heater unit 208c is configured to heat both the side wall of the reaction tube 203 and the temperature sensor protection tube 263a.
　ヒータユニット２０８ｄは、排気管２３１のうち反応管２０３との接続箇所の周辺部分を加熱するよう配設されたユニットである。 The heater unit 208d is a unit arranged to heat a peripheral portion of a connection portion with the reaction tube 203 in the exhaust pipe 231.
　なお、炉口部側壁のうち、ガス供給管２３２ａ、温度センサ保護管２６３ａ、排気管２３１等の配管が接続されている箇所の周辺部分を、以下、総称して「突出部領域」と称することがある。 In addition, the peripheral part of the location where the piping such as the gas supply pipe 232a, the temperature sensor protection pipe 263a, the exhaust pipe 231 and the like is connected is collectively referred to as a “projection part region” hereinafter. There is.
　ヒータユニット２０８ａ～２０８ｃは、後述するように、それぞれが炉口部側壁の外周面温度を測定する側壁温度センサ（３０３ａ，３０３ｂ）を備えることが可能な構成となっており、ヒータ２０８は、互いに外周方向に離間した位置に配置された、少なくとも複数の側壁温度センサを備えている。これらの複数の側壁温度センサでそれぞれ測定された温度に基づいてヒータ２０８を制御することにより、反応管２０３の側壁の温度を外周方向において均等になるように加熱することができる。なお、側壁温度センサは、ヒータ２０８において少なくとも２以上備えられればよく、ヒータユニット２０８ａ～２０８ｃの全てが側壁温度センサを備える必要はない。 As will be described later, each of the heater units 208a to 208c can include a side wall temperature sensor (303a, 303b) that measures the outer peripheral surface temperature of the furnace port side wall. At least a plurality of side wall temperature sensors are provided at positions spaced apart in the outer circumferential direction. By controlling the heater 208 based on the temperatures respectively measured by the plurality of side wall temperature sensors, the temperature of the side wall of the reaction tube 203 can be heated to be uniform in the outer circumferential direction. Note that at least two or more side wall temperature sensors may be provided in the heater 208, and all of the heater units 208a to 208c do not have to include the side wall temperature sensor.
また、ヒータユニット２０８ｂ～２０８ｄは、後述するように、それぞれがガス供給管２３２ａ等の配管周辺の温度を測定するガス供給管温度センサ３０４ｂや排気管温度センサ３０４ｄを備えることが可能な構成となっている。これらの配管周辺の温度センサで測定された温度に基づいてヒータ２０８を制御することにより、反応管２０３に接続された配管を個別に加熱して、反応管２０３の側壁の温度を外周方向においてより精密に均等になるように加熱することができる。 Further, as will be described later, each of the heater units 208b to 208d can include a gas supply pipe temperature sensor 304b and an exhaust pipe temperature sensor 304d for measuring the temperature around the pipe such as the gas supply pipe 232a. ing. By controlling the heater 208 based on the temperatures measured by the temperature sensors around these pipes, the pipes connected to the reaction tube 203 are individually heated, and the temperature of the side wall of the reaction tube 203 is more increased in the outer circumferential direction. It can be heated to be precisely uniform.
　ヒータユニット２０８ａ～２０８ｄはヒータ電源ユニット２１０に接続されており、ヒータ電源ユニット２１０からは、ヒータユニット２０８ａ～２０８ｃそれぞれに対して電力が供給されるように構成されている。また、複数の側壁温度センサは、後述する制御部としてのコントローラ１２１に接続されており、コントローラ１２１は測定された温度に基づいて、ヒータ電源ユニット２１０を介してヒータユニット２０８ａ～２０８ｄへの供給電力を個別に制御するよう構成されている。反応管２０３の外周方向に配列された複数のヒータユニットそれぞれが個別に温度制御を行うことにより、炉口部側壁を周方向で均等に加熱することが容易になる。なお、ヒータユニット２０８ａ～２０８ｄは、それぞれが個別のヒータ電源ユニットを備え、それぞれがコントローラ１２１により制御されるように構成されていてもよい。 The heater units 208a to 208d are connected to the heater power supply unit 210, and the heater power supply unit 210 is configured to supply power to the heater units 208a to 208c. Further, the plurality of side wall temperature sensors are connected to a controller 121 as a control unit to be described later, and the controller 121 supplies power to the heater units 208a to 208d via the heater power supply unit 210 based on the measured temperature. Are configured to be controlled individually. By individually controlling the temperature of each of the plurality of heater units arranged in the outer peripheral direction of the reaction tube 203, it becomes easy to uniformly heat the furnace port side wall in the circumferential direction. Each of the heater units 208a to 208d may include an individual heater power supply unit and may be configured to be controlled by the controller 121.
（ヒータユニット２０８ａ）
　ヒータユニット２０８ａ及びその周辺の構成について、図３（ａ）（ｂ）を参照しながら以下詳述する。　ヒータユニット２０８ａは、炉口部側壁外周に沿って配設されている。より具体的には、ヒータユニット２０８ａは、反応管２０３の下端をなすフランジの上にＯリング保護部２７３を介して載置されている。また、ヒータユニット２０８ａとヒータ２０７の間にはＳＵＳ等で形成された仕切り部３０８が設けられており、その間にはヒータ２０７からの熱影響やヒータユニット２０８ａからの熱逃げを抑制するために断熱材３０７が充填されている。 (Heater unit 208a)
The configuration of the heater unit 208a and its periphery will be described in detail below with reference to FIGS. 3 (a) and 3 (b). The heater unit 208a is disposed along the outer periphery of the side wall of the furnace port. More specifically, the heater unit 208 a is placed on a flange that forms the lower end of the reaction tube 203 via an O-ring protection part 273. In addition, a partition portion 308 formed of SUS or the like is provided between the heater unit 208a and the heater 207, and in order to suppress heat influence from the heater 207 and heat escape from the heater unit 208a. Material 307 is filled.
　また、シールキャップ２１９の下面には、シールキャップ２１９の上面（より具体的には上面ベース２１９ａの上面）を所定の温度（例えば９０℃）とするようにシールキャップ２１９を加熱するキャップヒータ２０９が配設されている。なお、シールキャップ２１９には、反応管２０３の炉口周辺におけるガス供給管２３２ａ等のような突出した構造が比較的少ない。そのため、キャップ２０９によってシールキャップ２１９を均等に加熱することは、比較的容易である。 A cap heater 209 that heats the seal cap 219 so that the upper surface of the seal cap 219 (more specifically, the upper surface of the upper surface base 219a) is at a predetermined temperature (for example, 90 ° C.) is provided on the lower surface of the seal cap 219. It is arranged. The seal cap 219 has relatively few protruding structures such as the gas supply pipe 232a around the furnace port of the reaction tube 203. Therefore, it is relatively easy to heat the seal cap 219 evenly with the cap 209.
　上面ベース部２１９ａの上面には、反応管２０３の下端と当接するシール部材としてのＯリング２２０ａが設けられている。また、下面ベース部２１９ｂの上面には、上面ベース部２１９ａの下面と当接するシール部材としてのＯリング２２０ｂが設けられている。Ｏリング保護部２７３内に設けられた冷媒流路２７４、及び下面ベース２１９ｂ内に設けられた冷媒流路２７０はそれぞれ、Ｏリング２２０ａ及びＯリング２２０ｂが所定の温度以上に加熱されないように、それらを冷却するように構成されている。 On the upper surface of the upper surface base portion 219a, an O-ring 220a is provided as a seal member that contacts the lower end of the reaction tube 203. Further, an O-ring 220b as a seal member that comes into contact with the lower surface of the upper surface base portion 219a is provided on the upper surface of the lower surface base portion 219b. The refrigerant flow path 274 provided in the O-ring protection part 273 and the refrigerant flow path 270 provided in the lower surface base 219b are respectively set so that the O-ring 220a and the O-ring 220b are not heated to a predetermined temperature or higher. It is configured to cool.
　ヒータユニット２０８ａは、発熱線３０１ａ、発熱線３０１ａを格納するブロック状に一体形成された発熱線格納部３０５、及び発熱線格納部３０５を囲うように設けられたヒータカバー３０６により構成されている。また、発熱線格納部３０５及びヒータカバー３０６を貫通して配置された、炉口部側壁の外周面温度を測定する側壁温度センサ３０３ａを備えることができる。 The heater unit 208a includes a heating wire 301a, a heating wire storage unit 305 integrally formed in a block shape for storing the heating wire 301a, and a heater cover 306 provided so as to surround the heating wire storage unit 305. Moreover, the side wall temperature sensor 303a which measures the outer peripheral surface temperature of the furnace port part side wall arrange | positioned through the heating wire storage part 305 and the heater cover 306 can be provided.
　発熱線３０１ａは、らせん状（バネ状）に形成されたカンタル線等によって形成され、反応管２０３の外周に面する位置に、外周の周方向に沿って設けられている。　発熱線３０１ａは、１本又は複数本の互いに平行な発熱線により構成される。反応管２０３の側壁を高さ方向において均等に加熱するためには、互いに平行な発熱線を複数本とすることが好ましい。本実施形態では、発熱線３０１ａは４本の互いに平行に配置されたカンタル線により構成されている。なお、本実施形態では、それぞれが独立した複数本の発熱線により発熱線３０１ａを構成しているが、１本のカンタル線を複数回折り返すことにより４本の互いに平行な発熱線を形成することもできる。 The exothermic wire 301a is formed of a spiral (spring-like) Kanthal wire or the like, and is provided at a position facing the outer periphery of the reaction tube 203 along the circumferential direction of the outer periphery. The heating wire 301a is composed of one or a plurality of parallel heating wires. In order to heat the side wall of the reaction tube 203 evenly in the height direction, it is preferable to use a plurality of parallel heating lines. In the present embodiment, the heating wire 301a is composed of four Kanthal wires arranged in parallel to each other. In the present embodiment, the heating line 301a is constituted by a plurality of independent heating lines, but four parallel heating lines are formed by folding a single Kanthal line a plurality of times. You can also.
