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WO2016080450A1 - Procédé de croissance en phase vapeur - Google Patents

Procédé de croissance en phase vapeur Download PDF

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Publication number
WO2016080450A1
WO2016080450A1 PCT/JP2015/082425 JP2015082425W WO2016080450A1 WO 2016080450 A1 WO2016080450 A1 WO 2016080450A1 JP 2015082425 W JP2015082425 W JP 2015082425W WO 2016080450 A1 WO2016080450 A1 WO 2016080450A1
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WO
WIPO (PCT)
Prior art keywords
reaction chamber
gas
film
wafer
vapor phase
Prior art date
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Ceased
Application number
PCT/JP2015/082425
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English (en)
Japanese (ja)
Inventor
佐藤　裕輔
拓未 山田
英志 高橋
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Nuflare Technology Inc
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Nuflare Technology Inc
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Filing date
Publication date
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Publication of WO2016080450A1 publication Critical patent/WO2016080450A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H10P14/2905—
    • 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
    • H10P14/24—
    • H10P14/2926—
    • H10P14/3216—
    • H10P14/3248—
    • H10P14/3416—

Definitions

  • the present invention relates to a vapor phase growth method for forming a film by supplying a gas.
  • a method of forming a high-quality semiconductor film there is an epitaxial growth technique in which a single crystal film is grown on a wafer by vapor phase growth.
  • a vapor phase growth apparatus using an epitaxial growth technique a wafer is placed on a support in a reaction chamber that is maintained at normal pressure or reduced pressure. Then, while heating the wafer, a process gas such as a source gas, which is a raw material for film formation, is supplied to the wafer surface from, for example, a shower plate above the reaction chamber. A thermal reaction of the source gas occurs on the wafer surface, and an epitaxial single crystal film is formed on the wafer surface.
  • a process gas such as a source gas, which is a raw material for film formation
  • Patent Document 1 describes a method of forming an AlN (aluminum nitride) buffer layer on a Si wafer and a method of desorbing hydrogen atoms on the surface of the Si wafer before forming GaN.
  • Patent Document 2 describes a method of flowing chlorine gas in order to remove deposits from chamber components in the process of forming a GaN-based semiconductor film using MOCVD.
  • a support portion 12 is provided in the reaction chamber 10 below the shower plate 11 and on which, for example, a wafer W, which is a semiconductor substrate, can be placed.
  • the support unit 12 may be, for example, an annular holder having an opening at the center as shown in FIG. 1 or a susceptor having a structure in contact with almost the entire back surface of the wafer W.
  • the rotating body unit 14 which rotates by arrange
  • the rotating body unit 14 has a rotating shaft 18 connected to a rotation driving mechanism 20 positioned below.
  • the rotation drive mechanism 20 can rotate the wafer W around the center of rotation, for example, at 50 rpm or more and 1000 rpm or less.
  • the diameter of the cylindrical rotating body unit 14 is substantially the same as the outer diameter of the support portion 12.
  • the rotating shaft 18 is rotatably provided at the bottom of the reaction chamber 10 via a vacuum seal member.
  • a wafer inlet / outlet and a gate valve (not shown) for loading / unloading a wafer are provided at the side wall portion of the reaction chamber 10.
  • the wafer W is configured to be transferred by a handling arm (not shown) between, for example, a load lock chamber (not shown) and the reaction chamber 10 connected by the gate valve.
  • a handling arm formed of synthetic quartz can be inserted into the space between the shower plate 100 and the support portion 12.
  • FIG. 2 is a process flow diagram of the vapor phase growth method of the present embodiment.
  • the vapor phase growth method of this embodiment is performed using the single wafer type epitaxial growth apparatus shown in FIG.
  • the vapor phase growth method of the present embodiment includes a first substrate carry-in step (S10), an AlN film formation step (S11), a GaN film formation step (S12), a first substrate carry-out step (S14), and a cleaning step (S16). ), A second substrate carry-in step (S18), an AlN film formation step (S20), a GaN film formation step (S22), and a second substrate carry-out step (S24).
  • a first substrate for example, a first wafer W1, which is a (111) -plane Si wafer
  • a first wafer W1 which is a (111) -plane Si wafer
  • a gate valve at the wafer entrance / exit of the reaction chamber 10 is opened, and the first wafer W1 in the load lock chamber is transferred into the reaction chamber 10 by a handling arm (not shown).
