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WO2019078036A1 - サセプター - Google Patents

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Publication number
WO2019078036A1
WO2019078036A1 PCT/JP2018/037342 JP2018037342W WO2019078036A1 WO 2019078036 A1 WO2019078036 A1 WO 2019078036A1 JP 2018037342 W JP2018037342 W JP 2018037342W WO 2019078036 A1 WO2019078036 A1 WO 2019078036A1
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WO
WIPO (PCT)
Prior art keywords
susceptor
temperature
wafer
graphite
electrical resistivity
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2018/037342
Other languages
English (en)
French (fr)
Inventor
修一 大窪
輝 ▲高▼橋
俊哉 鈴木
薄葉　秀彦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Techno-Carbon Co Ltd
Original Assignee
Nippon Techno-Carbon Co Ltd
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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=66173632&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=WO2019078036(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Nippon Techno-Carbon Co Ltd filed Critical Nippon Techno-Carbon Co Ltd
Priority to US16/618,916 priority Critical patent/US20200385864A1/en
Priority to KR1020207002541A priority patent/KR102088493B1/ko
Priority to CN201880046563.0A priority patent/CN110914955B/zh
Priority to EP18868072.2A priority patent/EP3627536B1/en
Priority to JP2019549207A priority patent/JP6621971B2/ja
Publication of WO2019078036A1 publication Critical patent/WO2019078036A1/ja
Anticipated expiration legal-status Critical
Priority to US18/214,798 priority patent/US20230349045A1/en
Ceased legal-status Critical Current

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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
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
    • 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
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
    • H01L21/687—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches
    • H01L21/68714—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches the wafers being placed on a susceptor, stage or support
    • H01L21/68757—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using mechanical means, e.g. chucks, clamps or pinches the wafers being placed on a susceptor, stage or support characterised by a coating or a hardness or a material
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • C23C16/325—Silicon carbide
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/342—Boron nitride
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/42—Silicides
    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4581—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber characterised by material of construction or surface finish of the means for supporting the substrate
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
    • C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
    • C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
    • C23C16/4584—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally the substrate being rotated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4582—Rigid and flat substrates, e.g. plates or discs
    • C23C16/4583—Rigid and flat substrates, e.g. plates or discs the substrate being supported substantially horizontally
    • C23C16/4586—Elements in the interior of the support, e.g. electrodes, heating or cooling devices
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/12—Substrate holders or susceptors
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403—AIII-nitrides
    • 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
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67098—Apparatus for thermal treatment
    • H01L21/67103—Apparatus for thermal treatment mainly by conduction
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    • 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
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
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    • H01L21/67115—Apparatus for thermal treatment mainly by radiation
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    • 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
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    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67242—Apparatus for monitoring, sorting or marking
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    • C—CHEMISTRY; METALLURGY
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    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Definitions

  • the present invention relates to a susceptor which is used in a CVD apparatus for epitaxially growing a semiconductor film on a wafer in the field of manufacturing LEDs (light emitting diodes), power devices, etc., and which carries the wafer and generates heat by induction heating. .
  • Patent Document 1 A susceptor for mounting the wafer is installed in the epitaxial growth apparatus, and the wafer is heated by heat transfer from the susceptor that generates heat by induction heating, and the wafer is mounted on the wafer using MOCVD (metal organic chemical vapor deposition).
  • MOCVD metal organic chemical vapor deposition
  • a semiconductor film is formed to produce a wafer product.
  • the wafer product on which the semiconductor film is formed is cut into chips of a certain size depending on the application and used for semiconductor parts of LEDs and power devices.
  • a sapphire substrate is mounted on a susceptor and heating is performed, and a GaN film is formed on a sapphire substrate by flowing hydrogen as a carrier gas, ammonia as a source gas, and TMG (trimethylgallium) on a sapphire substrate.
  • a buffer layer doped with Al, an n-type layer doped with Si, an active layer doped with In, and a p-type layer doped with Mg are stacked in this order (Patent Document 2).
  • the quality of the GaN film different in these components can be maintained by heating the wafer to an optimum temperature, and the quality can be maintained, and the productivity can be maintained by adjusting the susceptor temperature rapidly for each film stack. Be done.
  • the susceptor is a graphite base having heat resistance and conductivity so that the temperature can be quickly adjusted, and heat is generated by induction heating.
  • the epitaxial growth apparatus is designed to make the temperature distribution of the susceptor uniform by dividing the heat generation zone into a plurality of induction heating coils or rotating the susceptor with respect to the induction heating coils. There is.
  • the heat generation characteristics of the susceptor directly affect the temperature of the wafer, so the characteristics of the electrical resistivity of the graphite substrate constituting the susceptor are optimized. Without it, precise temperature control can not be performed.
  • the susceptor needs to quickly adjust the wafer temperature in order to deposit the semiconductor film on the wafer within a limited process time, and has a good response to temperature control in terms of wafer product quality and productivity. Is required.
  • the electrical resistivity of the graphite substrate is temperature-dependent, and if the electrical resistivity of the graphite substrate does not match the temperature change associated with induction heating, temperature control with good response becomes difficult, which is optimal.
  • the deviation from the temperature causes a decrease in the quality of wafer products and a decrease in productivity due to the extension of the process time.
  • the electrical resistivity distribution of the graphite base material is largely dispersed, the heat generation is uneven, the temperature difference in the susceptor surface is increased, and the susceptor is damaged due to the thermal stress, and the durability problem also occurs.
  • the present invention is to provide a susceptor with improved temperature control response by matching the high specific resistance of the graphite base to the induction heating, so that a high quality wafer can be obtained without loss of productivity.
  • the purpose is to obtain a product.
  • the present invention is a susceptor comprising a graphite substrate and a ceramic coating layer and generating heat by induction heating, wherein the variation ( ⁇ max / ⁇ min ) of the in-plane electrical resistivity distribution of the graphite substrate at room temperature is 1.00 to
  • the susceptor is characterized in that it is 1.05, and the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) of the electric specific resistance at 800 ° C. and 1600 ° C. is 1.14 to 1.30.
  • the ceramic coating layer at least one material of SiC, TaC, and PBN (pyrolytic boron nitride) is suitable.
  • the temperature response of the susceptor temperature by induction heating is high, temperature control can be performed accurately and quickly, and it is possible to simultaneously improve the quality of the wafer product and the improvement of the productivity by shortening the process time. it can.
  • the susceptor of the present invention is a susceptor that generates heat by induction heating, and has a graphite base and a ceramic coating layer. And, the variation ( ⁇ max / ⁇ min ) of the in-plane electrical resistivity distribution at room temperature of the graphite substrate is 1.00 to 1.05, and the high temperature change rate of the electrical resistivity at 800 ° C. and 1600 ° C. ( ⁇ 1600 / ⁇ 800) ) Is 1.14 to 1.30.
  • the heat generation in the susceptor surface is uniform relative to the induction heating As a result, the temperature in the susceptor surface becomes uniform.
  • the plurality of mounted wafers can be heated at the same temperature, and variations in the quality of the wafer product can be eliminated.
  • the temperature in the susceptor plane uniform, it is possible to solve the problem of durability such as avoiding damage to the susceptor due to thermal stress.
  • the susceptor according to the present invention improves the temperature response to induction heating by setting the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) of the electrical resistivity of the graphite base to 1.14 to 1.30, thereby controlling the temperature of the susceptor. It can be done accurately and quickly.
  • the high temperature electrical resistivity ( ⁇ t ) of the graphite substrate was measured at room temperature to a ratio R t / R 0 of the resistance value R t measured at high temperatures (800 ° C. and 1600 ° C.) and the room temperature resistance value R 0 It can be obtained by multiplying the electrical resistivity 0 0 .
  • High temperature electrical resistivity t t 0 0 (R t / R 0 )
  • the high temperature change rate (( 1600 / / 800 ) of the electrical specific resistance at 800 ° C. and 1600 ° C. can be calculated using the resistance values (R 1600 , R 800 ) at 800 ° C. and 1600 ° C.