発熱線３０１ａは、８０～１００℃付近で発熱する時に放射する熱線のピーク波長が５～１０μｍ付近となる特性を有するもの（例えばカンタル線）を用いることが特に好ましい。これらの波長は石英に吸収され易く、石英で形成された、反応管２０３やガス供給管２３２ａ等の構造物を効率的に加熱するために適している。後述する発熱線３０１ｂ,３０２ｂ，３０２ｄについても同様である。 As the heating wire 301a, it is particularly preferable to use a wire having a characteristic that the peak wavelength of the heat rays radiated when generating heat at around 80 to 100 ° C. is around 5 to 10 μm (for example, Kanthal wire). These wavelengths are easily absorbed by quartz and are suitable for efficiently heating structures such as the reaction tube 203 and the gas supply tube 232a formed of quartz. The same applies to heating lines 301b, 302b, and 302d described later.
　発熱線格納部３０５は、ポーラス状の工業用アルミナボード等の低熱伝導率材料（熱伝導率が０．３Ｗ／ｍ・Ｋ以下）により形成されており、発熱線３０１ａを構成する各発熱線間の温度干渉を抑制している。すなわち、発熱線間格納部３０５は、発熱線間の温度干渉を防止する離間部材として機能する。 The heating wire storage portion 305 is formed of a low thermal conductivity material (thermal conductivity is 0.3 W / m · K or less) such as a porous industrial alumina board, and between the heating wires constituting the heating wire 301a. Temperature interference is suppressed. That is, the heating wire storage unit 305 functions as a separation member that prevents temperature interference between the heating wires.
　ただし、発熱線３０１ａを構成する各発熱線間における温度干渉を完全に遮断することは一般に困難である。そのため、本実施形態では、平行に配置された複数本の発熱線のうち、上下端に配置された発熱線の発熱量が、それらの発熱線に挟まれた他の発熱線の発熱量よりも大きくなるように発熱線３０１ａを構成することにより、反応管２０３の側壁が高さ方向において均等に加熱されるようにしている。より具体的には、上下端に配置された発熱線の太さが、それらの発熱線に挟まれた他の発熱線の太さよりも細くなるように構成している。これにより、各発熱線の電気抵抗値を異ならせて、同じ供給電流量に対して発熱量を異ならせている。 However, it is generally difficult to completely block the temperature interference between the heating wires constituting the heating wire 301a. Therefore, in the present embodiment, the heat generation amount of the heat generation lines arranged at the upper and lower ends among the plurality of heat generation lines arranged in parallel is larger than the heat generation amount of the other heat generation lines sandwiched between those heat generation lines. By configuring the heating wire 301a to be large, the side wall of the reaction tube 203 is heated evenly in the height direction. More specifically, the thickness of the heating lines arranged at the upper and lower ends is configured to be thinner than the thickness of other heating lines sandwiched between the heating lines. Thereby, the electric resistance value of each heating wire is made different so that the heating value is made different for the same supply current amount.
　ヒータ電源ユニット２１０から発熱線３０１ａへ供給される電力は、主に側壁温度センサ３０３ａの測定温度に基づいて、コントローラ１２１により制御される。但し、当該ヒータユニット２０８ａに側壁温度センサ３０３ａが設けられていない場合には、他のヒータユニットに設けられた側壁温度センサの測定温度に基づいて供給電力を制御することもできる。また、側壁温度センサ３０３ａの測定温度と他の側壁温度センサの測定温度の両方に基づいて供給電力を制御することもできる。 The electric power supplied from the heater power supply unit 210 to the heating wire 301a is controlled by the controller 121 mainly based on the measured temperature of the side wall temperature sensor 303a. However, when the side wall temperature sensor 303a is not provided in the heater unit 208a, the supplied power can be controlled based on the measured temperature of the side wall temperature sensor provided in another heater unit. In addition, the supplied power can be controlled based on both the measured temperature of the sidewall temperature sensor 303a and the measured temperature of the other sidewall temperature sensor.
（ヒータユニット２０８ｂ）
　ヒータユニット２０８ｂ及びその周辺の構成について、図４（ａ）（ｂ）を参照しながら以下詳述する。　ヒータユニット２０８ｂは、ヒータユニット２０８ａと同様に、炉口部側壁外周に沿って配設されている。具体的な構成のうち、ヒータユニット２０８ａ及びその周辺の構成と同じものについては、図４（ａ）（ｂ）において同じ符号を付しており説明を省略する。 (Heater unit 208b)
The configuration of the heater unit 208b and its periphery will be described in detail below with reference to FIGS. 4 (a) and 4 (b). Similarly to the heater unit 208a, the heater unit 208b is disposed along the outer periphery of the side wall of the furnace port. Among the specific configurations, the same components as those of the heater unit 208a and its surroundings are denoted by the same reference numerals in FIGS. 4A and 4B, and description thereof is omitted.
　ヒータユニット２０８ｂは、発熱線３０１ｂ及び発熱線３０２ｂ、発熱線３０１ａ及び３０２ｂを格納する発熱線格納部３０５、及びガス供給管２３２ａの近傍温度を測定する配管温度センサとしてのガス供給管温度センサ３０４ｂを備えている。また、ヒータユニット２０８ａと同様に、炉口部側壁の外周面温度を測定する側壁温度センサ３０３ｂを備えることができる。なお、ガス供給管温度センサ３０４ｂは、反応管２０３の側壁近傍のガス供給管２３２ａの温度状態を把握できれば、ガス供給管２３２ａ自体の温度を直接測定するものであってもよい。 The heater unit 208b includes a heating line 301b and a heating line 302b, a heating line storage unit 305 that stores the heating lines 301a and 302b, and a gas supply pipe temperature sensor 304b as a pipe temperature sensor that measures the temperature in the vicinity of the gas supply pipe 232a. I have. Moreover, the side wall temperature sensor 303b which measures the outer peripheral surface temperature of a furnace port part side wall can be provided similarly to the heater unit 208a. Note that the gas supply pipe temperature sensor 304b may directly measure the temperature of the gas supply pipe 232a itself as long as the temperature state of the gas supply pipe 232a in the vicinity of the side wall of the reaction tube 203 can be grasped.
　発熱線３０１ｂは、反応管２０３の外周に面する位置に、外周の周方向に沿って設けられており、発熱線３０１ａと同様の構成を備えている。ただし、発熱線３０１ｂは発熱線３０１ａと異なり、ガス供給管２３２ａが配置された位置を避ける位置にのみ配置されている。 The heating wire 301b is provided along the circumferential direction of the outer periphery at a position facing the outer periphery of the reaction tube 203, and has the same configuration as the heating wire 301a. However, unlike the heating wire 301a, the heating wire 301b is disposed only at a position that avoids the position where the gas supply pipe 232a is disposed.
　発熱線３０２ｂは、ガス供給管２３２ａの近傍に配置され、且つガス供給管２３２ａの延伸方向に沿って（延伸方向に対して平行に）配置された、１本又は複数本の発熱線により構成される。複数本の発熱線により構成されている場合、これらの発熱線はガス供給管２３２ａを取り囲むように配置される。ここで、発熱線３０１ｂのみでは、反応管２０３の側壁から突出したガス供給管２３２ａのうち、反応管２０３の側壁直近部分のみを加熱するにとどまり、ガス供給管２３２ａを延伸方向において十分に加熱することが困難である。そのため、反応管２０３の側壁からガス供給管２３２ａへの熱逃げを防ぐことができない。一方、本実施形態によれば、発熱線３０２ｂはガス供給管２３２ａに対して平行に配置されているため、ガス供給管２３２ａを延伸方向において均等に加熱することができる。 The heating wire 302b is composed of one or a plurality of heating wires arranged in the vicinity of the gas supply pipe 232a and arranged along the extending direction of the gas supply pipe 232a (parallel to the extending direction). The In the case of a plurality of heating lines, these heating lines are arranged so as to surround the gas supply pipe 232a. Here, only the exothermic wire 301b heats only the portion immediately adjacent to the side wall of the reaction tube 203 among the gas supply tube 232a protruding from the side wall of the reaction tube 203, and sufficiently heats the gas supply tube 232a in the extending direction. Is difficult. Therefore, heat escape from the side wall of the reaction tube 203 to the gas supply tube 232a cannot be prevented. On the other hand, according to this embodiment, since the heating wire 302b is arranged in parallel to the gas supply pipe 232a, the gas supply pipe 232a can be heated uniformly in the extending direction.
　ガス供給管温度測定センサ３０４ｂは、ガス供給管２３２ａに対して平行に発熱線格納部３０５内に挿入されている。発熱線３０２ｂの複数本の発熱線からは均等な距離をもって離間していることが好ましい。 The gas supply pipe temperature measurement sensor 304b is inserted into the heating wire storage unit 305 in parallel to the gas supply pipe 232a. It is preferable that the heating lines 302b are spaced apart from each other by a uniform distance.
　発熱線格納部３０５は、発熱線３０１ｂと発熱線３０２ｂを格納する、一体形成された部材（格納ブロック）として構成されおり、発熱線３０１ｂと発熱線３０２ｂの間の温度干渉を抑制している。後述するように、発熱線３０１ｂ及び発熱線３０２ｂの温度（供給電力）は制御部により個別に制御され、反応管２０３の側壁とガス供給管２３２ａをそれぞれ個別に加熱するように構成されている。ここで、発熱線３０１ｂと発熱線３０２ｂの間の温度干渉を抑えることにより、反応管２０３の側壁とガス供給管２３２ａに対して、独立した緻密な加熱制御を行うことが容易になる。 The heating wire storage unit 305 is configured as an integrally formed member (storage block) that stores the heating wire 301b and the heating wire 302b, and suppresses temperature interference between the heating wire 301b and the heating wire 302b. As will be described later, the temperatures (supply power) of the heating wire 301b and the heating wire 302b are individually controlled by the control unit, and the side wall of the reaction tube 203 and the gas supply tube 232a are individually heated. Here, by suppressing temperature interference between the heating wire 301b and the heating wire 302b, independent and precise heating control can be easily performed on the side wall of the reaction tube 203 and the gas supply tube 232a.