  • baking for example, hydrogen gas is supplied to the reaction chamber 10 through the gas supply unit 13. After baking for a predetermined time, for example, the heating output of the heating unit 16 is lowered to set the first wafer W1 to an epitaxial growth temperature, for example, 1000 ° C. or higher and 1100 ° C. or lower.
  • process gas is supplied from the gas supply unit 13 into the reaction chamber 10 via the shower plate 11.
  • AlN aluminum nitride
  • the process gas is, for example, trimethylaluminum (TMA), ammonia (NH 3 ), and hydrogen gas (H 2 ) as a carrier gas.
  • TMA trimethylaluminum
  • NH 3 ammonia
  • H 2 hydrogen gas
  • Trimethylaluminum (TMA) is a source gas of aluminum (Al)
  • ammonia (NH 3 ) is a source gas of nitrogen (N).
  • process gas is supplied from the gas supply unit 13 into the reaction chamber 10 via the shower plate 11.
  • a GaN (gallium nitride) film as the first film is formed on the surface of the AlN film of the first wafer W1 by epitaxial growth (S12).
  • the process gas includes a source gas containing gallium (Ga).
  • the process gas is, for example, trimethylgallium (TMG), ammonia (NH 3 ), and hydrogen gas (H 2 ) as a carrier gas.
  • TMG trimethylgallium
  • NH 3 ammonia
  • H 2 hydrogen gas
  • Trimethylgallium (TMG) is a gallium (Ga) source gas
  • ammonia (NH 3 ) is a nitrogen (N) source gas.
  • the reaction product adheres to the portions other than the first wafer W1 in the reaction chamber 10 as deposits.
  • a large amount of deposits adhere to the region of the support portion 12 where the reaction is promoted at a high temperature that is not covered with the wafer.
  • the deposit is, for example, GaN.
  • the film formed as the first film is not limited to GaN as long as the film is formed by supplying a source gas containing gallium (Ga).
  • Ga gallium
  • InGaN indium gallium nitride
  • AlGaN aluminum gallium nitride
  • GaAs gallium arsenide
  • the supply of the source gas from the gas supply unit 13 is stopped, the supply of the source gas onto the first wafer W1 is shut off, and only the hydrogen gas (H 2 ) of the carrier gas flows, The growth of the crystal film is finished.
  • the temperature of the first wafer W1 starts to be lowered.
  • the first wafer W1 on which the GaN single crystal film is formed is placed on the support unit 12, and the heating output of the heating unit 16 is stopped and lowered to a predetermined temperature.
  • the rotation of the rotating body unit 14 is stopped.
  • the push-up pins are raised to detach the first wafer W1 from the support portion 12.
  • the gate valve is opened again, and the handling arm is inserted between the shower plate 11 and the support portion 12.
  • the push-up pin is lowered and the first wafer W1 is placed on the handling arm.
  • the first wafer W1 which is the first substrate, is carried out of the reaction chamber 10 (S14).
  • cleaning is performed by supplying a cleaning gas containing chlorine atoms into the reaction chamber 10 (S16). By the cleaning, the deposits attached to the support portion 12 are removed.
  • a dummy wafer may be placed on the support portion 12.
  • the support portion 12 is an annular holder having an opening at the center as shown in FIG. 1, it is desirable to place a dummy wafer in order to protect the heating portion 16 and the like from the cleaning gas.
  • a second wafer having a silicon (Si) surface different from the first wafer W1 is carried into the reaction chamber 10 (S18).
  • the second wafer is, for example, a second wafer W2 that is a Si wafer having a (111) surface.
  • the second wafer W2 is loaded into the reaction chamber 10 in the same manner as the first wafer W1.
  • a vacuum pump (not shown) is operated to exhaust the gas in the reaction chamber 10 from the gas discharge unit 26 through a pressure adjusting valve (not shown) to a predetermined pressure.
  • the second wafer W ⁇ b> 2 placed on the support unit 12 is heated by the heating unit 16.
  • the heating output of the heating unit 16 is increased to raise the temperature of the second wafer W2 to a predetermined temperature, for example, a temperature of 1150 ° C. or higher and 1250 ° C. or lower.
  • baking for example, hydrogen gas is supplied to the reaction chamber 10 through the gas supply unit 13. After baking for a predetermined time, for example, the heating output of the heating unit 16 is lowered to set the second wafer W2 to an epitaxial growth temperature, for example, 1000 ° C. or higher and 1100 ° C. or lower.
  • the process gas is, for example, trimethylaluminum (TMA), ammonia (NH 3 ), and hydrogen gas (H 2 ) as a carrier gas.
  • TMA trimethylaluminum
  • NH 3 ammonia
  • H 2 hydrogen gas
  • Trimethylaluminum (TMA) is a source gas of aluminum (Al)
  • ammonia (NH 3 ) is a source gas of nitrogen (N).
  • the film formed as the second film is not limited to AlN.