  • the temperature dependence of the electrical resistivity of the graphite material decreases from room temperature to around 600 to 800 ° C., and after a local minimum at around 600 to 800 ° C., the temperature dependence of the resistivity is linear with the temperature rise It is known that the crystallite size of the graphite material is larger (the crystallinity of the graphite material is higher), the slope of this line is larger (carbon, No.
  • the electrical resistivity of the graphite substrate linearly increases with the temperature rise, and the present invention shows that the high temperature change rate at this time ( ⁇ 1600 / ⁇ 800 ) Is made by finding that it affects the responsiveness of the temperature control of the susceptor. Although the reason for this is not clear, the following reasons can be considered.
  • the susceptor installed in the epitaxial growth apparatus generates an eddy current in the graphite base by supplying power to the induction heating coil therebelow, and generates heat by Joule heat (Joule's law).
  • Joule heat (P) eddy current (I) ⁇ eddy current (I) ⁇ electrical resistance (R)
  • the electric resistance (R) of the susceptor is designed on the basis of the heat treatment capability of the epitaxial growth apparatus, and the electric resistivity of the graphite base is selected in accordance with the electric resistance (R). Since the electrical resistance (R) has a correlation with the electrical resistivity ( ⁇ ) of the graphite substrate, the term of electrical resistance can be treated the same as the electrical resistivity.
  • the susceptor can control the temperature by changing the eddy current (I) by adjusting the power supplied to the induction heating coil.
  • I eddy current
  • the electrical resistivity of the graphite substrate also starts to increase simultaneously at 800 ° C. or higher, so both the eddy current (I) and the electrical resistance (R) contribute to the temperature rise of the susceptor.
  • the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) of the electrical resistivity is larger, the electric resistance (R) of the susceptor along with the temperature rise becomes larger, the Joule heat (P) increases, and the temperature rise is promoted.
  • the temperature response of the susceptor is improved because the temperature rise of the susceptor appears earlier than the readjustment of the power of the induction heating coil. Since the susceptor of the present invention has improved temperature responsiveness due to induction heating, rapid temperature control can be performed with respect to the target temperature, and standby time for temperature stabilization is minimized. High quality wafer products can be obtained without losing the quality.
  • the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) As the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) is larger, the temperature rise is promoted and the temperature response is improved, but if it is more than 1.30, the temperature when approaching the target temperature tends to hunting and becomes a constant temperature. It takes time. Therefore, the upper limit of 1600 1600 / ⁇ 800 of the present invention is 1.30.
  • the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) is smaller than 1.14, the temperature response of the susceptor is reduced. In this case, the increase in electrical resistivity due to the temperature rise is small, and the eddy current due to the power adjustment of the induction heating coil mainly contributes to heat generation, so the temperature response of the susceptor becomes dull and stable at the target temperature It takes time. Since the wafer product is manufactured by repeatedly adjusting to different temperatures, if the high temperature change rate ( 1600 1600 / ⁇ 800 ) is smaller than 1.14, the time required for one cycle becomes longer and the productivity of the wafer product is lowered
  • the susceptor is exposed to an etching gas such as hydrogen and ammonia at a high temperature, so the surface is coated with a highly corrosion resistant ceramic coating to prevent rapid consumption of the graphite substrate.
  • the ceramic coating layer can be selected from at least one material of SiC (silicon carbide), TaC (tantalum carbide), or PBN (pyrolytic boron nitride), and is coated on the surface of a graphite substrate by a general CVD method can do.
  • FIG. 1 is a schematic view when a susceptor is installed in an epitaxial growth apparatus to manufacture a wafer product.
  • the susceptor 1 of the present invention can be installed above the induction heating coil 2 provided in the apparatus, and when power is supplied to the induction heating coil, the susceptor 1 generates heat by induction heating.
  • a wafer holder 3 and a protective member 4 are disposed on the upper surface of the susceptor 1 and are heated by heat transfer from the susceptor 1 which generates heat.
  • the wafer holder 3 is formed with a pocket for holding the wafer 5 and heats the wafer 5 loaded in the pocket by heat transfer.
  • the wafer holder 3 and the protective member 4 are generally the same material as the susceptor 1.
  • the temperature of the wafer 5 and the susceptor 1 can be measured by the radiation thermometers 6 and 7 respectively, but it is desirable to control the wafer temperature with the radiation thermometer 6 and manufacture for quality control of wafer products. . Since the temperature of the wafer 5 is adjusted by heat transfer from the susceptor 1, the temperature of the susceptor 1 must naturally be higher than the temperature of the wafer 5.
  • the induction heating temperature controller 8 senses the wafer temperature measured by the radiation thermometer 6, sends a signal to the induction heating power source based on a preset temperature program, and adjusts the power of the induction heating coil. .
  • the radiation thermometer 6 feeds back a change in wafer temperature after power adjustment to the temperature controller 8 to readjust the power of the induction heating coil and perform temperature control.
  • the responsiveness of the temperature control of the epitaxial growth apparatus is primarily determined by the performance of the temperature controller 8, the induction heating power supply 9, and the induction heating coil 2.
  • a carrier gas and a raw material gas can flow in the upper space of the wafer, and a semiconductor film is laminated on the heated wafer 5 by the MOCVD method to manufacture a wafer product.
  • FIG. 2 is a schematic cross-sectional view showing an example of a wafer product 11 manufactured using the susceptor of the present invention.
  • the first layer on the sapphire substrate 12 has an AlGaN buffer layer 13 in which GaN is doped with Al, and a Si-doped n-type GaN layer 14, an In-doped InGaN well layer 15a and an undoped GaN barrier layer 15b are alternately stacked.
  • the active layer 15 of the multiple quantum well structure and the p-type GaN layer 16 doped with Mg are stacked in this order.
  • FIG. 3 is a pattern of a temperature program showing an example when a wafer product is manufactured using the susceptor of the present invention.
  • the heating temperature of the wafer is controlled in the range of about 600 to 1100 ° C.
  • the temperature of the susceptor generates heat at a temperature about 100 to 200 ° C. higher than that.
  • the susceptor mounts a sapphire substrate and induction heating is started.
  • a heat treatment called thermal cleaning is performed without flowing the source gas at a high temperature.
  • the film is laminated while sequentially performing temperature control for laminating each GaN layer constituting the wafer product, and the wafer product is manufactured within a determined process time of one cycle.
  • the quality of the GaN film laminated on the sapphire substrate (wafer) can be evaluated by an optical analysis method using a photoluminescence method (PL method). For example, when a wafer product is irradiated with laser light, electron-hole pairs are generated in the intrinsic band gap of the semiconductor, and light is emitted when these are recombined. By measuring the emission spectrum, the band gap, the crystallinity, the doping amount and the like can be evaluated. (The 11th Nitride Semiconductor Application Study Group “Observation of nitride crystal growth using in-situ monitor” 2011. 7.7)
  • FIG. 4 is a schematic view of a method of measuring the wavelength (PL wavelength) of the emission spectrum when the wafer product 11 is irradiated with laser light from the PL analyzer 21 mounted on the epitaxial growth apparatus.
  • the analysis of the wafer product is performed by measuring the PL wavelength corresponding to the place on the entire surface of the semiconductor film by scanning the entire surface of the wafer with laser light at minute intervals.
  • the quality evaluation of a wafer product is performed using an average value and a standard deviation (STD) obtained by statistically processing PL wavelengths measured on the entire surface of the wafer.
  • STD standard deviation
  • the average value of the PL wavelength obtained for each wafer is, for example, an index for determining that the product conforms to the wavelength standard of an LED different from product to product, and in the present invention, ⁇ 3 nm of the target PL wavelength was accepted.