　発熱線３０１ｂ及び発熱線３０２ｂに対するヒータ電源ユニット２１０からの電力供給は、コントローラ１２１によりそれぞれ個別に制御される。コントローラ１２１は、ヒータ電源ユニット２１０を介して、発熱線３０１ｂへの供給電力を、主に側壁温度センサ３０３ｂの測定温度に基づいて制御する。また、コントローラ１２１は、ヒータ電源ユニット２１０を介して、発熱線３０２ｂへの供給電力を、主にガス供給管温度センサ３０４ｂの測定温度に基づいて制御する。但し、発熱線３０１ｂ及び発熱線３０２ｂの少なくとも一方の供給電力を、側壁温度センサ３０３ｂの測定温度とガス供給管温度センサ２０４ｂの測定温度の両方に基づいて制御することもできる。 The power supply from the heater power supply unit 210 to the heating wire 301b and the heating wire 302b is individually controlled by the controller 121. The controller 121 controls the power supplied to the heating wire 301b via the heater power supply unit 210 mainly based on the measured temperature of the side wall temperature sensor 303b. The controller 121 controls the power supplied to the heating wire 302b through the heater power supply unit 210 mainly based on the measured temperature of the gas supply pipe temperature sensor 304b. However, the power supplied to at least one of the heating wire 301b and the heating wire 302b can be controlled based on both the measured temperature of the side wall temperature sensor 303b and the measured temperature of the gas supply pipe temperature sensor 204b.
（ヒータユニット２０８ｂの変形例）
　本実施形態では、ヒータユニット２０８ｂが配置された反応管２０３の側壁の突出部領域に対して、１本のガス供給管２３２ａが接続されている。これに対して、１つのヒータユニットヒータが配置された突出部領域に対して、複数本のガス供給管が接続される変形例が考えられる。図５（ａ）（ｂ）は、この変形例におけるヒータユニット２０８ｂ－１及びその周辺の構成を示している。　具体的な構成のうち、ヒータユニット２０８ｂ及びその周辺の構成と同じものについては、図５（ａ）（ｂ）において同じ符号を付しており説明を省略する。 (Modification of heater unit 208b)
In the present embodiment, one gas supply pipe 232a is connected to the protruding region on the side wall of the reaction tube 203 in which the heater unit 208b is disposed. On the other hand, a modification in which a plurality of gas supply pipes are connected to the projecting region where one heater unit heater is disposed is conceivable. 5A and 5B show the configuration of the heater unit 208b-1 and its surroundings in this modification. Among the specific configurations, the same components as those of the heater unit 208b and its surroundings are denoted by the same reference numerals in FIGS. 5A and 5B, and description thereof is omitted.
　ヒータユニット２０８ｂ－１は特に、複数のガス供給管２３２ａのそれぞれに対して、発熱線３０２ｂが１本又は複数本配置されている。図５（ｂ）に示した構成のように、本変形例では、複数のガス供給管２３２ａの間隔が狭くなっており、このような場合、従来は発熱線の配置が困難であった。一方、本変形例によれば、発熱線３０２ｂがガス供給管２３２ａに対して平行に配置されているため、ガス供給管の間隔が狭い場合であっても、ガス供給管を均等に加熱することができる。また、複数のガス供給管２３２ａの間隔が狭い場合、隣り合うガス供給管２３２ａの間に発熱線３０２ｂを配置することにより、１本の発熱線で複数のガス供給管を加熱するよう構成することができる。 In particular, the heater unit 208b-1 is provided with one or a plurality of heating wires 302b for each of the plurality of gas supply pipes 232a. As in the configuration shown in FIG. 5B, in this modification, the intervals between the plurality of gas supply pipes 232a are narrow, and in such a case, it has been difficult to arrange the heating lines in the past. On the other hand, according to this modification, the heating wire 302b is arranged in parallel to the gas supply pipe 232a, so that the gas supply pipe is heated evenly even when the interval between the gas supply pipes is narrow. Can do. Further, when the intervals between the plurality of gas supply pipes 232a are narrow, the heat generation lines 302b are arranged between the adjacent gas supply pipes 232a so that the plurality of gas supply pipes are heated by one heat generation line. Can do.
　また、ガス供給管温度測定センサ３０４ｂは、複数のガス供給管２３２ａの少なくとも１本に対して設けられるが、複数のガス供給管２３２ａそれぞれに対して設けてもよい。 The gas supply pipe temperature measurement sensor 304b is provided for at least one of the plurality of gas supply pipes 232a, but may be provided for each of the plurality of gas supply pipes 232a.
（ヒータユニット２０８ｃ）
　ヒータユニット２０８ｃ及びその周辺の構成は、ヒータユニット２０８ｂと同様である。ヒータユニット２０８ｂはガス供給管２３２ａの接続箇所を加熱する一方、ヒータユニット２０８ｃは温度センサ保護管２６３ａの接続箇所を加熱することのみが異なる。 (Heater unit 208c)
The configuration of the heater unit 208c and its periphery is the same as that of the heater unit 208b. The heater unit 208b heats the connection location of the gas supply pipe 232a, whereas the heater unit 208c differs only in heating the connection location of the temperature sensor protection pipe 263a.
（ヒータユニット２０８ｄ）
　ヒータユニット２０８ｄは、ヒータユニット２０８ａ～２０８ｃと同様に、炉口部側壁外周に沿って配設されている。ヒータユニット２０８ｄ及びその周辺の構成について、図６を参照しながら以下詳述する。 (Heater unit 208d)
Similarly to the heater units 208a to 208c, the heater unit 208d is disposed along the outer periphery of the side wall of the furnace port. The configuration of the heater unit 208d and its periphery will be described in detail below with reference to FIG.
　ヒータユニット２０８ｄは、発熱線３０２ｄ、発熱線３０２ｄを格納する格納部材３０５ａと、発熱線３０２ｄを格納しない格納部材３０５ｂ及び３０５ｃ、及び排気管２３１の外周と発熱線３０２ｄの間に、排気管２３１を覆うように設けられた均熱シート３２０を備えている。また、ヒータユニット２０８ｂにおけるガス供給管温度センサ３０４ｂと同様に、排気管２３１の近傍の温度を測定する配管温度センサとしての排気管温度センサ３０４ｄを備えることができる。 The heater unit 208d includes a heating wire 302d, a storage member 305a that stores the heating wire 302d, storage members 305b and 305c that do not store the heating wire 302d, and an exhaust pipe 231 between the outer periphery of the exhaust pipe 231 and the heating wire 302d. A soaking sheet 320 is provided so as to cover it. Further, similarly to the gas supply pipe temperature sensor 304b in the heater unit 208b, an exhaust pipe temperature sensor 304d as a pipe temperature sensor for measuring the temperature in the vicinity of the exhaust pipe 231 can be provided.
　発熱線３０２ｄは、発熱線３０２ｂと同様に、排気管２３１の近傍に配置され、且つ排気管２３１に対して平行に配置された複数本の発熱線により構成される。ここで、例えばヒータユニットの設置位置等の理由により、発熱線３０２ｄを排気管２３１の外周面の全面を取り囲むように配置できない場合がある。そこで、ヒータユニット２０８ｄは、これらの発熱線の少なくとも１本が、排気管２３１の外周面の一部のみに沿うように配置され、発熱線が配置できない残りの外周面に沿う位置には配置されない。 The heating line 302d is configured by a plurality of heating lines arranged in the vicinity of the exhaust pipe 231 and in parallel with the exhaust pipe 231 similarly to the heating line 302b. Here, for example, due to reasons such as the installation position of the heater unit, the heating wire 302d may not be disposed so as to surround the entire outer peripheral surface of the exhaust pipe 231. Therefore, the heater unit 208d is arranged so that at least one of these heat generation lines extends along only a part of the outer peripheral surface of the exhaust pipe 231 and is not disposed at a position along the remaining outer peripheral surface where the heat generation lines cannot be arranged. .
　格納部材３０５ａ～３０５ｃは、発熱線格納部３０５と同様に、低熱伝導率材料により形成されている。また、格納部材３０５ａ～３０５ｃは分割されており、排気管２３１への取り付けを容易にしている。 The storage members 305a to 305c are made of a low thermal conductivity material, similar to the heating wire storage portion 305. In addition, the storage members 305a to 305c are divided to facilitate attachment to the exhaust pipe 231.
　均熱シート３２０は、排気管２３１の外周面の一部のみに沿うように配置された発熱線３０２ｄからの熱を外周面の全体に伝導させて、排気管２３１の外周面を均等に加熱するように設けられている。 The soaking sheet 320 conducts heat from the heating wire 302d disposed along only a part of the outer peripheral surface of the exhaust pipe 231 to the entire outer peripheral surface, and uniformly heats the outer peripheral surface of the exhaust pipe 231. It is provided as follows.
　均熱シート３２０は、図７に示すように、アルミナクロス等の材料で構成された絶縁材３２１の内部に、アルミニウムシート等の材料で構成された高熱伝導材３２２と、カーボンシート等の材料で構成されたクッション材３２３とが積層されて配置された構造を有している。高熱伝導材３２２は発熱線３０２ｄに近い側に配置され、発熱線３０２ｄの熱を排気管２３１の外周方向全体に均等に伝導させる。クッション材３２３は排気管２３１に近い側に配置され、均熱シート３２０を排気管２３１の外周面に密着させる。均熱シート３２０の厚さは３～５ｍｍ程度である。 As shown in FIG. 7, the soaking sheet 320 is made of an insulating material 321 made of a material such as alumina cloth, a high heat conductive material 322 made of a material such as an aluminum sheet, and a material such as a carbon sheet. The structured cushioning material 323 is laminated and disposed. The high heat conductive material 322 is disposed on the side close to the heating wire 302d, and conducts the heat of the heating wire 302d evenly in the entire outer circumferential direction of the exhaust pipe 231. The cushion material 323 is disposed on the side close to the exhaust pipe 231, and causes the soaking sheet 320 to adhere to the outer peripheral surface of the exhaust pipe 231. The thickness of the soaking sheet 320 is about 3 to 5 mm.