  • any film that does not hinder the growth may be used.
  • thin SiN silicon nitride
  • SiN silicon nitride
  • a third film for example, a GaN single crystal film is grown on the AlN film (second film) (S22).
  • a process gas for forming the GaN film is supplied from the gas supply unit 13.
  • the temperature of the second wafer W2 is, for example, not less than 1000 ° C. and not more than 1100 ° C.
  • the process gas includes a source gas containing gallium (Ga).
  • the process gas is, for example, trimethylgallium (TMG), ammonia (NH 3 ), and hydrogen gas (H 2 ) as a carrier gas.
  • TMG trimethylgallium
  • NH 3 ammonia
  • H 2 hydrogen gas
  • Trimethylgallium (TMG) is a gallium (Ga) source gas
  • ammonia (NH 3 ) is a nitrogen (N) source gas.
  • the film formed as the third film is not limited to GaN.
  • InGaN indium gallium nitride
  • AlGaN aluminum gallium nitride
  • GaAs gallium arsenide
  • the supply of the source gas from the gas supply unit 13 is stopped, the supply of the source gas onto the second wafer W2 is shut off, and the growth of the GaN single crystal film is completed.
  • the temperature of the second wafer W2 starts to be lowered.
  • the second wafer W2 on which the GaN single crystal film is formed is placed on the support unit 12, and the heating output of the heating unit 16 is stopped and adjusted so as to decrease to a predetermined temperature.
  • the second wafer W2 which is the second substrate, is unloaded from the reaction chamber 10 (S24).
  • the first wafer W1 is unloaded and the vapor phase growth apparatus is used. Cleaning is performed while heating the support 12. That is, the cleaning is performed in a state where there is no wafer or only a dummy wafer in which no film is formed in the reaction chamber 10.
  • deposits attached to the support portion 12 are removed particularly during the film formation of the first wafer W1. It can be considered that this deposit contains Ga (gallium) that is flowed as a process gas when the first wafer W1 is formed.
  • the present embodiment by removing the deposit containing Ga, the Ga that has been present as the deposit when the second film is formed on the second wafer W2 after the cleaning is removed from the second wafer W2.
  • the reaction with Si on the surface of the wafer W2 is avoided. Therefore, it is possible to form a high quality film on the second wafer W2. That is, according to the present embodiment, it is possible to provide a vapor phase growth method for forming a high-quality film on Si in the same reaction chamber in which a gas containing Ga is supplied. After the film containing Ga is formed on the second wafer W2, cleaning can be performed in the same manner, and a high-quality film can be similarly formed on the wafer whose surface is Si.
  • FIG. 3 is a process flow diagram of the vapor phase growth method of the present embodiment.
  • the vapor phase growth method of this embodiment is performed using the single wafer type epitaxial growth apparatus shown in FIG.
  • hydrogen baking is performed after cleaning (S16).
  • the hydrogen baking is performed by supplying hydrogen gas (H 2 ) as a baking gas into the reaction chamber 10 and performing a heat treatment.
  • the heating output of the heating unit 16 is decreased while the hydrogen gas from the gas supply unit 13 is being supplied, and the temperature of the support unit 12 is decreased.
  • Hydrogen gas has the effect of etching GaN. According to the present embodiment, by performing hydrogen baking in addition to cleaning, it is possible to improve the effect of removing deposits such as GaN adhering to the support portion 12. Therefore, a higher quality film can be formed on the second wafer W2.
  • hydrogen baking is performed at a higher temperature than cleaning. By performing the cleaning at a higher temperature than the cleaning, the desorption of the gas adsorbed on the inner wall of the reaction chamber 10 or the members in the reaction chamber 10 is promoted.
  • the temperature of hydrogen baking is preferably 1100 ° C. or higher and 1250 ° C. or lower, and more preferably 1150 ° C. or higher and 1200 ° C. or lower. It is because it will become difficult to improve the removal effect of the deposit
  • the temperature of hydrogen baking be higher than the film formation temperature when forming the second film and the third film on the second wafer.
  • FIG. 4 is a process flow diagram of the vapor phase growth method of the present embodiment.
  • the vapor phase growth method of this embodiment is performed using the single wafer type epitaxial growth apparatus shown in FIG.
  • the cleaning (S16) is omitted from the process flow of the vapor phase growth method of the second embodiment shown in FIG.
  • FIG. 5 is a process flow diagram of the vapor phase growth method of the present embodiment.
  • the vapor phase growth method of this embodiment is performed using the single wafer type epitaxial growth apparatus shown in FIG.