  • STD which is an indicator of variation obtained for each wafer, affects the number of LED chips obtained as non-defective products from one wafer product. The smaller the STD value, the smaller the variation in PL wavelength, so it is judged that the quality of the wafer product is better. In the present invention, the STD of less than 2 nm is accepted.
  • FIG. 5 shows the place where the in-plane electric specific resistance was measured for the graphite base of the susceptor schematic view used as an example of the present invention.
  • the in-plane electrical resistivity can be nondestructively measured at fourteen points ((marks) on the surface of the graphite substrate by the four-point probe method.
  • the variation ( ⁇ max / ⁇ min ) of the electrical resistivity distribution can be indexed by the ratio of the maximum value ( ⁇ max ) to the minimum value ( ⁇ min ) measured at multiple locations on the graphite substrate.
  • An average value ( ⁇ av ) was obtained by averaging the measured 16 specific resistances.
  • FIG. 6 shows a schematic view of an apparatus for measuring high temperature electrical resistance.
  • the measurement of the electrical resistance at high temperature sets the graphite sample 1A ( ⁇ 10 x 100 mm) cut out from the graphite base in the electric furnace 31 and heats from room temperature to 1600 ° C while applying DC power to terminals attached to both ends of the graphite sample 1A.
  • 32 was connected to measure the current value and the voltage drop value by the ammeter 33 and the potentiometer 34.
  • the temperature was measured by a temperature recorder 36 with a thermocouple 35 attached directly to the center of the graphite sample 1A.
  • the resistance value R t of each temperature was calculated using the current value and the voltage drop value measured here.
  • the manufacturing method of the graphite base material used for the susceptor of this invention is demonstrated, it is not limited to the following method.
  • it can be obtained by machining a graphite material by cold isostatic pressing (CIP) into the shape of a susceptor.
  • CIP cold isostatic pressing
  • aggregate used as a raw material is manufactured using needle coke powder or needle coke powder. Pulverized powder of artificial graphite, natural graphite powder and the like are used.
  • the physical properties of the graphite material can be adjusted by blending amorphous coke powder as the aggregate.
  • the aggregate raw material to be used in the present invention is preferably a mixture of two or more of them.
  • a mixed material of 30 to 80 parts by weight of amorphous coke powder and 20 to 70 parts by weight of needle coke powder is preferable.
  • a mixed material of 50 to 80 parts by weight of amorphous coke powder and 20 to 50 parts by weight of graphite powder is preferable.
  • the aggregate is used after being crushed to a predetermined particle size, but in the present invention, it is preferable that the particle size is distributed in the range of 1 to 200 ⁇ m and the average particle size (median particle size D 50 ) does not exceed 20 ⁇ m.
  • the fine powder is removed in the classification operation after grinding to adjust the particle size to coarse particles.
  • the average particle diameter is larger than 20 ⁇ m, the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) of the graphite substrate may be excessive.
  • the average particle size is 5 to 15 ⁇ m.
  • the above aggregate is heat-kneaded with a binder (tar, pitch, etc.) at a predetermined blending ratio, cooled to around room temperature, and then crushed by a grinder.
  • the pulverized powder is filled in a rubber rubber case and sealed, and then pressed by a CIP molding machine to obtain a molded body.
  • the obtained molded body is heat-treated to 1000 ° C. in a non-oxidizing atmosphere to be calcined and carbonized.
  • the fired body can be impregnated with the hot-melted pitch for impregnation and fired again as required. By pitch impregnation, the bulk density and strength of the obtained graphite material are increased, and the electrical resistivity is reduced.
  • the obtained sintered body can be heat treated at a range of 2800 to 3000 ° C. in a graphitization furnace to graphitize to obtain a graphite material.
  • the heat treatment temperature at the time of graphitization may be made uniform.
  • an atchison furnace or a high frequency induction furnace is used as the graphitization furnace, but since the variation in the distribution of electrical resistivity tends to increase as the size of the graphite base increases, it is preferable to use the high frequency induction furnace rather than the atchison furnace.
  • the physical properties of the graphite substrate were obtained by cutting test pieces / TP (10 ⁇ 10 ⁇ 50 mm) from arbitrary locations of the graphite substrate, and measuring bulk density, thermal expansion coefficient, flexural strength, and electrical resistivity.
  • the bulk density is calculated by measuring the weight and volume of the test piece.
  • the thermal expansion coefficient was calculated by measuring the linear expansion coefficient when the test piece was heated from room temperature to 500 ° C. using a commercially available thermal analysis device equipped with a differential transformer.
  • the bending strength was calculated by measuring the maximum load when broken at a distance of 40 mm between the fulcrums and at a load rate of 0.5 mm / min with reference to JIS R 7222: 1997 (Method of measuring physical characteristics of graphite material).
  • the electrical resistivity was measured by a voltage drop method according to JIS R 7222: 1997 (Method of measuring physical characteristics of graphite material).
  • the physical properties of a graphite substrate that can be used as a susceptor include, for example, a bulk density of 1.70 to 1.80 g / cm 3 , a thermal expansion coefficient of 3.5 to 4.5 ⁇ 10 ⁇ 6 / K, and a flexural strength of 35 to 60 MPa And specific electric resistance ( ⁇ 0 ) of 8.0 to 13.0 ⁇ m.
  • the susceptor of the present invention is one in which a graphite substrate having a graphite material machined into the shape of the susceptor is coated with a ceramic film, preferably by the CVD method.
  • the ceramic coating layer is desirably at least one material of SiC, TaC, or PBN. In particular, a laminate of two or more layers of the same or different materials is preferable.
  • the thickness of the ceramic coating layer is preferably 50 to 200 ⁇ m.
  • the susceptor is exposed to reactive gases such as NH 3 and H 2 at high temperature, so that the ceramic coating excellent in corrosion resistance to these gases can be used repeatedly by coating the susceptor.
  • the method of coating the surface of the graphite substrate with a ceramic coating is by a known method using a CVD method.
  • Example 1 As an aggregate raw material, amorphous coke and needle coke were individually crushed to a maximum particle size of 200 ⁇ m by an atomizer crusher to obtain an aggregate having an average particle size of 15 ⁇ m each time.
  • the particle diameter of each aggregate is a value obtained by measurement using a laser diffraction type particle size distribution measuring device, and the average particle diameter is shown as a median diameter.
  • 40 parts by weight of amorphous coke powder and 60 parts by weight of acicular coke powder were blended to obtain an aggregate.
  • One hundred parts by weight of the aggregate was put into a kneading machine together with 70 parts by weight of a binder pitch, and was kneaded for 10 hours while heating at 220 ° C.
  • this kneaded material After cooling this kneaded material, it was reground to a maximum particle size of 250 ⁇ m to obtain a secondary powder for molding.
  • the resultant was filled in a rubber case and molded by a cold isostatic press (CIP) at a pressure of 1 t / cm 2 .
  • CIP cold isostatic press
  • the obtained compact was packed in a firing furnace, and fired and carbonized to 1000 ° C. in a non-oxidizing atmosphere to obtain a fired body.
  • the obtained fired body was impregnated with the pitch for impregnation and fired again at 1000 ° C. This was transferred to a high frequency induction furnace (HF) and heated to 3000 ° C. in a non-oxidative atmosphere to graphitize to obtain a graphite material.
  • HF high frequency induction furnace
  • a plurality of graphite substrates were processed into a doughnut-shaped susceptor shape from the obtained graphite material.
  • a test piece (10 ⁇ 10 ⁇ 50 mm) of a graphite material was cut out of one of them, and the physical property value at room temperature was measured (Table 2).
  • the distribution of electrical resistivity was obtained by measuring the electrical resistivity at 16 points shown in FIG. 5 in the plane of the graphite substrate.
  • the measurement of the electrical resistivity was performed using a resistivity instrument (Loresta-EP) manufactured by Dia Instruments.
  • Table 2 shows the average value av , the maximum value ⁇ max , and the minimum value min min of the obtained electric specific resistances.
  • the variation in electrical resistivity ( ⁇ max. / ⁇ min ) calculated using this result is shown in Table 3.