　均熱シート３２０を設けることにより、発熱線３０２ｄに面した排気管２３１の外周面において局所的な高温部が発生するのを抑制し、発熱線３０２ｄが配置されていない排気管２３１の外周面において局所的な低温部が発生するのを抑制することができる。 By providing the soaking sheet 320, local high temperature portions are suppressed from being generated on the outer peripheral surface of the exhaust pipe 231 facing the heating line 302d, and on the outer peripheral surface of the exhaust pipe 231 where the heating line 302d is not disposed. Generation of a local low temperature part can be suppressed.
　ヒータ電源ユニット２１０から発熱線３０２ｄへ供給される電力は、主に排気管温度センサや、他のヒータユニットに設けられた側壁温度センサの測定温度に基づいて、コントローラ１２１により制御される。 The electric power supplied from the heater power supply unit 210 to the heating wire 302d is controlled by the controller 121 mainly based on the measured temperature of the exhaust pipe temperature sensor or the side wall temperature sensor provided in another heater unit.
（側壁温度センサの取り付け構造）
　側壁温度センサ３０３ａの温度測定センサ部である先端部は、図８に示す構造により、炉口部側壁に押し付けられるように接触している。ヒータカバー３０６には固定部材３０９が固定されており、側壁温度センサ３０３ａの突出部と固定部材３０９の間には、弾性部材であるバネ３１０が設けられている。バネ３１０は固定部材３０９を支点として、側壁温度センサ３０３ａを反応管２０３の側壁に押付けるように構成されている。なお、側壁温度センサ３０３ｂも同様の構造により設置されている。 (Side wall temperature sensor mounting structure)
The tip part which is the temperature measurement sensor part of the side wall temperature sensor 303a is in contact with the furnace port part side wall by the structure shown in FIG. A fixing member 309 is fixed to the heater cover 306, and a spring 310, which is an elastic member, is provided between the protruding portion of the side wall temperature sensor 303a and the fixing member 309. The spring 310 is configured to press the side wall temperature sensor 303a against the side wall of the reaction tube 203 with the fixing member 309 as a fulcrum. The side wall temperature sensor 303b is also installed with a similar structure.
（側壁温度センサの設置位置）
　ヒータユニット２０８ａが設置されている反応管２０３側壁の平坦部領域は、ヒータユニット２０８ｂ,２０８ｃ,２０８ｄが設置されている突出部領域よりも高温になり易く、逆に突出部領域は、平坦部領域よりも低温になり易い傾向がある。これは、平坦部領域ではガス供給管２３２ａ等の突出部からの熱逃げが起こりにくいことや、突出部領域では発熱線３０１ｂや３０１ｃ等が配置される面積が限られるため、高さ方向における均等な加熱が難しいことなどが理由としてある。 (Installation position of side wall temperature sensor)
The flat region on the side wall of the reaction tube 203 where the heater unit 208a is installed is likely to be hotter than the projecting region where the heater units 208b, 208c and 208d are installed, and conversely, the projecting region is a flat region. The temperature tends to be lower than that. This is because heat escape from the protruding portion such as the gas supply pipe 232a hardly occurs in the flat portion region, and the area in which the heating lines 301b and 301c are arranged in the protruding portion region is uniform. The reason is that it is difficult to heat properly.
　本実施形態では、最も長い平坦部領域を加熱するヒータユニット２０８ａに側壁温度センサ３０３ａを設け、ヒータ２０８ａと対向する位置に配置されたヒータユニット２０８ａ´に側壁温度センサ３０３ａ´を設け、突出部領域を加熱するヒータユニット２０８ｂ´に側壁温度センサ３０３ｂを設けている。 In the present embodiment, the side wall temperature sensor 303a is provided in the heater unit 208a that heats the longest flat portion region, the side wall temperature sensor 303a ′ is provided in the heater unit 208a ′ disposed at a position facing the heater 208a, and the protruding portion region is provided. A side wall temperature sensor 303b is provided in the heater unit 208b ′ for heating the heater.
　反応管２０３の外周方向において互いに離間した位置をヒータ制御点として、これらの位置に各側壁温度センサを配置しているため、それぞれで測定された温度に基づいて、反応管２０３の側壁の温度が外周方向において均等になるように、ヒータユニット２０８ａ～２０８ｄを個別に制御することができる。 Since the side wall temperature sensors are arranged at these positions with heater control points at positions separated from each other in the outer peripheral direction of the reaction tube 203, the temperature of the side wall of the reaction tube 203 is determined based on the temperature measured at each position. The heater units 208a to 208d can be individually controlled so as to be uniform in the outer circumferential direction.
　ここで、ヒータユニット２０８ａ～２０８ｄを個別に制御する際に、高温になり易い平坦部領域の温度を測定する側壁温度センサ３０３ａ，３０３ａ´により測定される温度の目標値（第１目標温度）は、低温になり易い突出部領域の温度を測定する側壁温度センサ３０３ｂにより測定される温度の目標値（第２目標温度）よりも低く設定することが好ましい。これにより、反応管２０３の側壁の温度が外周方向において均等になるようにヒータ２０８を制御することが容易になる。 Here, when individually controlling the heater units 208a to 208d, the target temperature value (first target temperature) measured by the side wall temperature sensors 303a and 303a ′ for measuring the temperature of the flat portion region that is likely to become high is as follows. It is preferable to set the temperature lower than the target value (second target temperature) of the temperature measured by the side wall temperature sensor 303b that measures the temperature of the protruding region that tends to be low. This makes it easy to control the heater 208 so that the temperature of the side wall of the reaction tube 203 is uniform in the outer circumferential direction.
　さらに、平坦部領域の温度を測定する側壁温度センサ３０３ａ，３０３ａ´により測定された温度が所定の温度（例えば後述する第１上限温度）を超えないように、主にヒータユニット２０８ａ，２０８ａ´を制御することにより、炉口周辺の側壁において局所的な高温領域が発生することを防ぐことが容易になる。 Further, the heater units 208a and 208a ′ are mainly arranged so that the temperature measured by the side wall temperature sensors 303a and 303a ′ that measure the temperature of the flat region does not exceed a predetermined temperature (for example, a first upper limit temperature described later). By controlling, it becomes easy to prevent a local high temperature region from being generated on the side wall around the furnace port.
　また、突出部領域の温度を測定する側壁温度センサ３０３ｂにより測定された温度が所定の温度（例えば後述する第１下限温度）未満とならないように、主にヒータユニット２０８ｂ´を制御することにより、炉口周辺の側壁において局所的な低温領域が発生することを防ぐことが容易になる。 Further, mainly by controlling the heater unit 208b ′ so that the temperature measured by the side wall temperature sensor 303b that measures the temperature of the protruding region does not become lower than a predetermined temperature (for example, a first lower limit temperature described later), It becomes easy to prevent a local low temperature region from occurring on the side wall around the furnace port.
　したがって、反応管２０３の側壁の温度が外周方向において所定の温度範囲（例えば第１下限温度以上、第１上限温度以下）になるように、ヒータ２０８を制御することをより容易にすることができる。 Therefore, it is possible to more easily control the heater 208 so that the temperature of the side wall of the reaction tube 203 falls within a predetermined temperature range (for example, the first lower limit temperature or higher and the first upper limit temperature or lower) in the outer peripheral direction. .
　なお、本実施形態では側壁温度センサを３個設けているが、ヒータユニット２０８ａが配置される平坦部領域と、ヒータユニット２０８ｂ～２０８ｄが配置される突出部領域のそれぞれに少なくとも１個ずつ側壁温度センサを設けることによって、上述の効果を得ることができる。ただし、反応管２０３の側壁の温度を外周方向においてより均等に近づけるためには、側壁温度センサは３個以上設けることが望ましい。 In this embodiment, three sidewall temperature sensors are provided. However, at least one sidewall temperature sensor is provided for each of the flat region where the heater unit 208a is disposed and the protruding region where the heater units 208b to 208d are disposed. By providing the sensor, the above-described effects can be obtained. However, in order to bring the temperature of the side wall of the reaction tube 203 closer to each other in the outer circumferential direction, it is desirable to provide three or more side wall temperature sensors.
（ヒータユニット間の接続構造）
　ヒータユニット２０８ａ～２０８ｄは互いに、図９に示すようなクランク状の端面が組み合わされる構造により接続されている。また、ヒータユニット２０８ａ～２０８ｄの接続箇所の外周面は、ＳＵＳ等の材料で構成された保護カバー３３０によりカバー（被覆）される。このような接続構造を有することにより、ヒータ２０８と反応管２０３の側壁との間の空間（内周空間）の雰囲気がヒータ２０８の外周側に漏れることを防止し、内周空間と外周側との間の気流置換による温度低下を最小限にすることができる。なお、各ヒータユニットの端面の形状はクランク状に限らず、凸形状と凹形状の組合せなど、端面に凹凸が形成された形状の組合せであればよい。 (Connection structure between heater units)
The heater units 208a to 208d are connected to each other by a structure in which crank-shaped end faces are combined as shown in FIG. In addition, the outer peripheral surfaces of the connection portions of the heater units 208a to 208d are covered (covered) with a protective cover 330 made of a material such as SUS. By having such a connection structure, the atmosphere in the space (inner peripheral space) between the heater 208 and the side wall of the reaction tube 203 is prevented from leaking to the outer peripheral side of the heater 208, and the inner peripheral space and the outer peripheral side The temperature drop due to the air flow replacement during the period can be minimized. Note that the shape of the end face of each heater unit is not limited to the crank shape, and may be a combination of shapes in which irregularities are formed on the end face, such as a combination of a convex shape and a concave shape.
　図２に示すように、制御部であるコントローラ１２１は、ＣＰＵ１２１ａ、ＲＡＭ１２１ｂ、記憶装置１２１ｃ、Ｉ／Ｏポート１２１ｄを備えたコンピュータとして構成されている。ＲＡＭ１２１ｂ、記憶装置１２１ｃ、Ｉ／Ｏポート１２１ｄは、内部バス１２１ｅを介してＣＰＵ１２１ａとデータ交換可能なように構成されている。コントローラ１２１には、タッチパネル等として構成された入出力装置１２２が接続されている。 As shown in FIG. 2, the controller 121 as a control unit is configured as a computer including a CPU 121a, a RAM 121b, a storage device 121c, and an I / O port 121d. The RAM 121b, the storage device 121c, and the I / O port 121d are configured to exchange data with the CPU 121a via the internal bus 121e. An input / output device 122 configured as a touch panel or the like is connected to the controller 121.
