WO2016047972A2 - Appareil pour fabriquer un film et procédé pour fabriquer un film utilisant ledit appareil - Google Patents

Appareil pour fabriquer un film et procédé pour fabriquer un film utilisant ledit appareil Download PDF

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Publication number
WO2016047972A2
WO2016047972A2 PCT/KR2015/009824 KR2015009824W WO2016047972A2 WO 2016047972 A2 WO2016047972 A2 WO 2016047972A2 KR 2015009824 W KR2015009824 W KR 2015009824W WO 2016047972 A2 WO2016047972 A2 WO 2016047972A2
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source
container
reactor
gallium
vessel
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PCT/KR2015/009824
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English (en)
Korean (ko)
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WO2016047972A3 (fr
Inventor
이성국
심광보
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한양대학교 산학협력단
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Publication of WO2016047972A3 publication Critical patent/WO2016047972A3/fr

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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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
    • 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
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02538—Group 13/15 materials
    • H01L21/0254—Nitrides

Definitions

  • the present invention relates to a film production apparatus and a method for producing a film using the same.
  • the Republic of Korea Patent Publication No. 10-2012-0071695 Application No. 10-2010-0133341, Applicant Samsung LED Co., Ltd.
  • the susceptor body portion formed of a light transmissive material having an upper surface formed with a pocket for accommodating the substrate
  • a method for chemically vapor-depositing a susceptor including a light absorbing part formed of a light absorbing material, even if warpage occurs in the substrate, a method of uniformly heating the substrate is disclosed.
  • Korean Patent Laid-Open Publication No. 10-2002-0056194 (Application No. 10-2000-0085507, Applicant Hynix Semiconductor) discloses an ultraviolet lamp as a heater in a conventional single wafer type low pressure chemical vapor deposition apparatus.
  • a single crystal silicon fabrication apparatus is disclosed which, in connection with a halogen lamp assembly, reduces process heat load and has a high growth rate.
  • One technical problem to be solved by the present invention is to provide a high reliability film production apparatus, and a film production method using the same.
  • Another technical problem to be solved by the present invention is to provide a film production apparatus with reduced process time and manufacturing cost, and a film production method using the same.
  • Another technical problem to be solved by the present invention is to provide a film production apparatus with improved production yield, and a film production method using the same.
  • Another technical problem to be solved by the present invention is to provide a film production apparatus having a reduced dislocation density, and a film production method using the same.
  • Another technical problem to be solved by the present invention is to provide an apparatus for producing a high quality bulk monocrystalline gallium nitride film, and a method for producing a gallium nitride film using the same.
  • the problem to be solved by the present invention is not limited to the above.
  • the present invention provides a film production apparatus.
  • the membrane manufacturing apparatus is disposed in the reactor, the container (container), the first source is accommodated, the first source supply for supplying the first source in the container, and in the container, the first A second source supply for supplying a second source that reacts with the one source, wherein the container includes a bottom surface, a side extending upward from the bottom surface, and a plurality of openings provided in the side surface.
  • the container includes a bottom surface, a side extending upward from the bottom surface, and a plurality of openings provided in the side surface.
  • the first source and the second source may react to generate a reaction gas in the container, and the reaction gas may be discharged out of the container through the plurality of openings.
  • the membrane manufacturing apparatus may include a third source supply unit disposed in the reactor and supplying a third source, and disposed in the reactor and receiving the discharged reactant gas and the third source. It may further include a support for supporting the base substrate is formed.
  • the first source may include gallium (Ga)
  • the second source may include chlorine (Cl)
  • the fraudulent third source may include nitrogen (N).
  • the apparatus for manufacturing a film may include a first heating part surrounding a part of the reactor in which the container is located and supplying heat, and a second heating part surrounding a part of the reactor in which the support part is located and supplying heat.
  • the heating unit may further include.
  • the second heating unit may include supplying heat at a higher temperature than the first heating unit.
  • the first source supply unit a first source tank in which the first source is stored, a first extending from the first source tank to the inside of the container, providing a supply path of the first source It may include a source supply line, and a valve portion provided to the first source supply line, for adjusting the supply amount of the first source.
  • the first source supply unit may further include a first source heating unit for supplying heat to the first source stored in the first source tank.