  • the characteristic of high temperature electrical resistivity is the relative value of each temperature to room temperature ( ⁇ t / ⁇ using the resistance value measured by setting the graphite sample ( ⁇ 10 x 100 mm) cut from the graphite base in the apparatus of FIG. 0 ) (Fig. 7). Using the relative values at 800 ° C. and 1600 ° C., the high temperature change rate ( ⁇ 1600 / ⁇ 800 ) of the electrical resistivity was calculated and is shown in Table 3.
  • the graphite substrate processed into a susceptor shape is placed in a purification furnace and purified with Cl 2 gas under high temperature, and then put into a CVD furnace to introduce a mixed gas of SiCl 4 and C 3 H 8 under high temperature together with H 2 carrier gas Then, a SiC film having a thickness of 100 ⁇ m (50 ⁇ m twice coated) was formed on the surface of the graphite substrate to obtain a susceptor.
  • the susceptor was placed in an epitaxial growth apparatus (A), 11 sapphire substrates of 4 inches were mounted, and a GaN film was laminated by a MOCVD method for 8 hours for a processing time to produce a wafer product for LED (target wavelength 443 nm) .
  • the active layer of the obtained wafer product was measured at an in-plane 1 ⁇ 1 mm interval by a photoluminescence (PL) analyzer, and statistical processing was performed for each wafer and 11 sheets were averaged.
  • the PL wavelength was 443.8 nm
  • the standard deviation (STD) was 1.3. As a result of repeated use of the susceptor, it could be used for more than 200 cycles.
  • Example 2 A susceptor was obtained in the same manner as in Example 1 except that 50 parts by weight of amorphous coke powder and 50 parts by weight of needle coke powder were blended to form an aggregate. Using this susceptor, a wafer product was produced in the same procedure as in Example 1 to measure the PL wavelength. As a result, the PL wavelength had an average value of 443.5 nm and a standard deviation of 1.4. As a result of repeated use of the susceptor, it could be used for more than 200 cycles.
  • Example 3 As an aggregate raw material, the cutting powder of the artificial graphite material manufactured with needle-like coke was crushed with an atomizer crusher to obtain an aggregate having an average particle diameter of 70 ⁇ m. Same as Example 1 except that 67 parts by weight of amorphous coke powder and 33 parts by weight of the above-mentioned artificial graphite powder were blended to make an aggregate, and the obtained sintered body was graphitized without impregnating the pitch. A graphite material was obtained by the method. After a graphite substrate processed into a susceptor shape was obtained from this graphite material, a susceptor was obtained by the same method as in Example 1.
  • This susceptor was installed in an epitaxial growth apparatus (B), 14 sapphire substrates of 4 inches were mounted, and a GaN film was laminated by a MOCVD method for 8 hours for a processing time to produce a wafer product for LED (target wavelength 443 nm) .
  • the active layer of the obtained wafer product was measured at an in-plane 1 ⁇ 1 mm interval by a photoluminescence (PL) analyzer, and statistical processing was performed on each wafer to average 14 sheets, and the PL wavelength had an average value of 443.2 nm, The standard deviation was 1.6. As a result of repeated use of the susceptor, it could be used for more than 200 cycles.
  • Example 4 A susceptor was obtained in the same manner as in Example 3, except that 60 parts by weight of amorphous coke powder and 40 parts by weight of needle coke powder were blended to form an aggregate. Using this susceptor, a wafer product was produced in the same procedure as in Example 3, and the PL wavelength was measured. As a result, the PL wavelength had an average value of 443.6 nm and a standard deviation of 1.7. As a result of repeated use of the susceptor, it could be used for more than 200 cycles.
  • Example 5 A susceptor was obtained in the same manner as in Example 3 except that 70 parts by weight of amorphous coke powder and 30 parts by weight of needle coke powder were blended to form an aggregate. Using this susceptor, a wafer product was produced in the same procedure as in Example 3, and the PL wavelength was measured. As a result, the PL wavelength had an average value of 444.1 nm and a standard deviation (STD) of 1.8. As a result of repeated use of the susceptor, it could be used for more than 200 cycles.
  • STD standard deviation
  • Comparative Example 1 60 parts by weight of powder obtained by grinding amorphous coke to a maximum particle diameter of 30 ⁇ m by an atomizer crusher and 60 parts by weight of needle-like coke to a maximum particle diameter of 200 ⁇ m by an atomizer crusher 40 parts by weight of powder having an average particle diameter of 50 ⁇ m obtained by removing 30% of the fine powder was blended to obtain an aggregate, and the obtained sintered body was graphitized without impregnating the pitch, A susceptor was obtained in the same manner as in Example 1. Using this susceptor, a wafer product was produced in the same procedure as in Example 1 to measure the PL wavelength.
  • the PL wavelength had an average value of 447.8 nm and a standard deviation (STD) of 1.6, and the PL wavelength deviated from the target value and the wafer product became defective. For this reason, the use of the susceptor was discontinued.
  • Comparative example 2 A susceptor was obtained in the same manner as in Example 1 except that 80 parts by weight of amorphous coke powder and 20 parts by weight of needle coke powder were blended to form an aggregate. Using this susceptor, a wafer product was produced in the same procedure as in Example 1 to measure the PL wavelength. The wafer wavelength became defective because the PL wavelength deviated from the target value. For this reason, the use of the susceptor was discontinued.
  • Comparative example 3 50 parts by weight of amorphous coke powder and 50 parts by weight of acicular coke powder are combined to form an aggregate, pitch impregnated in a fired body and fired again at 1000 ° C., then graphitization is performed with an Atchison furnace (AC) 2500
  • a susceptor was obtained by the same method as in Example 3 except that the temperature was changed to ° C.
  • a wafer product was produced in the same procedure as in Example 3, and the PL wavelength was measured. Both PL wavelength and STD deviated from the target value or the standard value, and the wafer product became defective.
  • the susceptor was discontinued from use because the SiC coating was damaged in one use.
  • Comparative example 4 After pitch-impregnating the fired body and firing again at 1000 ° C., a susceptor was obtained in the same manner as in Example 4 except that the graphitization treatment was performed at 2500 ° C. Using this susceptor, a wafer product was produced in the same procedure as in Example 4 to measure the PL wavelength. The wafer wavelength became defective because the PL wavelength deviated from the target value. For this reason, the use of the susceptor was discontinued.
  • Comparative example 5 A susceptor was obtained by the same method as in Example 5, except that the fired body was pitch impregnated and fired again at 1000 ° C., and then the graphitization treatment was performed at 2500 ° C. A wafer product was produced by the same procedure as in Example 5 using this susceptor, but although the quality of the wafer product passed, the temperature response was inferior and the process time had to be 10 hours.
  • Table 1 shows the used aggregate and graphitization conditions.
  • the physical properties of the obtained graphite base are shown in Table 2.
  • the evaluation results of the obtained susceptor are summarized in Table 3.
  • the PL wavelength (average value) of the wafer product manufactured by the MOCVD method is the target value of 443 ⁇ 3 nm Within, standard deviation (STD) was less than 2 and satisfied the quality standard.
  • Comparative Example 3 where the variation ( ⁇ max / ⁇ min ) of the electrical resistivity exceeds 1.05, the standard deviation (STD) is greater than 3 because the temperature variation of the susceptor is large, and the coating film cracked.
  • Comparative Example 5 in which the high temperature change rate 1600 1600 / ⁇ 800 of the electrical resistivity is less than 1.14 passed the quality of the wafer product by extending the process time to 10 hours although the temperature response of the susceptor was low. However, because the productivity of wafer products decreased, it could not be used for mass production.
  • the present invention can be suitably used for a susceptor used when performing vapor phase epitaxial growth.