  • cleaning gas discharge (S28) and ammonia supply (S30) are performed after cleaning (S16).
  • the process up to cleaning (S16) is the same as in the first embodiment.
  • supply of the cleaning gas from the gas supply unit 13 is stopped.
  • the craning gas in the reaction chamber 10 is discharged by evacuation (S28).
  • ammonia is supplied from the gas supply unit 13 (S30). After supplying ammonia for a predetermined time, the supply of ammonia is stopped.
  • the chlorine atoms contained in the cleaning gas may remain on the inner surface of the reaction chamber 10 or in the piping. Then, when the chlorine atoms later form an AlN film or the like, there is a possibility that the chlorine atoms aggregate at the interface between the wafer and the AlN film or the like.
  • chlorine atoms are present at the interface, the quality of the AlN film or GaN film formed on the wafer may be deteriorated. Further, when a device is manufactured using a wafer on which an AlN film, a GaN film, or the like is formed, chlorine atoms may deteriorate characteristics with the device.
  • the cleaning gas discharge (S28) instead of evacuation, or before or after that, only supply of the cleaning gas is stopped, and hydrogen gas (H 2 ), nitrogen gas (N 2 ), argon gas (Ar) Alternatively, the cleaning gas may be purged by flowing only an inert gas such as the above or a mixed gas thereof.
  • FIG. 6 is a process flow diagram of the vapor phase growth method of the present embodiment.
  • the vapor phase growth method of this embodiment is performed using the single wafer type epitaxial growth apparatus shown in FIG.
  • the process up to hydrogen baking (S17) is the same as in the second embodiment. After the hydrogen baking is completed, for example, ammonia is supplied from the gas supply unit 13 (S30). After supplying ammonia for a predetermined time, the supply of ammonia is stopped.
  • the chlorine atoms contained in the cleaning gas may remain on the inner surface of the reaction chamber 10 or in the piping. Then, when the chlorine atoms later form an AlN film or the like, there is a possibility that the chlorine atoms aggregate at the interface between the wafer and the AlN film or the like.
  • chlorine atoms are present at the interface, the quality of the AlN film or GaN film formed on the wafer may be deteriorated. Further, when a semiconductor device is manufactured using a wafer on which an AlN film, a GaN film, or the like is formed, chlorine atoms may deteriorate characteristics with the semiconductor device.
  • a film was formed by the same process as in the second embodiment.
  • a (111) -plane Si wafer (first wafer) on which an AlN film is formed under a condition of 200 nm thickness is applied to a GaN film under a condition of a thickness of 3000 nm in a reaction chamber of a vertical single wafer type epitaxial apparatus.
  • a gas obtained by diluting TMG with hydrogen gas and ammonia were used as a source gas.
  • the Si wafer was unloaded from the reaction chamber.
  • a SiC dummy wafer was carried into the reaction chamber and heated to 1000 ° C. At this time, the temperature of the support portion is also heated to about 1000 ° C. Then, cleaning gas obtained by diluting hydrochloric acid gas with hydrogen gas to 10% by volume was supplied to the reaction chamber, and cleaning was performed for 5 minutes.
  • the dummy wafer and the support were heated to 1150 ° C. And 100 volume% hydrogen gas was supplied to the reaction chamber, and hydrogen baking was performed for 5 minutes. Thereafter, the dummy wafer was unloaded from the reaction chamber.
  • an AlN film having a thickness of 200 nm and a GaN film having a thickness of 3000 nm were epitaxially grown.
  • the temperature during the formation of the AlN film and the GaN film was 1000 ° C.
  • the Si wafer (second wafer) was carried out of the reaction chamber.
  • FIG. 7 is an optical photograph of the wafer surface of the example and the comparative example.
  • FIG. 7A shows an example
  • FIG. 7B shows a comparative example.
  • the wafer surface was a mirror surface, and it was confirmed that the AlN film and the GaN film were well formed.
  • the surface was uneven, and a clouded area was seen in the center of the wafer. In a region that was clouded by cross-sectional observation with an electron microscope, the Si wafer was etched to form holes.
  • a vertical single-wafer epitaxial apparatus for forming a film for each wafer has been described as an example.
  • the vapor phase growth apparatus is not limited to a single-wafer epitaxial apparatus.
  • the present invention can be applied to a planetary epitaxial apparatus that forms films on a plurality of wafers that revolve and revolves simultaneously, a lateral epitaxial apparatus, and the like. Further, a vapor phase growth apparatus other than the epitaxial apparatus may be used.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