  • the plurality of openings may include being provided adjacent to the upper end of the side.
  • the present invention provides a film production method.
  • the method of manufacturing a film may include preparing a base substrate on a support in a reactor, nitriding an upper surface of the base substrate, and gallium (Ga) on the upper surface of the base substrate.
  • the method may include forming a gallium nitride film by providing a reaction gas including and a source including nitrogen.
  • a vessel including a bottom surface, a side extending from the bottom surface, and a plurality of openings provided in the side is provided in the reactor, the gallium is contained in the vessel, the reaction gas is And generated in the container and provided to the upper surface of the base substrate in the container through the plurality of openings.
  • the method may further include continuously supplying gallium into the container.
  • the gallium may include a 0.057 ⁇ 0.058g / min is supplied.
  • the present invention provides a film production apparatus.
  • the apparatus for manufacturing a film may include a reactor, a support part disposed in the reactor and a base substrate disposed thereon, and a container disposed in the reactor and generating a reactive gas, wherein the container may have a bottom surface. And a side surface extending upward from the bottom surface, wherein the side surface of the container includes a plurality of openings, and the reaction gas passes through the plurality of openings of the side surface of the container to the base substrate.
  • a reactor a support part disposed in the reactor and a base substrate disposed thereon
  • a container disposed in the reactor and generating a reactive gas
  • the container may have a bottom surface.
  • a side surface extending upward from the bottom surface, wherein the side surface of the container includes a plurality of openings, and the reaction gas passes through the plurality of openings of the side surface of the container to the base substrate.
  • the apparatus may further include a first source supply providing the first source in the container, and a second source supply providing the second source in the container, wherein the first source is provided in a liquid state.
  • the second source may be provided in the container in a gaseous state.
  • the reaction gas may be generated by reacting the first source in a liquid state with the second source in a gaseous state.
  • the first source supply unit may supply heat to the first source tank on which the first source is stored, and the first source tank to supply liquid to the first source in the first source tank. It may include a first source heating to maintain the.
  • the first source may be gallium
  • the second source may be hydrogen chloride (HCl) gas.
  • one end of the first source supply part from which the first source is discharged and one end of the second source supply part from which the second source is discharged may be disposed in the container.
  • the bottom surface of the container is circular
  • the side of the container extends up along the outer peripheral surface of the bottom surface
  • the top of the container may be open (open).
  • a first source may be accommodated in a container and a second source may be introduced into the container.
  • the first source and the second source may be reacted to generate a reaction gas in the vessel.
  • the reaction gas may be discharged through a plurality of openings provided in the sidewall of the container, and may be smoothly provided on the base substrate.
  • the first source may be continuously supplied into the vessel depending on the amount by which the first source is reduced by the generation of the reaction gas. For this reason, the change of the production amount and supply amount of the reaction gas can be minimized.
  • a film production apparatus which reduces processing time and manufacturing cost, improves production yield, and can produce a thick bulk single crystal film on the base substrate.
  • FIG. 1 is a view for explaining a film production apparatus according to an embodiment of the present invention.
  • FIG. 2 is an enlarged perspective view illustrating a container included in a film production apparatus according to an embodiment of the present invention.
  • FIG. 3 is a flowchart illustrating a film production method using a film production apparatus according to an embodiment of the present invention.
  • FIG. 4 is a photograph of a gallium nitride film prepared according to a comparative example of the embodiment of the present invention.
  • FIG. 5 is a photograph of a gallium nitride film prepared according to an embodiment of the present invention.
  • first, second, and third are used to describe various components, but these components should not be limited by these terms. These terms are only used to distinguish one component from another. Thus, what is referred to as a first component in one embodiment may be referred to as a second component in another embodiment.
  • first component in one embodiment may be referred to as a second component in another embodiment.
  • second component in another embodiment.
  • Each embodiment described and illustrated herein also includes its complementary embodiment.
  • the term 'and / or' is used herein to include at least one of the components listed before and after.
  • connection is used herein to mean both indirectly connecting a plurality of components, and directly connecting.
  • FIG. 1 is a view for explaining a film production apparatus according to an embodiment of the present invention
  • Figure 2 is an enlarged perspective view for explaining a container included in the film production apparatus according to an embodiment of the present invention.