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Abstract

温度コントロールの応答性が向上したサセプターを提供するものであり、生産性を損なうことなく高品質のウエハ製品を得ることを目的とする。　誘導加熱によって発熱するサセプターであって、黒鉛基材とセラミックコーティング層を有し、黒鉛基材の室温における面内の電気比抵抗分布のバラツキ（ρmax/ρmin）が1.00～1.05であり、800℃と1600℃の電気比抵抗の高温変化率（ρ1600/ρ800）が1.14～1.30であることを特徴とするサセプター。

Description

サセプター
　本発明は、LED（発光ダイオード）、パワーデバイス等の製造分野において、ウエハ上に半導体被膜をエピタキシャル成長させるためのCVD装置内で用いられ、ウエハを搭載して誘導加熱によって発熱するサセプターに関するものである。
　エピタキシャル成長による半導体被膜はSiの他にGaNやSiC等の化合物半導体が知られており、コストダウンを目的に複数のウエハを大型サセプターに搭載して1600℃まで加熱処理することができるエピタキシャル成長装置が提案されている（特許文献1）。
　エピタキシャル成長装置にはウエハを搭載するためのサセプターが設置されており、誘導加熱によって発熱したサセプターからの伝熱でウエハが加熱され、MOCVD法（有機金属気相成長法)を利用してウエハ上に半導体被膜を形成してウエハ製品が製造される。この半導体被膜を形成したウエハ製品は、用途に応じて一定のサイズのチップに切断されてLEDやパワーデバイスの半導体部品に供される。
　白色LEDに供されるウエハ製品は、一般にサファイア基板をサセプターに搭載して加熱を行い、サファイア基板上にキャリアガスの水素、原料ガスのアンモニアとTMG(トリメチルガリウム)を流すことでGaN被膜を形成したものであるが、LEDとしての機能を発現させるために、例えばAlをドープしたバッファ層、Siをドープしたn型層、Inをドープした活性層、Mgをドープしたp型層の順番で積層されている(特許文献2）。
　これら含有成分が異なるGaN被膜は、最適な温度にウエハを加熱して成膜されることで品質を保つことができ、各被膜の積層毎にサセプター温度を迅速に調整することで生産性が維持される。
　サセプターは、温度の調節が迅速にできるように耐熱性と導電性を備えた黒鉛基材が採用されており、誘導加熱で発熱する。また、エピタキシャル成長装置は、誘導加熱コイルを複数化して発熱ゾーンを分割することや、誘導加熱コイルに対してサセプターを回転駆動させることによって、サセプターの温度分布を均一にするための装置設計がされている。
特表２００４－５０７６１９号公報 特開２００４－２８１８６３号公報
　しかしながら、エピタキシャル成長装置で均一加熱の設計がなされたとしても、誘導加熱の場合、サセプターの発熱特性がウエハの温度に直接影響するので、サセプターを構成する黒鉛基材の電気比抵抗の特性を最適化しなければ精密な温度コントロールができない。サセプターは、限られたプロセス時間内で半導体被膜をウエハに積層させるために、迅速にウエハ温度を調節する必要があり、ウエハ製品の品質と生産性の観点から温度コントロールに対して良好な応答性が求められる。
　一方で、黒鉛基材の電気比抵抗は温度依存性があり、誘導加熱に伴う温度変化に対して黒鉛基材の電気比抵抗が適合しなければ、応答性の良い温度コントロールが困難となり、最適温度からのズレによるウエハ製品の品質低下やプロセス時間の延長による生産性の低下が発生する。また、黒鉛基材の電気比抵抗分布のバラツキが大きいと、発熱にムラが生じてサセプター面内の温度差が大きくなり、熱応力によりサセプターが破損するなど耐久性の問題も発生する。
　本発明は、誘導加熱に対して黒鉛基材の高温における電気比抵抗を適合させることで、温度コントロールの応答性が向上したサセプターを提供するものであり、生産性を損なうことなく高品質のウエハ製品を得ることを目的とする。
　本発明は、黒鉛基材とセラミックコーティング層からなり、かつ誘導加熱によって発熱するサセプターであって、黒鉛基材の室温における面内の電気比抵抗分布のバラツキ（ρmax/ρmin）が1.00～1.05であり、800℃と1600℃の電気比抵抗の高温変化率（ρ1600/ρ800）が1.14～1.30であることを特徴とするサセプターである。
　上記セラミックコーティング層としては、SiC、TaC、PBN（熱分解窒化ホウ素）の少なくとも１種の材料が適する。
　本発明によれば、誘導加熱によるサセプターの温度の応答性が高いので、精度よく迅速に温度コントロールすることができ、ウエハ製品の品質向上とプロセス時間の短縮による生産性の向上を両立することができる。
サセプターの装置内での模式図 ウエハ製品の模式断面図 ウエハ製品を製造するときの温度プログラム ウエハ製品の品質評価の模式図 黒鉛基材の面内の電気比抵抗の測定場所 高温の電気比抵抗測定装置の模式図 本発明の実施例による黒鉛基材の電気比抵抗の温度依存性 本発明の比較例による黒鉛基材の電気比抵抗の温度依存性
　本発明のサセプターは、誘導加熱によって発熱するサセプターであって、黒鉛基材とセラミックコーティング層を有する。そして、黒鉛基材の室温における面内の電気比抵抗分布のバラツキ（ρmax/ρmin）が1.00～1.05であり、800℃と1600℃の電気比抵抗の高温変化率（ρ1600/ρ800）が1.14～1.30である。
　本発明によれば、黒鉛基材の室温における面内の電気比抵抗分布のバラツキ（ρmax/ρmin）を1.00～1.05にすることにより、誘導加熱に対してサセプター面内の発熱が均一になり、サセプター面内の温度が均一化する。
　これにより、搭載された複数のウエハを同一温度で加熱することができてウエハ製品の品質のバラツキを解消することができる。また、サセプター面内の温度の均一化により、熱応力よるサセプターの破損を回避するなど耐久性の問題も解決することができる。
　ρmax/ρminが1.00のときはバラツキがないので面内で最も均一に発熱するが、ρmax/ρminが1.05を超えると面内で温度分布の差が大きくなって、搭載した複数のウエハ間で同一の温度にすることができず、ウエハ製品の品質がばらつく。しかも、サセプター面内の温度分布のバラツキが過大なため、サセプターに熱応力が発生してセラミック被膜（セラミックコーティング層）が損傷する場合や、渦電流の集中による局所的な異常過熱によってセラミック被膜が熱分解する場合がある。
　本発明のサセプターは、黒鉛基材の電気比抵抗の高温変化率(ρ1600/ρ800)を1.14～1.30にすることで、誘導加熱に対する温度の応答性が向上して、サセプターの温度コントロールを精度よく迅速に行うことができる。
　黒鉛基材の高温の電気比抵抗(ρt)は、高温（800℃と1600℃）で実測した抵抗値Rtと室温の抵抗値R0の比Rt /R0に、室温で実測した電気比抵抗ρ0を乗じることで求めることができる。
　　　　　　　　高温の電気比抵抗　ρt   =  ρ0(Rt/R0)
　また、800℃と1600℃の電気比抵抗の高温変化率（ρ1600/ρ800）は、800℃と1600℃の抵抗値（R1600、R800）を用いて計算することができる。
　黒鉛材料の電気比抵抗の温度依存性は、一般的に室温から600～800℃付近までは電気比抵抗は減少し、600～800℃付近で極小を経た後、温度の上昇に伴って直線的に増加することが知られており、黒鉛材料の結晶子のサイズが大きい(黒鉛材料の結晶性が高い)ほど、この直線の傾きは大きくなる（炭素,No.268,166-170,2015.）。
　ウエハ製品を製造する温度域（800℃以上）では、黒鉛基材の電気比抵抗は温度の上昇に伴い直線的に増加するのであり、本発明はこのときの高温変化率(ρ1600/ρ800)がサセプターの温度コントロールの応答性に影響することを見出すことによってなされたものである。この理由については明らかではないが、以下の理由が考えられる。