La présente invention concerne, selon un de ses modes de réalisation, un procédé de croissance en phase vapeur, caractérisé par les étapes consistant à: amener un gaz source contenant du gallium (Ga) jusqu'à une chambre de réaction; former un premier film sur un premier substrat placé sur une partie de soutien dans la chambre de réaction; extraire le premier substrat de la chambre de réaction; chauffer la partie de soutien après avoir évacué le premier substrat de la chambre de réaction pour éliminer une fixation rattachée à la partie de soutien; introduire dans la chambre de réaction, un deuxième substrat qui est différent du premier substrat et présente une surface en silicium (Si), après avoir éliminé la fixation; et former un deuxième film sur le deuxième substrat placé sur la partie de soutien.
PCT/JP2015/082425 2014-11-20 2015-11-18 Procédé de croissance en phase vapeur Ceased WO2016080450A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2014235259 2014-11-20
JP2014-235259 2014-11-20

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WO2016080450A1 true WO2016080450A1 (fr) 2016-05-26

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TW (1) TW201630053A (fr)
WO (1) WO2016080450A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6439774B2 (ja) * 2016-11-21 2018-12-19 トヨタ自動車株式会社 半導体装置の製造方法
JP7188256B2 (ja) * 2019-04-18 2022-12-13 株式会社Sumco 気相成長方法及び気相成長装置

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007109928A (ja) * 2005-10-14 2007-04-26 Taiyo Nippon Sanso Corp 窒化物半導体製造装置部品の洗浄方法と洗浄装置
JP2012525708A (ja) * 2009-04-28 2012-10-22 アプライド マテリアルズ インコーポレイテッド Ｌｅｄ製造のためのｍｏｃｖｄシングルチャンバスプリットプロセス
JP2013012719A (ja) * 2011-05-31 2013-01-17 Hitachi Kokusai Electric Inc 基板処理装置および基板処理方法
JP2013062342A (ja) * 2011-09-13 2013-04-04 Toshiba Corp 成膜装置のクリーニング方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007109928A (ja) * 2005-10-14 2007-04-26 Taiyo Nippon Sanso Corp 窒化物半導体製造装置部品の洗浄方法と洗浄装置
JP2012525708A (ja) * 2009-04-28 2012-10-22 アプライド マテリアルズ インコーポレイテッド Ｌｅｄ製造のためのｍｏｃｖｄシングルチャンバスプリットプロセス
JP2013012719A (ja) * 2011-05-31 2013-01-17 Hitachi Kokusai Electric Inc 基板処理装置および基板処理方法
JP2013062342A (ja) * 2011-09-13 2013-04-04 Toshiba Corp 成膜装置のクリーニング方法

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JP2016105471A (ja) 2016-06-09

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