　記憶装置１２１ｃはフラッシュメモリやＨＤＤ等により構成されている。記憶装置１２１ｃ内には、基板処理装置の動作を制御する制御プログラムや、後述する基板処理の手順や条件が記載されたプロセスレシピ等が、読み出し可能に格納されている。プロセスレシピは、後述する各手順をコントローラ１２１に実行させ、所定の結果を得ることが出来るように組み合わされたものであり、プログラムとして機能する。以下、このプロセスレシピや制御プログラム等を総称して、単に、プログラムともいう。また、プロセスレシピを、単に、レシピともいう。本明細書においてプログラムという言葉を用いた場合は、レシピ単体のみを含む場合、制御プログラム単体のみを含む場合、または、それらの両方を含む場合がある。ＲＡＭ１２１ｂは、ＣＰＵ１２１ａによって読み出されたプログラムやデータ等が一時的に保持されるメモリ領域として構成されている。 The storage device 121c is configured by a flash memory, an HDD, or the like. In the storage device 121c, a control program that controls the operation of the substrate processing apparatus, a process recipe that describes the procedure and conditions of the substrate processing described later, and the like are stored in a readable manner. The process recipe is a combination of functions so that a predetermined result can be obtained by causing the controller 121 to execute each procedure described later, and functions as a program. Hereinafter, the process recipe, the control program, and the like are collectively referred to simply as a program. The process recipe is also simply called a recipe. When the term “program” is used in this specification, it may include only a recipe, only a control program, or both. The RAM 121b is configured as a memory area that temporarily stores programs, data, and the like read by the CPU 121a.
　Ｉ／Ｏポート１２１ｄは、上述のＭＦＣ２４１ａ、バルブ２４３ａ、ガス発生器２５０ａ、圧力センサ２４５、ＡＰＣバルブ２４４、真空ポンプ２４６、ヒータ電源ユニット２１０、温度センサ２６３、側壁温度センサ３０３ａ，３０３ｂ、ガス供給管温度センサ３０４ｂ、排気管温度センサ３０４ｄ、回転機構２６７、ボートエレベータ１１５等に接続されている。 The I / O port 121d includes the MFC 241a, the valve 243a, the gas generator 250a, the pressure sensor 245, the APC valve 244, the vacuum pump 246, the heater power supply unit 210, the temperature sensor 263, the side wall temperature sensors 303a and 303b, and the gas supply pipe. The temperature sensor 304b, the exhaust pipe temperature sensor 304d, the rotation mechanism 267, the boat elevator 115, and the like are connected.
　ＣＰＵ１２１ａは、記憶装置１２１ｃから制御プログラムを読み出して実行すると共に、入出力装置１２２からの操作コマンドの入力等に応じて記憶装置１２１ｃからレシピを読み出すように構成されている。ＣＰＵ１２１ａは、読み出したレシピの内容に沿うように、ガス発生器２５０ａによるガス生成動作、ＭＦＣ２４１ａによるガスの流量調整動作、バルブ２４３ａの開閉動作、圧力センサ２４５に基づくＡＰＣバルブ２４４による圧力調整動作、真空ポンプ２４６の起動および停止、温度センサ２６３、側壁温度センサ３０３ａ，３０３ｂ、ガス供給管温度センサ３０４ｂ、排気管温度センサ３０４ｄに基づくヒータ電源ユニット２１０からヒータ２０７，２０８，キャップヒータ２０９への電力供給量の調整動作、回転機構２６７によるボート２１７の回転および回転速度調節動作、ボートエレベータ１１５によるボート２１７の昇降動作等を制御するように構成されている。 The CPU 121a is configured to read out and execute a control program from the storage device 121c and to read a recipe from the storage device 121c in response to an operation command input from the input / output device 122 or the like. The CPU 121a performs a gas generation operation by the gas generator 250a, a gas flow rate adjustment operation by the MFC 241a, an opening / closing operation of the valve 243a, a pressure adjustment operation by the APC valve 244 based on the pressure sensor 245, and a vacuum in accordance with the contents of the read recipe. Starting and stopping of pump 246, temperature sensor 263, side wall temperature sensors 303a and 303b, gas supply pipe temperature sensor 304b, and exhaust pipe temperature sensor 304d, the amount of power supplied from heater power supply unit 210 to heaters 207 and 208 and cap heater 209 Adjustment operation, rotation and rotation speed adjustment operation of the boat 217 by the rotation mechanism 267, and lifting / lowering operation of the boat 217 by the boat elevator 115, and the like.
　コントローラ１２１は、外部記憶装置（例えば、ＨＤＤ等の磁気ディスク、ＣＤ等の光ディスク、ＭＯ等の光磁気ディスク、ＵＳＢメモリ等の半導体メモリ）１２３に格納された上述のプログラムを、コンピュータにインストールすることにより構成することができる。記憶装置１２１ｃや外部記憶装置１２３は、コンピュータ読み取り可能な記録媒体として構成されている。以下、これらを総称して、単に、記録媒体ともいう。本明細書において記録媒体という言葉を用いた場合は、記憶装置１２１ｃ単体のみを含む場合、外部記憶装置１２３単体のみを含む場合、または、それらの両方を含む場合がある。なお、コンピュータへのプログラムの提供は、外部記憶装置１２３を用いず、インターネットや専用回線等の通信手段を用いて行ってもよい。 The controller 121 installs the above-mentioned program stored in an external storage device (for example, a magnetic disk such as an HDD, an optical disk such as a CD, a magneto-optical disk such as an MO, or a semiconductor memory such as a USB memory) 123 in a computer. Can be configured. The storage device 121c and the external storage device 123 are configured as computer-readable recording media. Hereinafter, these are collectively referred to simply as a recording medium. When the term “recording medium” is used in this specification, it may include only the storage device 121c alone, may include only the external storage device 123 alone, or may include both of them. The program may be provided to the computer using a communication means such as the Internet or a dedicated line without using the external storage device 123.
（２）基板処理工程
　続いて、上述の基板処理装置を用い、半導体装置の製造工程の一工程として実施される基板処理工程の一例について、図１１を用いて説明する。以下の説明において、基板処理装置を構成する各部の動作は、コントローラ１２１により制御される。　なお、この基板処理工程において所定の処理が施される基板の表面には、シラザン結合（－Ｓｉ－Ｎ－）を有する膜（ポリシラザン膜）が形成されている。この膜には、シリコン（Ｓｉ）の他、窒素（Ｎ）、水素（Ｈ）が含まれ、さらに、炭素（Ｃ）や他の不純物が混ざっている場合がある。この基板処理工程では、ウエハ２００上に形成されたポリシラザン膜に対し、比較的低温の条件下でＨ２Ｏ２を含む気化ガスを供給することで、この膜を改質（酸化）する。 (2) Substrate Processing Step Next, an example of a substrate processing step performed as one step of a semiconductor device manufacturing process using the above-described substrate processing apparatus will be described with reference to FIG. In the following description, the operation of each part constituting the substrate processing apparatus is controlled by the controller 121. Note that a film having a silazane bond (—Si—N—) (polysilazane film) is formed on the surface of the substrate that is subjected to predetermined processing in the substrate processing step. In addition to silicon (Si), this film contains nitrogen (N) and hydrogen (H), and may further contain carbon (C) and other impurities. In this substrate processing step, the polysilazane film formed on the wafer 200 is modified (oxidized) by supplying a vaporized gas containing H 2 O 2 under a relatively low temperature condition.
（基板搬入工程）
　表面にポリシラザン膜が形成された複数枚のウエハ２００が、ボート２１７に装填される。その後、図１に示すように、複数枚のウエハ２００を支持したボート２１７は、ボートエレベータ１１５によって持ち上げられて処理室２０１内へ搬入される。この状態で、シールキャップ２１９は、Ｏリング２２０ａを介して反応管２０３の下端をシールした状態となる。 (Substrate loading process)
A plurality of wafers 200 having a polysilazane film formed on the surface are loaded into a boat 217. Thereafter, as shown in FIG. 1, the boat 217 that supports the plurality of wafers 200 is lifted by the boat elevator 115 and carried into the processing chamber 201. In this state, the seal cap 219 is in a state of sealing the lower end of the reaction tube 203 via the O-ring 220a.
（圧力・温度調整工程）
　処理室２０１内、すなわち、ウエハ２００が存在する空間が所定の圧力（改質圧力）となるように、真空ポンプ２４６によって処理室２０１内が真空排気される。また、ヒータ２０７，２０８、キャップヒータ２０９により、反応管２０３、処理室２０１に収容されたウエハ２００、シールキャップ２１９、等が加熱される。 (Pressure / temperature adjustment process)
The inside of the processing chamber 201 is evacuated by the vacuum pump 246 so that the space in which the wafer 200 exists, that is, the space where the wafer 200 exists becomes a predetermined pressure (reforming pressure). Further, the reaction tube 203, the wafer 200 accommodated in the processing chamber 201, the seal cap 219, and the like are heated by the heaters 207 and 208 and the cap heater 209.
　この際、領域Ａに収容されたウエハ２００が所定の温度となるように、温度センサ２６３が検出した温度情報に基づいて、ヒータ電源ユニット２１０からヒータ２０７への通電具合がフィードバック制御される。 At this time, the state of energization from the heater power supply unit 210 to the heater 207 is feedback controlled based on the temperature information detected by the temperature sensor 263 so that the wafer 200 accommodated in the region A has a predetermined temperature.
　また、ヒータ２０８に設けられた温度センサ（側壁温度センサ３０３ａ，３０３ｂ、ガス供給管温度センサ３０４ｂ、排気管温度センサ３０４ｄ）が検出した温度情報に基づいて、反応管２０３の炉口部の側壁の温度と、ガス供給管２３２ａ、温度センサ保護管２６３ａ及び排気管２３１の温度とがそれぞれ所定の温度（又は所定の温度分布）となるように、ヒータ電源ユニット２１０からヒータユニット２０８ａ～２０８ｄそれぞれへの通電具合がフィードバック制御される。 Further, based on the temperature information detected by the temperature sensors (side wall temperature sensors 303a and 303b, gas supply pipe temperature sensor 304b, and exhaust pipe temperature sensor 304d) provided in the heater 208, the side wall of the furnace port portion of the reaction tube 203 is detected. From the heater power supply unit 210 to each of the heater units 208a to 208d, the temperature and the temperature of the gas supply pipe 232a, the temperature sensor protection pipe 263a, and the exhaust pipe 231 are each set to a predetermined temperature (or a predetermined temperature distribution). The state of energization is feedback controlled.