　エピタキシャル成長装置に設置したサセプターは、その下部の誘導加熱コイルに電力供給することで、黒鉛基材に渦電流が発生してジュール熱によって発熱する（ジュールの法則）。
　　　　ジュール熱（P) ＝ 渦電流(I) × 渦電流(I) × 電気抵抗(R)
　サセプターの電気抵抗(R)は、エピタキシャル成長装置の熱処理能力にもとづいて設計されており、電気抵抗(R)に見合った黒鉛基材の電気比抵抗が選択される。電気抵抗(R)は、黒鉛基材の電気比抵抗(ρ)と相関関係があるので、電気抵抗の項は電気比抵抗と同等に扱うことができる。
　サセプターは、誘導加熱コイルに供給する電力を調節することで、渦電流(I)が変化して温度をコントロールすることができる。サセプターの温度が上昇を開始すると、800℃以上では黒鉛基材の電気比抵抗も同時に増加し始めるので、渦電流(I)と電気抵抗(R)の両方がサセプターの温度上昇に寄与する。このため、電気比抵抗の高温変化率(ρ1600/ρ800)が大きいほど温度上昇に伴うサセプターの電気抵抗(R)が大きくなりジュール熱(P)が増えて温度上昇を促進する。従って、誘導加熱コイルの電力を再調整するよりも早くサセプターの温度上昇が発現するので、サセプターの温度の応答性が向上すると考えられる。
　本発明のサセプターは、誘導加熱による温度の応答性が向上するので、目標の温度に対して迅速な温度調節ができて、温度の安定化のための待機時間が最小化されることで、生産性を損なうことなく高品質なウエハ製品を得ることができる。
　高温変化率(ρ1600/ρ800)は大きいほど温度上昇を促進して温度の応答性は向上するが、1.30より大きいと目標温度に近づいたときの温度がハンチングしやすく一定温度になるのに時間を要する。従って、本発明のρ1600/ρ800の上限は1.30とした。
　一方、高温変化率(ρ1600/ρ800)が1.14より小さいとサセプターの温度の応答性が低下する。この場合、温度上昇に伴う電気比抵抗の増加は小さく、誘導加熱コイルの電力調整による渦電流が主に発熱に寄与するので、サセプターの温度の応答性が鈍くなり目標とする温度に安定するまで時間を要する。ウエハ製品は異なる温度に繰り返し調整して製造されるので、高温変化率(ρ1600/ρ800)が1.14より小さいと、1サイクルに要する時間が長くなりウエハ製品の生産性が低下する。
　サセプターは、高温で水素およびアンモニア等のエッチング性ガスに曝されるので、黒鉛基材の急激な消耗を防ぐために表面を耐食性に優れたセラミック被膜でコーティングする。セラミックコーティング層は、SiC（炭化ケイ素）、TaC（炭化タンタル）、又はPBN（熱分解窒化ホウ素）の少なくとも１種の材料から選ぶことができ、一般的なCVD法で黒鉛基材の表面にコーティングすることができる。
　ウエハ製品の製造方法の一例を、図１により説明する。図１は、エピタキシャル成長装置にサセプターを設置してウエハ製品を製造するときの模式図である。
　本発明のサセプター１は装置内に装備された誘導加熱コイル２の上方に設置することができ、誘導加熱コイルに電力供給するとサセプター１が誘導加熱によって発熱する。サセプター１の上面にはウエハホルダー３と保護部材４が設置されており、発熱したサセプター１からの伝熱によって加熱される。ウエハホルダー３はウエハ５を保持するためのポケットが形成されており、ポケットに搭載されたウエハ５を伝熱によって加熱する。ウエハホルダー３と保護部材４はサセプター１と同じ材料であることが一般的である。
　ウエハ５とサセプター１は、それぞれの放射温度計６，７によって温度を測定することができるが、ウエハ製品の品質管理のために放射温度計６でウエハの温度を管理して製造するのが望ましい。ウエハ５の温度はサセプター１からの伝熱によって調節されるので、自ずとサセプター１の温度はウエハ５の温度より高くする必要がある。
　誘導加熱の温度調節器８は、放射温度計６で測定されたウエハ温度を感知して、事前に設定された温度プログラムに基づいて誘導加熱電源に信号を送り、誘導加熱コイルの電力を調節する。放射温度計６は、電力調節後のウエハ温度の変化を温度調節器８にフィードバックすることで、誘導加熱コイルの電力が再調節されて温度コントロールされる。
　以上の通り、エピタキシャル成長装置の温度コントロールの応答性は、一次的には温度調節器８、誘導加熱電源９、誘導加熱コイル２の機器性能によって決まる。
　ウエハの上部空間には、キャリアガスと原料ガスを流すことができ、加熱されたウエハ５上にはMOCVD法によって半導体被膜が積層されてウエハ製品が製造される。
　図２は、本発明のサセプターを用いて製造されたウエハ製品１１の一例を示す模式断面図である。サファイア基板１２上の一層目はGaNにAlをドープしたAlGaN緩衝層１３があり、Siをドープしたn型GaN層１４、InをドープしたInGaN井戸層１５ａとアンドープのGaN障壁層１５ｂを交互に積層した多重量子井戸構造の活性層１５、Mgをドープしたp型GaN層１６の順番で積層されている。
　図３は、本発明のサセプターを用いてウエハ製品を製造したときの一例を示す温度プログラムのパターンである。例えば、ウエハの加熱温度が600～1100℃位の範囲で制御された場合、サセプターの温度はそれより100～200℃程度高い温度で発熱する。
　サセプターはサファイア基板を搭載して誘導加熱が開始される。初めにサファイア基板の表面を清浄化するために、高温で原料ガスを流すことなくサーマルクリーニングと呼ばれる熱処理を行う。続いて、ウエハ製品を構成する各GaN層を積層するための温度コントロールを逐次行いながら被膜を積層して、1サイクルの決められたプロセス時間内でウエハ製品を製造する。
　サファイア基板（ウエハ）に積層したGaN被膜の品質は、フォトルミネッセンス法(PL法)を利用した光学的分析手法で評価することができる。
　例えば、ウエハ製品にレーザー光を照射すると半導体の固有のバンドギャップよりに電子-正孔対が生成し、これらが再結合するときに発光する。この発光スペクトルを測定することで、バンドギャップ、結晶性、ドーピング量などを評価できる。（第11回窒化物半導体応用研究会「in-situ モニターを用いた窒化物結晶成長の観測」2011.7.7）
　図４は、エピタキシャル成長装置に搭載されたPL分析装置２１から、ウエハ製品１１にレーザー光を照射したときの発光スペクトルの波長(PL波長)を測定する方法の模式図である。
　ウエハ製品の分析は、ウエハ全面を微小間隔でレーザー光が走査することで、半導体被膜の全面について場所に対応したPL波長を測定して行われる。ウエハ製品の品質評価は、ウエハ全面で測定されたPL波長を統計処理して得られる平均値と標準偏差(STD)を用いて行われる。
　ウエハ毎に得られるPL波長の平均値は、例えば製品毎に異なるLEDの波長規格に適合したことを判断するための指標となり、本発明では目標のPL波長の±3nm以内を合格とした。
　ウエハ毎に得られるバラツキの指標となるSTDは、1枚のウエハ製品から良品として得られるLEDチップの数量に影響する。STD値が小さいほどPL波長のバラツキが少ないので、ウエハ製品の品質は良いと判断される。本発明ではSTDが2nm未満を合格とした。
　図５は、本発明の一例として用いられたサセプター模式図の黒鉛基材について、面内の電気比抵抗を測定した場所を示した。面内の電気比抵抗は、四探針法によって黒鉛基材の表面の16箇所（●印）を非破壊で測定することができる。
　電気比抵抗分布のバラツキ（ρmax/ρmin）は、黒鉛基材の複数箇所で測定された最小値（ρmin）に対する最大値（ρmax）の比で指標化することができる。測定された16箇所の電気比抵抗を平均することで平均値(ρav)を得た。
　図６は、高温の電気抵抗を測定する装置の模式図を示した。