　ヒータ２０７，２０８のフィードバック制御は、少なくともウエハ２００に対する処理が終了するまでの間は継続して行われる。また、回転機構２６７によるウエハ２００の回転を開始する。真空ポンプ２４６の稼働、ウエハ２００の加熱および回転は、いずれも、少なくとも、ウエハ２００に対する処理が終了するまでの間は継続して行われる。 The feedback control of the heaters 207 and 208 is continuously performed at least until the processing on the wafer 200 is completed. Further, the rotation of the wafer 200 by the rotation mechanism 267 is started. The operation of the vacuum pump 246 and the heating and rotation of the wafer 200 are continuously performed at least until the processing on the wafer 200 is completed.
（改質工程）
　続いて、ガス発生器２５０ａへの液体原料及びキャリアガスの供給を開始し、ガス発生器２５０ａによりＨ２Ｏ２ガスおよびＨ２Ｏガスを含む気化ガスを発生させる。気化ガスの発生量や濃度等が安定したら、バルブ２４３ａを開き、ＭＦＣ２４１ａにより流量制御しながら、ガス供給ポート２３２ｐを介した処理室２０１内への気化ガスの供給を開始する。処理室２０１内へ供給された気化ガスは、排気管２３１から排気される。このとき、ウエハ２００に対して気化ガスが供給される。その結果、ウエハ２００の表面で酸化反応が生じ、ウエハ２００上のポリシラザン膜は、シリコン酸化膜（ＳｉＯ膜）へと改質される。 (Reforming process)
Then, to start the supply of the liquid raw material and the carrier gas to the gas generator 250a, to generate a vaporized gas containing H 2 O 2 gas and H 2 O gas by the gas generator 250a. When the amount and concentration of vaporized gas are stabilized, supply of vaporized gas into the processing chamber 201 via the gas supply port 232p is started while the valve 243a is opened and the flow rate is controlled by the MFC 241a. The vaporized gas supplied into the processing chamber 201 is exhausted from the exhaust pipe 231. At this time, vaporized gas is supplied to the wafer 200. As a result, an oxidation reaction occurs on the surface of the wafer 200, and the polysilazane film on the wafer 200 is modified into a silicon oxide film (SiO film).
　所定時間が経過し、ポリシラザン膜のＳｉＯ膜への改質が終了したら、バルブ２４３ａを閉じ、処理室２０１内への気化ガスの供給を停止する。 When the predetermined time has elapsed and the modification of the polysilazane film to the SiO film is completed, the valve 243a is closed and the supply of the vaporized gas into the processing chamber 201 is stopped.
　改質工程の処理条件としては、以下が例示される。
　液体原料のＨ２Ｏ２濃度：２０～４０％、好ましくは２５～３５％
　液体原料の気化条件：略大気圧下で１２０～２００℃に加熱
　改質圧力：７００～１０００ｈＰａ（大気圧、微減圧および微加圧のうちいずれか）
　ウエハ２００の温度：７０～１１０℃、好ましくは７０～８０℃ Examples of the processing conditions for the reforming step include the following.
H 2 O 2 concentration of liquid raw material: 20 to 40%, preferably 25 to 35%
Liquid raw material vaporization conditions: Heated to 120 to 200 ° C. at approximately atmospheric pressure Reforming pressure: 700 to 1000 hPa (any of atmospheric pressure, slightly reduced pressure, and slightly increased pressure)
Wafer 200 temperature: 70 to 110 ° C., preferably 70 to 80 ° C.
　ここで述べた温度条件下では、処理室２０１内へ供給された気化ガスが処理室２０１内で再液化し、これにより生じた液体が炉口周辺（シールキャップ２１９の上面等）に滞留する可能性がある。特に、炉口部側壁や、処理室２０１内のガス供給管２３２ａ、温度センサ保護管２６３ａ等では、上述の通り、局所的な低温領域が生じることがあり、局所的に発生した低温領域に接触することで気化ガスが再液化しやすい。 Under the temperature conditions described here, the vaporized gas supplied into the processing chamber 201 is liquefied in the processing chamber 201, and the liquid thus generated can stay around the furnace port (such as the upper surface of the seal cap 219). There is sex. In particular, in the side wall of the furnace port, the gas supply pipe 232a in the processing chamber 201, the temperature sensor protection pipe 263a, and the like, a local low temperature region may be generated as described above, and the locally generated low temperature region is contacted. By doing so, the vaporized gas tends to re-liquefy.
　本実施形態では、上述の通り構成されたヒータ２０８を制御することにより、反応管２０３の炉口の側壁等を均等に加熱し、局所的な低温領域が生じるのを防止する。ここで、再液化を防止するため、炉口周辺の側壁等において、所定温度（第１下限温度）を下回る領域が発生しないように温度制御を行う。下限温度は気化ガスの濃度等の条件により異なるが、例えば上述の処理条件においては８０℃以上である。 In this embodiment, by controlling the heater 208 configured as described above, the side wall of the furnace port of the reaction tube 203 and the like are heated evenly, and a local low temperature region is prevented from being generated. Here, in order to prevent reliquefaction, temperature control is performed so that a region below a predetermined temperature (first lower limit temperature) does not occur on the side wall and the like around the furnace port. The lower limit temperature varies depending on conditions such as the concentration of vaporized gas, but is, for example, 80 ° C. or higher under the above-described processing conditions.
　また、気化ガスの再液化によって生じた液体は、Ｈ２Ｏ２が高濃度に濃縮された状態、すなわち、高濃度Ｈ２Ｏ２液となる傾向がある。また、滞留した高濃度Ｈ２Ｏ２液は、Ｈ２Ｏ２がさらに高濃度に濃縮された状態に変化する傾向がある。高濃度Ｈ２Ｏ２液は、非常に反応性が高く、強力な腐食作用を有することから、炉口部の部材に深刻なダメージを与える可能性がある。 Further, the liquid generated by re-liquefaction of the vaporized gas tends to be in a state where H 2 O 2 is concentrated to a high concentration, that is, a high concentration H 2 O 2 solution. Further, the retained high concentration H 2 O 2 liquid tends to change to a state in which H 2 O 2 is further concentrated to a higher concentration. The high-concentration H 2 O 2 liquid is very reactive and has a strong corrosive action, which may cause serious damage to the furnace port member.
　また、炉口付近に滞留した高濃度Ｈ２Ｏ２液が何らかの要因で再気化した場合、これにより発生した再気化ガスはＨ２Ｏ２を非常に高濃度に含むガスとなり、作業の安全性をさらに脅かす可能性がある。例えば、再気化ガスに含まれるＨ２Ｏ２の濃度が大気圧下において２６モル％を超える状態では、高濃度Ｈ２Ｏ２液に含まれるＨ２Ｏ２がＯ２ガスとＨ２Ｏガスとに急激に分解して膨張し、上述の爆発的分解反応を引き起こす懸念もある。 Further, when the high concentration H 2 O 2 liquid staying in the vicinity of the furnace port is re-vaporized for some reason, the re-vaporized gas generated thereby becomes a gas containing H 2 O 2 at a very high concentration, and the safety of the work. May further threaten. For example, in the state in which the concentration of H 2 O 2 contained in the re-vaporized gas is more than 26 mol% under atmospheric pressure, H 2 O 2 is O 2 gas and the H 2 O gas contained in the high concentration H 2 O 2 solution There is also a concern that it rapidly decomposes and expands to cause the above-mentioned explosive decomposition reaction.
　ここで、爆発的分解反応とは、Ｈ２Ｏ２を含む液体が酸素ガス（Ｏ２）と水蒸気（Ｈ２Ｏ）とに急激に分解して膨張し、爆発や燃焼、或いは、これらに近い現象を起こすことである。爆発的分解反応は、あるＨ２Ｏ２液の濃度及び圧力において、Ｈ２Ｏ２液が決まった温度（爆発臨界温度）を超えた場合に起こり得る。そのため、再液化により滞留した高濃度Ｈ２Ｏ２液は、爆発臨界温度を超えないように維持されなければならない。爆発臨界温度は、高濃度Ｈ２Ｏ２液におけるＨ２Ｏ２の濃度によって変動し、具体的には、Ｈ２Ｏ２の濃度の増加に伴って低温化する。但し、爆発臨界温度の低温化は、高濃度Ｈ２Ｏ２液の濃度が１００％に到達した時点で下限となる。従って、処理圧力を大気圧とした場合、高濃度Ｈ２Ｏ２液の温度を、濃度が１００％の場合における爆発臨界温度である１１２℃未満の温度に維持することにより、爆発的分解反応の発生を確実に回避することが可能となる。 Here, the explosive decomposition reaction means that a liquid containing H 2 O 2 is rapidly decomposed into oxygen gas (O 2 ) and water vapor (H 2 O) and expands to explode, burn, or close to these. It is to cause a phenomenon. An explosive decomposition reaction can occur when the H 2 O 2 liquid exceeds a certain temperature (explosion critical temperature) at a certain H 2 O 2 liquid concentration and pressure. Therefore, the high concentration H 2 O 2 liquid retained by reliquefaction must be maintained so as not to exceed the explosion critical temperature. The explosion critical temperature varies depending on the concentration of H 2 O 2 in the high-concentration H 2 O 2 liquid, and specifically decreases as the concentration of H 2 O 2 increases. However, the lowering of the explosion critical temperature becomes the lower limit when the concentration of the high concentration H 2 O 2 liquid reaches 100%. Therefore, when the treatment pressure is atmospheric pressure, the temperature of the high concentration H 2 O 2 liquid is maintained at a temperature lower than 112 ° C., which is the explosion critical temperature when the concentration is 100%. Occurrence can be reliably avoided.