　高温の電気抵抗の測定は、黒鉛基材から切り出した黒鉛試料１Ａ（φ10ｘ100mm）を電気炉３１にセットして、室温から1600℃まで加熱しながら、黒鉛試料１Ａの両端に取り付けた端子に直流電源３２を接続し、電流計３３、電位差計３４によって電流値と電圧降下値を測定して行った。温度は、黒鉛試料１Ａの中央に熱電対３５を直接取り付けて温度記録計３６によって測定した。ここで測定された電流値と電圧降下値を用いて、各温度の抵抗値Rtを算出した。
　本発明のサセプターに使用される黒鉛基材の製造方法について説明するが、以下の方法に限定されるものではない。
　好ましくは、冷間静水圧成形（Cold Isostatic Pressing/CIP）による黒鉛材料をサセプターの形状に機械加工して得ることができる。
　本発明に用いられる黒鉛材料は、黒鉛の結晶子のサイズが大きく黒鉛の結晶性が高いことが望ましいので、原料となる骨材は針状コークス粉、或いは針状コークス粉を用いて製造された人造黒鉛の粉砕粉、天然黒鉛粉等が利用される。更に、骨材としてアモルファスコークス粉を配合することで黒鉛材料の物性を調整することができる。本発明で使用する骨材原料はこれらを2種以上混合して使用するものが好ましい。例えば、アモルファスコークス粉３０～８０重量部と針状コークス粉２０～７０重量部との混合原料が好適である。また、アモルファスコークス粉５０～８０重量部と黒鉛粉２０～５０重量部との混合原料も好適である。
　骨材は所定の粒径に粉砕して利用されるが、本発明では粒径が1～200μmの範囲で分布して平均粒径（メジアン粒径D50）が20μmを越えないことが好ましい。特に針状コークス粉は、黒鉛基材の結晶子のサイズを大きく(黒鉛材料の結晶性を高く)するのに効果があるので、粉砕後の分級操作で微粉を除去して粗粒に粒度調整することや、平均粒径を20μmより大きくすることは、黒鉛基材の高温変化率(ρ1600/ρ800)を過大にする恐れがある。好ましくは平均粒径5～15μmである。
　上記の骨材は所定の配合割合で結合材（タール、ピッチ等）と共に熱混練した後、室温付近まで冷却してから粉砕機で粉砕する。粉砕粉はゴム製のラバーケースに充填して密封したのちCIP成形機で加圧して成形体を得る。
　得られた成形体は、非酸化性雰囲気で1000℃まで熱処理して焼成炭化される。焼成体は必要に応じて熱溶融した含浸用ピッチを含浸して再度焼成することができる。ピッチ含浸することで、得られる黒鉛材料のかさ密度や強度が高くなり電気比抵抗が低下する。
　得られた焼成体は、黒鉛化炉で2800～3000℃の範囲で熱処理して黒鉛化することで黒鉛材料を得ることができる。黒鉛化温度は高いほど黒鉛の結晶子のサイズが大きくなり、結晶性が高くなるので、熱処理温度は3000℃が望ましい。
　黒鉛基材の電気比抵抗分布のバラツキを抑制するには、黒鉛化時の熱処理温度が均一になるように行えばよい。一般に黒鉛化炉はアチソン炉あるいは高周波誘導炉が使用されるが、黒鉛基材のサイズが大きくなるほど電気比抵抗分布のバラツキは大きくなりやすいので、アチソン炉より高周波誘導炉を利用することが望ましい。
　黒鉛基材の物性値は、テストピース/TP（10ｘ10ｘ50mm）を黒鉛基材の任意の場所から切り出して、かさ密度、熱膨張係数、曲げ強度、電気比抵抗を測定した。
　かさ密度は、テストピースの重量と体積を実測して算出される。熱膨張係数は、差動トランスを装備した市販の熱分析装置を用いて、テストピースを室温から500℃まで加熱した時の線膨張率を測定して算出した。曲げ強度は、JIS R 7222：1997(黒鉛素材の物理特性測定方法)を参考にして支点間の距離40mm、荷重速度0.5mm/minで破壊したときの最大荷重を測定して算出した。電気比抵抗は、JIS R 7222：1997(黒鉛素材の物理特性測定方法)による電圧降下法で測定した。
　サセプターとして使用できる黒鉛基材の物性としては、例えば、かさ密度が１．７０～１．８０g/cm3、熱膨張係数が３．５～４．５ｘ１０-6/K、曲げ強度が３５～６０ＭＰａ、電気比抵抗（ρ0）が８．０～１３．０μΩｍが挙げられる。
（セラミックコーティング層）
　本発明のサセプターは、黒鉛材料をサセプターの形状に機械加工した黒鉛基材を好ましくはCVD法によってセラミック被膜でコーティングされたものである。
　セラミックコーティング層は、SiC、TaC、又はPBNの少なくとも１種の材料であることが望ましい。特に、同種又は異種材料を2層以上積層してなるものが好ましい。セラミックコーティング層の厚みは、好ましくは５０～２００μｍである。
　サセプターは高温でNH3、H2等の反応性ガスに曝されるので、これらのガスに対して耐食性が優れた上記セラミック被膜をサセプターにコーティングすることによって繰返しの使用が可能となる。
　黒鉛基材の表面をセラミック被膜でコーティングする方法はCVD法を用いた公知の方法による。
　以下、本発明を実施例に基づいて具体的に説明するが、本発明のサセプターはこれらの実施例の内容によって制限されるものではない。
実施例1
　骨材原料として、アモルファスコークスと針状コークスをアトマイザー粉砕機により最大粒径200μmまで個別に粉砕して其々平均粒径15μmの骨材を得た。各骨材の粒径はレーザー回折式粒度分布測定装置を用いて測定して得た値であり、平均粒径はメジアン径として示した。
　アモルファスコークス粉40重量部と針状コークス粉60重量部を配合して骨材とした。
　この骨材100重量部をバインダーピッチ70重量部と共にニーディング装置に投入し、220℃で加熱しながら10時間混練した。この混練物を冷却後、最大粒径250μmまで再粉砕して成形用の二次粉末を得た。これをラバーケースに充填して冷間静水圧プレス(CIP)により1t/cm2の圧力で成形した。得られた成形体を焼成炉に詰めて、非酸化性雰囲気で1000℃まで焼成炭化処理して焼成体を得た。得られた焼成体は含浸用ピッチを含浸して再度1000℃で焼成した。これを高周波誘導炉（HF）に移して、非酸化性雰囲気で3000℃まで加熱して黒鉛化することで黒鉛材料を得た。
　得られた黒鉛材料から、ドーナツ型のサセプター形状に黒鉛基材を複数加工した。そのうちの1枚から黒鉛材料のテストピース（10ｘ10ｘ50mm）を切り出して、室温における物性値を測定した（表2）。
　電気比抵抗の分布は、黒鉛基材の面内について図５に示した16箇所の電気比抵抗を測定して得た。電気比抵抗の測定は、ダイアインスツルメンツ社製抵抗率計（ロレスタ-EP）を用いて行った。得られた電気比抵抗について、平均値ρav、最大値ρmax、最小値ρminを表2に示した。この結果を用いて計算された電気比抵抗のバラツキ(ρmax./ρmin)を表3に示した。
　高温の電気比抵抗の特性は、黒鉛基材から切出した黒鉛試料（φ10ｘ100mm）を図６の装置にセットして測定された抵抗値を用いて、室温に対する各温度の相対値(ρt /ρ0)として示した（図７）。800℃と1600℃における相対値を用いて電気比抵抗の高温変化率（ρ1600/ρ800）を算出して表3に示した。
　サセプター形状に加工した黒鉛基材は、純化炉に入れて高温下Cl2ガスで精製してから、CVD炉に入れて高温下SiCl4とC3H8の混合ガスをH2キャリアガスと共に導入し、黒鉛基材の表面に厚さ100μm（50μmを2回コート）のSiC被膜を形成してサセプターを得た。
　このサセプターをエピタキシャル成長装置(A)に設置して、4インチのサファイア基板11枚を載せて、MOCVD法によりGaN被膜をプロセス時間8時間で積層してLED向けウエハ製品(目標波長443nm)を作製した。
　得られたウエハ製品の活性層をフォトルミネッセンス(PL)分析装置で面内1×1mm間隔で測定して、ウエハ毎に統計処理して11枚を平均した結果、PL波長は平均値443.8nm、標準偏差(STD)1.3であった。サセプターを繰り返し使用した結果、200サイクルを越えて使用することができた。
実施例2