　本実施形態では、上述の通り構成されたヒータ２０８を制御することにより、反応管２０３の炉口の側壁等を均等に加熱し、局所的な高温領域が生じるのを防止する。ここで、滞留した高濃度Ｈ２Ｏ２液の爆発的分解反応の発生を防止するため、炉口周辺の側壁等において、所定温度（第１上限温度）を上回る領域が発生しないように温度制御を行う。第１上限温度は、処理圧力を大気圧とした場合、１１２℃以下とする。 In the present embodiment, by controlling the heater 208 configured as described above, the side wall and the like of the furnace port of the reaction tube 203 are evenly heated to prevent the occurrence of a local high temperature region. Here, in order to prevent the occurrence of an explosive decomposition reaction of the retained high concentration H 2 O 2 liquid, temperature control is performed so that a region exceeding a predetermined temperature (first upper limit temperature) does not occur on the side wall around the furnace port. I do. The first upper limit temperature is 112 ° C. or lower when the processing pressure is atmospheric pressure.
　また、本実施形態は、輻射による熱伝達よりも熱伝導による熱伝達の影響が大きい温度領域（すなわち１２０℃以下、より好ましくは１００℃以下の温度領域）における温度制御を行う際に適用することにより、温度制御性を高めることができる。例えば、側壁温度センサ３０３ａ等の測定温度が、これらの温度領域内となる範囲で温度制御を行うことが好ましい。また、キャップヒータ２０９による加熱制御についても、これらの温度領域内となる範囲で実施することで、ヒータ２０８による温度制御性を維持することができる。 In addition, the present embodiment is applied when performing temperature control in a temperature region (that is, a temperature region of 120 ° C. or lower, more preferably 100 ° C. or lower) in which the influence of heat transfer by heat conduction is larger than that of heat transfer by radiation. Thus, temperature controllability can be improved. For example, it is preferable to perform temperature control in a range where the measured temperature of the sidewall temperature sensor 303a or the like falls within these temperature ranges. Further, the heating control by the cap heater 209 can be maintained within the temperature range so that the temperature controllability by the heater 208 can be maintained.
（乾燥工程）
　改質工程が終了したら、ヒータ２０７を制御し、ウエハ２００を、上述の改質温度よりも高い温度に加熱する。この温度を保持することにより、ウエハ２００と処理室２０１内とを緩やかに乾燥させる。 (Drying process)
When the reforming process is completed, the heater 207 is controlled to heat the wafer 200 to a temperature higher than the above-described reforming temperature. By maintaining this temperature, the wafer 200 and the inside of the processing chamber 201 are gently dried.
（降温・大気圧復帰工程）
　乾燥工程が終了した後、処理室２０１内を真空排気する。その後、処理室２０１内を大気圧に復帰させ、所定時間経過した後、処理室２０１内を所定の搬出可能温度に降温させる。 (Cooling temperature / atmospheric pressure recovery process)
After the drying process is completed, the inside of the processing chamber 201 is evacuated. Thereafter, the inside of the processing chamber 201 is returned to atmospheric pressure, and after a predetermined time has elapsed, the inside of the processing chamber 201 is lowered to a predetermined unloadable temperature.
（基板搬出工程）
　ボートエレベータ１１５によりシールキャップ２１９が下降され、反応管２０３の下端が開口される。そして、処理済のウエハ２００が反応管２０３の下端から反応管２０３の外部に搬出される。 (Substrate unloading process)
The seal cap 219 is lowered by the boat elevator 115 and the lower end of the reaction tube 203 is opened. Then, the processed wafer 200 is unloaded from the lower end of the reaction tube 203 to the outside of the reaction tube 203.
（３）実施例
　本実施形態の実施例と比較例について以下説明する。実施例として、本実施形態におけるヒータ２０８の温度制御を行い、図１２に示す温度モニタ点Ａ～Ｎにおける温度を測定した。モニタ点Ａ～Ｈは上面ベース２１９ａ上の点であり、モニタ点Ｉ～Ｎは炉口周辺の側壁の外周面上の点である。一方、比較例として、本実施形態のヒータ２０８に替えて以下に示す構成を有するヒータにより温度制御を行い、実施例と同様に、温度モニタ点Ａ，Ｂ，Ｅ，Ｆ，Ｉ，Ｋ，Ｌ，Ｎにおける温度を測定した。なお、実施例及び比較例のいずれについても、モニタ点Ａ～Ｈにおける目標温度を８０～１１２℃に設定し制御を行った。 (3) Example An example of the present embodiment and a comparative example will be described below. As an example, the temperature of the heater 208 in this embodiment was controlled, and the temperatures at the temperature monitoring points A to N shown in FIG. 12 were measured. Monitor points A to H are points on the upper surface base 219a, and monitor points I to N are points on the outer peripheral surface of the side wall around the furnace port. On the other hand, as a comparative example, temperature control is performed by a heater having the following configuration in place of the heater 208 of the present embodiment, and temperature monitoring points A, B, E, F, I, K, L are performed in the same manner as in the examples. , N were measured. In both the examples and comparative examples, the control was performed by setting the target temperature at the monitor points A to H to 80 to 112 ° C.
　比較例における基板処理装置は、図１３に示すように、炉口周辺の側壁を加熱するヒータ４００と、ガス供給管２３２ａ等の突出部を加熱するジャケットヒータ４０１を備えている。ヒータ４００は本実施形態の側壁温度センサ３０３ａ等を備えておらず、ヒータ出力のみにより温度制御を行うよう構成されている。ジャケットヒータ４０１は、ガス供給管２３２ａ等の突出部それぞれに巻き付けるように設置され、主に突出部のみを加熱することを目的として設けられている。 As shown in FIG. 13, the substrate processing apparatus in the comparative example includes a heater 400 that heats the side wall around the furnace port, and a jacket heater 401 that heats the protruding portion such as the gas supply pipe 232a. The heater 400 does not include the side wall temperature sensor 303a of this embodiment, and is configured to perform temperature control only by the heater output. The jacket heater 401 is installed so as to be wound around each protrusion such as the gas supply pipe 232a, and is mainly provided for the purpose of heating only the protrusion.
　図１４に、実施例と比較例それぞれにおけるモニタ点Ａ～Ｎにおける温度の測定結果を示す。比較例においては、特に突出部からの距離が大きいモニタ点ＡやＩにおいて、局所的な高温領域の発生が特に顕著にみられた。また、他のモニタ点においても第１上限温度としての１１２℃を超える結果となった。これに対して実施例においては、全てのモニタ点において、第１下限温度としての８０℃以上、且つ第１上限温度としての１１２℃以下の温度範囲を実現することができた。 FIG. 14 shows the measurement results of the temperatures at the monitor points A to N in the example and the comparative example. In the comparative example, the occurrence of a local high temperature region was particularly noticeable particularly at the monitor points A and I having a large distance from the protruding portion. Further, at other monitor points, the result exceeded 112 ° C. as the first upper limit temperature. On the other hand, in the example, it was possible to realize a temperature range of 80 ° C. or more as the first lower limit temperature and 112 ° C. or less as the first upper limit temperature at all monitor points.
＜本発明の他の実施形態＞
　以上、本発明の実施形態を具体的に説明したが、本発明は上述の実施形態に限定されるものではなく、その要旨を逸脱しない範囲で種々変更可能である。 <Other Embodiments of the Present Invention>
As mentioned above, although embodiment of this invention was described concretely, this invention is not limited to the above-mentioned embodiment, It can change variously in the range which does not deviate from the summary.
　上述の実施形態では、ポリシラザン膜が形成された基板を処理する例を示したが、本発明はこれに限定されない。すなわち、処理対象の膜がポリシラザン膜でなくとも、上述の実施形態と同様の効果が得られる。 In the above-described embodiment, an example in which a substrate on which a polysilazane film is formed is processed, but the present invention is not limited to this. That is, even if the film to be processed is not a polysilazane film, the same effect as that of the above-described embodiment can be obtained.
　上述の実施形態や変形例等は、適宜組み合わせて用いることができる。また、このときの処理手順、処理条件は、例えば上述の実施形態と同様な処理手順、処理条件とすることができる。 The above-described embodiments and modifications can be used in appropriate combination. In addition, the processing procedure and processing conditions at this time can be the same processing procedure and processing conditions as in the above-described embodiment, for example.
　本発明によれば、処理室を形成する部材の温度に局所的な偏りが生じることを防止するように加熱を行うことが可能な技術を提供することが可能となる。 According to the present invention, it is possible to provide a technique capable of performing heating so as to prevent local deviation in the temperature of the members forming the processing chamber.
　２００　ウエハ（基板）
　２０３　反応管
　２０８　ヒータ
　２３２ａ　ガス供給管
　１２１　コントローラ
  200 wafer (substrate)
203 reaction tube 208 heater 232a gas supply tube 121 controller

Claims (18)

  1. 基板を収容する反応管と、
    前記反応管に形成された炉口を閉塞する蓋部と、
    前記反応管の炉口近傍の側壁の外周に設けられたヒータと、
    前記反応管の炉口近傍の側壁における、前記側壁の周方向において互いに異なる複数の位置の温度をそれぞれ測定するよう構成された複数の温度センサと、
    前記複数の温度センサのそれぞれの測定値に基づいて、前記ヒータを制御するよう構成された制御部と、
    を備える基板処理装置。     A reaction tube containing a substrate;
    A lid for closing the furnace port formed in the reaction tube;
    A heater provided on the outer periphery of the side wall near the furnace port of the reaction tube;
    A plurality of temperature sensors configured to respectively measure temperatures at a plurality of positions different from each other in the circumferential direction of the side wall in the side wall near the furnace port of the reaction tube;
    A control unit configured to control the heater based on the measured values of the plurality of temperature sensors;
    A substrate processing apparatus comprising:
  2. 前記ヒータは、
    前記側壁の周方向において分割された複数のヒータユニットによって構成されている、
    請求項１記載の基板処理装置。     The heater is
    It is constituted by a plurality of heater units divided in the circumferential direction of the side wall.
    The substrate processing apparatus according to claim 1.