　アモルファスコークス粉50重量部と針状コークス粉50重量部を配合して骨材とした以外は、実施例1と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例1と同じ手順でウエハ製品を作製してPL波長を測定した。その結果、PL波長は平均値443.5nm、標準偏差1.4であった。サセプターを繰り返し使用した結果、200サイクルを越えて使用することができた。
実施例3
　骨材原料として、針状コークスで製造された人造黒鉛材料の切削粉をアトマイザー粉砕機で粉砕して平均粒径70μmの骨材を得た。
　アモルファスコークス粉67重量部と上記の人造黒鉛粉33重量部を配合して骨材としたこと、得られた焼成体にピッチを含浸することなく黒鉛化処理したこと以外は、実施例1と同一方法により黒鉛材料を得た。
　この黒鉛材料からサセプター形状に加工した黒鉛基材を得た後、実施例1と同一方法によりサセプターを得た。
　このサセプターをエピタキシャル成長装置(B)に設置して、4インチのサファイア基板14枚を載せて、MOCVD法によりGaN被膜をプロセス時間8時間で積層してLED向けウエハ製品(目標波長443nm)を作製した。
　得られたウエハ製品の活性層をフォトルミネッセンス(PL)分析装置で面内1×1mm間隔で測定して、ウエハ毎に統計処理して14枚を平均した結果、PL波長は平均値443.2nm、標準偏差1.6であった。サセプターを繰り返し使用した結果、200サイクルを越えて使用することができた。
実施例4
　アモルファスコークス粉60重量部と針状コークス粉40重量部を配合して骨材としたこと以外は、実施例3と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例3と同じ手順でウエハ製品を作製してPL波長を測定した。その結果、PL波長は平均値443.6nm、標準偏差1.7であった。サセプターを繰り返し使用した結果、200サイクルを越えて使用することができた。
実施例5
　アモルファスコークス粉70重量部、針状コークス粉30重量部を配合して骨材とした以外は、実施例3と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例3と同じ手順でウエハ製品を作製してPL波長を測定した。その結果、PL波長は平均値444.1nm、標準偏差(STD)1.8であった。サセプターを繰り返し使用した結果、200サイクルを越えて使用することができた。
比較例1
　アモルファスコークスをアトマイザー粉砕機により最大粒径30μmまで粉砕して得た平均粒径5μmの粉末60重量部と、針状コークスをアトマイザー粉砕機により最大粒径200μmまで粉砕した後、分級機により投入量の30%の微粉を除去して得た平均粒径50μmの粉末40重量部を配合して骨材としたこと、得られた焼成体にピッチを含浸することなく黒鉛化処理したこと以外は、実施例1と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例1と同じ手順でウエハ製品を作製してPL波長を測定した。その結果、PL波長は平均値447.8nm、標準偏差(STD)1.6であり、PL波長が上記目標値より外れてウエハ製品は不良になった。このためサセプターの使用を中止した。
比較例2
　アモルファスコークス粉80重量部と針状コークス粉20重量部を配合して骨材とした以外は、実施例1と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例1と同じ手順でウエハ製品を作製してPL波長を測定した。PL波長が上記目標値より外れてウエハ製品は不良になった。このためサセプターの使用を中止した。
比較例3
　アモルファスコークス粉50重量部と針状コークス粉50重量部を配合して骨材としたこと、焼成体にピッチ含浸して再度1000℃で焼成した後、黒鉛化処理をアチソン炉（AC）で2500℃としたこと以外は、実施例3と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例3と同じ手順でウエハ製品を作製してPL波長を測定した。PL波長、STD共に上記目標値又は規格値より外れてウエハ製品は不良になった。サセプターは１回の使用でSiC被膜が破損したので使用を中止した。
比較例4
　焼成体にピッチ含浸して再度1000℃で焼成した後、黒鉛化処理を2500℃としたこと以外は、実施例4と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例4と同じ手順でウエハ製品を作製してPL波長を測定した。PL波長が上記目標値より外れてウエハ製品は不良になった。このためサセプターの使用を中止した。
比較例5
　焼成体にピッチ含浸して再度1000℃で焼成した後、黒鉛化処理を2500℃としたこと以外は、実施例5と同一方法によりサセプターを得た。
　このサセプターを用いて、実施例5と同じ手順でウエハ製品を作製したが、ウエハ製品の品質は合格したものの、温度応答性が劣り、プロセス時間を10時間とせざるを得なかった。
　用いられた骨材と黒鉛化条件について表1に示した。得られた黒鉛基材の物性値について表2に示した。得られたサセプターの評価結果を表3にまとめた。

Figure JPOXMLDOC01-appb-T000001
  
Figure JPOXMLDOC01-appb-T000002
  
Figure JPOXMLDOC01-appb-T000003
  
（備考）
＊　　：PL波長が目標値（443nm）より外れてウエハ製品が不良になり、サセプターの使用を中止
＊＊　：ウエハ製品が不良になり、かつサセプターが破損し、サセプターの使用を中止
＊＊＊：プロセス時間の延長により生産性が劣り、サセプターの使用を中止
○　　：PL波長が所定範囲内に収まりウエハ製品が良好であり、生産性にも優れ、サセプターとして良好に使用できるもの
×　　：サセプターとして使用不可なもの
　表3の結果より、実施例1～5の本発明の範囲にある黒鉛基材を用いたサセプターでは、MOCVD法で製造されたウエハ製品のPL波長(平均値)は、目標値の443±3nm以内、標準偏差(STD)は2未満であり品質規格を満足した。
　これに対して、電気比抵抗の高温変化率(ρ1600/ρ800)が1.3より大きい比較例1と1.14未満の比較例2,3,4は、サセプターの温度が安定しなかったのでPL波長は±3nm以上外れた。また、電気比抵抗のバラツキ(ρmax/ρmin)が1.05を超す比較例3は、サセプターの温度のバラツキが大きいので標準偏差(STD)は3を超えて大きく、更に熱応力によってコーティング被膜は割れた。
　電気比抵抗の高温変化率ρ1600/ρ800が1.14未満の比較例5は、サセプターの温度の応答性が低いものの、プロセス時間を10時間に延長することによってウエハ製品の品質を合格した。しかしながら、ウエハ製品の生産性が低下したので量産向けには使用できなかった。
　本発明は気相エピタキシャル成長を行う際に使用されるサセプターに好適に利用できる。
　１　　　サセプター
　１Ａ　　黒鉛試料（黒鉛基材）
　５　　　ウエハ
　１１　　ウエハ製品
　１２　　サファイア基板（ウエハ） 

Claims (2)

  1. 　誘導加熱によって発熱するサセプターであって、黒鉛基材とセラミックコーティング層を有し、黒鉛基材の室温における面内の電気比抵抗分布のバラツキ（ρmax/ρmin）が1.00～1.05であり、800℃と1600℃の電気比抵抗の高温変化率（ρ1600/ρ800）が1.14～1.30であることを特徴とするサセプター。
  2. 　上記セラミックコーティング層は、SiC、TaC、及びPBN（熱分解窒化ホウ素）から選ばれる少なくとも１種の材料であることを特徴とする請求項１に記載のサセプター。
      
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