  3. 前記反応管の炉口近傍の側壁に接続する配管を備え、
    前記複数のヒータユニットの少なくとも1つは、前記反応管の炉口近傍の側壁の一部であって前記配管が接続された箇所の周辺部分及び前記配管を、共に加熱するように構成された第１のヒータユニットであり、
    前記複数のヒータユニットの少なくとも他の1つは、前記反応管の炉口近傍の側壁の一部であって前記配管が接続されていない部分を加熱するように構成された第２のヒータユニットである、
    請求項２記載の基板処理装置。     A pipe connected to the side wall near the furnace port of the reaction tube,
    At least one of the plurality of heater units is a part of a side wall in the vicinity of the furnace port of the reaction tube and is configured to heat both a peripheral portion of the place where the pipe is connected and the pipe. 1 heater unit,
    At least another one of the plurality of heater units is a second heater unit configured to heat a part of the side wall in the vicinity of the furnace port of the reaction tube that is not connected to the pipe. is there,
    The substrate processing apparatus according to claim 2.
  4. 前記制御部は、
    前記第１のヒータユニットと前記第２のヒータユニットとへ供給される電力をそれぞれ個別に制御して、前記反応管の炉口近傍の側壁及び前記配管を加熱させるよう構成される、
    請求項３記載の基板処理装置。     The controller is
    The power supplied to the first heater unit and the second heater unit is individually controlled to heat the side wall near the furnace port of the reaction tube and the pipe.
    The substrate processing apparatus according to claim 3.
  5. 前記複数の温度センサは、
    前記第１のヒータユニットにより加熱される前記反応管の側壁の部分の温度を測定するよう構成された第１の温度センサと、
    前記第２のヒータユニットにより加熱される前記反応管の側壁の部分の温度を測定するよう構成された第２の温度センサと、を含む、
    請求項３記載の基板処理装置。     The plurality of temperature sensors are:
    A first temperature sensor configured to measure the temperature of the side wall portion of the reaction tube heated by the first heater unit;
    A second temperature sensor configured to measure the temperature of the side wall portion of the reaction tube heated by the second heater unit;
    The substrate processing apparatus according to claim 3.
  6. 前記制御部は、
    前記第１の温度センサの測定値が第１温度となるように、前記第１のヒータユニットに供給される電力を制御し、
    前記第２の温度センサの測定値が前記第１温度よりも低い第２温度となるように、前記第２のヒータユニットに供給される電力を制御する、よう構成される、
    請求項５記載の基板処理装置。     The controller is
    Controlling the electric power supplied to the first heater unit so that the measured value of the first temperature sensor becomes the first temperature;
    The power supplied to the second heater unit is controlled so that the measured value of the second temperature sensor becomes a second temperature lower than the first temperature.
    The substrate processing apparatus according to claim 5.
  7. 前記第１のヒータユニットは、
    複数の前記配管、及び前記反応管の炉口近傍の側壁の一部であって前記複数の配管のそれぞれが接続される箇所の周辺部分を、共に加熱するように構成されている、
    請求項３記載の基板処理装置。     The first heater unit includes:
    A plurality of the pipes and a part of a side wall near the furnace port of the reaction tube, and a peripheral part of a portion to which each of the plurality of pipes is connected are configured to be heated together.
    The substrate processing apparatus according to claim 3.
  8. 前記配管は、
    前記反応管内に処理ガスを供給するガス供給配管、前記反応管内の雰囲気を排出するガス排気管、及び前記反応管内に挿入される温度センサを保護するように管状に構成され温度センサ保護管、より構成される群より選択される少なくとも１つである、
    請求項３記載の基板処理装置。     The piping is
    A gas supply pipe for supplying a processing gas into the reaction tube, a gas exhaust pipe for discharging the atmosphere in the reaction tube, and a temperature sensor protection tube configured in a tubular shape to protect a temperature sensor inserted into the reaction tube; At least one selected from the group consisting of:
    The substrate processing apparatus according to claim 3.
  9. 前記第１のヒータユニットは、
    前記側壁に対向するように前記側壁の周方向に沿って配置された第１の発熱線と、
    前記配管の周囲に前記配管の延伸方向に沿って配置された第２の発熱線と、を備える、
    請求項３記載の基板処理装置。     The first heater unit includes:
    A first heating wire disposed along the circumferential direction of the side wall so as to face the side wall;
    A second heating wire disposed around the pipe along the extending direction of the pipe,
    The substrate processing apparatus according to claim 3.
  10. 前記制御部は、
    前記第１の発熱線と前記第２の発熱線へ供給される電力をそれぞれ個別に制御して、前記側壁及び前記配管を加熱させるよう構成される、
    請求項９記載の基板処理装置。     The controller is
    The power supplied to the first heating wire and the second heating wire is individually controlled to heat the side wall and the pipe.
    The substrate processing apparatus according to claim 9.
  11. 前記第１のヒータユニットは、
    前記配管の温度を測定する配管温度センサを備え、
    前記制御部は、
    前記配管温度センサの測定値に基づいて前記第２の発熱線へ供給される電力を制御して、前記配管を加熱させるよう構成される、
    請求項９記載の基板処理装置。     The first heater unit includes:
    A pipe temperature sensor for measuring the temperature of the pipe;
    The controller is
    The electric power supplied to the second heating wire is controlled based on the measured value of the pipe temperature sensor, and the pipe is heated.
    The substrate processing apparatus according to claim 9.
  12. 前記第１のヒータユニットは、
    前記第２の発熱線と前記配管との間に高熱伝導率を有するシートを備えている、
    請求項９記載の基板処理装置。     The first heater unit includes:
    A sheet having high thermal conductivity is provided between the second heating wire and the pipe.
    The substrate processing apparatus according to claim 9.
  13. 前記第１のヒータユニットは、
    前記第１の発熱線及び前記第２の発熱線を格納する、ブロック状に一体形成された格納部材を備え、
    前記格納部材の熱伝導率は、０．３Ｗ／ｍ・Ｋ以下である、
    請求項９記載の基板処理装置。     The first heater unit includes:
    A storage member integrally formed in a block shape for storing the first heating wire and the second heating wire;
    The storage member has a thermal conductivity of 0.3 W / m · K or less.
    The substrate processing apparatus according to claim 9.
  14. 前記反応管は石英で構成され、
    前記ヒータは、
    ８０～１００℃で発熱する時に放射する熱線のピーク波長が５～１０μｍとなる特性を有する発熱線を備える、
    請求項１記載の基板処理装置。     The reaction tube is made of quartz,
    The heater is
    A heating wire having a characteristic that the peak wavelength of the heat rays radiated when generating heat at 80 to 100 ° C. is 5 to 10 μm;
    The substrate processing apparatus according to claim 1.
  15. 前記制御部は、
    前記複数の温度センサの測定値が１２０℃以下となるように、前記ヒータに供給される電力を制御するよう構成される、
    請求項１記載の基板処理装置。     The controller is
    The power supplied to the heater is controlled so that the measured values of the plurality of temperature sensors are 120 ° C. or less.
    The substrate processing apparatus according to claim 1.
  16. 前記反応管内に過酸化水素を含むガスを供給するよう構成されたガス供給系を備え、
    前記制御部は、
    前記複数の温度センサの測定値が８０℃以上１１２℃未満となるように、前記ヒータに供給され電力を制御するよう構成される、
    請求項１記載の基板処理装置。     A gas supply system configured to supply a gas containing hydrogen peroxide into the reaction tube;
    The controller is
    The power supplied to the heater is controlled so that the measured values of the plurality of temperature sensors are 80 ° C. or higher and lower than 112 ° C.,
    The substrate processing apparatus according to claim 1.
  17. 基板を収容する反応管と、前記反応管に形成された炉口を閉塞する蓋部と、前記反応管の炉口近傍の側壁に接続する配管と、を備える基板処理装置に設けられ、
    前記反応管の炉口近傍の側壁の外周に設けられて、前記側壁の周方向において複数に分割されたヒータを構成し、
    前記側壁に対向するように前記側壁の周方向に沿って配置された第１の発熱線と、前記配管の周囲に前記配管の延伸方向に沿って配置された第２の発熱線と、を備えるヒータユニット。     Provided in a substrate processing apparatus comprising: a reaction tube that accommodates a substrate; a lid that closes a furnace port formed in the reaction tube; and a pipe connected to a side wall near the furnace port of the reaction tube,
    Provided on the outer periphery of the side wall near the furnace port of the reaction tube, constituting a heater divided into a plurality in the circumferential direction of the side wall;
    A first heat generating line disposed along the circumferential direction of the side wall so as to face the side wall; and a second heat generating line disposed along the extending direction of the pipe around the pipe. Heater unit.
  18. 基板を収容する反応管と、前記反応管に形成された炉口を閉塞する蓋部と、前記反応管の炉口近傍の側壁の外周に設けられたヒータと、前記反応管の炉口近傍の側壁における、前記側壁の周方向において互いに異なる複数の位置の温度をそれぞれ測定するよう構成された複数の温度センサと、を備えた基板処理装置を提供する工程と、
    前記反応管内に前記基板を収容する工程と、
    前記基板を加熱する工程と、を有し、
    前記基板を加熱する工程では、前記複数の温度センサのそれぞれの測定値に基づいて、前記ヒータに供給される電力を制御して前記炉口近傍の側壁を加熱する、半導体装置の製造方法。 
          A reaction tube containing the substrate, a lid portion for closing the furnace port formed in the reaction tube, a heater provided on the outer periphery of the side wall near the furnace port of the reaction tube, and the vicinity of the furnace port of the reaction tube Providing a substrate processing apparatus comprising: a plurality of temperature sensors configured to respectively measure temperatures at a plurality of positions different from each other in the circumferential direction of the side wall in the side wall;
    Accommodating the substrate in the reaction tube;
    Heating the substrate,
    The method of manufacturing a semiconductor device, wherein in the step of heating the substrate, the power supplied to the heater is controlled based on the measured values of the plurality of temperature sensors to heat the side wall near the furnace port.
PCT/JP2017/012974 2017-03-29 2017-03-29 Substrate processing device, heater unit, and semiconductor device manufacturing method WO2018179157A1 (en)

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