  • a membrane manufacturing apparatus includes a reactor 100, a container 105 in the reactor 100, a first source supply unit 110, and a first source supply unit 110. And a second source supply unit 120, a third source supply unit 130, a carrier gas supply unit 140, a first heating unit 151, a second heating unit 152, a support unit 160, and an outlet 170. can do.
  • the vessel 105 is disposed in the reactor 100 and includes a bottom surface 105a, a side surface 105b extending upward from the bottom surface 105a, and a plurality of openings 105c provided in the side surface 105b, opening).
  • the plurality of openings 105c may be disposed adjacent to an upper end of the side surface 105b.
  • the container 105 may accommodate the first source S1.
  • the first source S1 may be gallium (Ga) melt.
  • the first source S1 may be accommodated in the container 105 such that the first source S1 does not flow out of the container 105 by the plurality of openings 105c of the container 105.
  • the plurality of openings 105c of the container 105 have been described as being circular, but the shape of the plurality of openings 105c is not limited thereto, and may be oval, polygonal, or grooved. Etc. may be provided in various forms.
  • the first source supply unit 110 may supply the first source S1 into the container 105.
  • the first source supply unit 110 may continuously provide the first source S1 in the container 105 to maintain the first source S1 at a predetermined level.
  • the first source supply unit 110 may be configured such that the first source S1 is not leaked out of the container 105 by the plurality of openings 105c of the container 105. S1) can be supplied to the container 105.
  • the first source supply unit 110 includes a first source tank 112 in which the first source S1 is stored, and extends into the container 105 from the first source tank 112 to the first source.
  • a first source supply line 114 providing a supply path of S1, and a valve unit 116 provided to the first source supply line 114 and adjusting a supply amount of the first source S1. can do.
  • the first source supply unit 110 may further include a first source heating unit 118 that supplies heat to the first source S1 stored in the first source tank 112. According to one embodiment, by the heat provided by the first source heating unit 118, the first source (S1) may be stored in the first source tank 112 in a liquid state. Thus, the first source supply unit 110 can stably supply the first source S1 into the container 105.
  • the second source supply unit 120 may supply a second source S2 into the container 105.
  • the second source S1 may react with the first source S1 accommodated in the container 105 to generate a reaction gas RG.
  • the second source S2 includes chlorine (Cl) and the reaction gas (RG) May include gallium (Ga) and chlorine (Cl).
  • the second source S2 may include HCl gas.
  • the first source (S1) and the second source (S2) may react as shown in ⁇ Formula 1>, to generate a GaCl reaction gas.
  • the reaction gas RG generated in the vessel 105 may be efficiently discharged to the outside of the vessel 105 through the plurality of openings 105c of the vessel 105.
  • the second source supply unit 120 may supply a carrier gas (for example, nitrogen gas, etc.) into the container 105 together with the second source S2. Accordingly, the second source S2 may be efficiently supplied to the container 105.
  • a carrier gas for example, nitrogen gas, etc.
  • the third source supply unit 130 may be disposed in the reactor 100 to supply a third source S3.
  • the third source S3 may include nitrogen.
  • the third source S3 may be NH 3 gas.
  • the carrier gas supply unit 140 may be disposed in the reactor 100 to supply a carrier gas CG.
  • the carrier gas CG may be nitrogen gas.
  • the support part 160 may include a support plate 162 supporting the base substrate 200, and a support rod 164 connected to the support plate 162.
  • the support plate 162 may be rotated by the support rod 164 with a rotation axis.
  • the source S3 may be provided on the base substrate 200.
  • the film 210 may be formed on the base substrate 200 by the reaction of the reaction gas RG and the third source S3.
  • the reaction gas RG is GaCl and the third source S3 is NH 3 gas
  • the reaction gas RG is GaCl and the third source S3 is NH 3 gas
  • the base substrate 200 on the base substrate 200, according to the following ⁇ Formula 2>
  • the gallium nitride film can be formed.
  • the first heating unit 151 and the second heating unit 152 may surround the reactor 100. Specifically, the first heating unit 151 surrounds a part of the reactor 100 in which the container 105 is located, and the second heating unit 152 is the reactor 100 in which the support unit 160 is located. Can surround a portion of the.
  • the first heating unit 151 and the second heating unit 152 may supply heat of different temperatures into the reactor 100, respectively.
  • the first heating unit 151 may be configured to efficiently generate the reaction gas RG by allowing the first source S1 and the second source S2 to react efficiently in the container 105. It can supply heat.
  • the second heating unit 152 may supply heat to easily generate the film 210 on the base substrate 200 by the reaction gas RG and the third source S2. have. According to an embodiment, the second heating unit 152 may supply heat at a higher temperature than the first heating unit 151.
  • Residual gas remaining after the reaction gas RG and the third source S3 are reacted, and other gases may be discharged to the outside of the reactor 100 through the outlet 170.
  • the first source S1 and the second source S2 may be reacted to generate the reaction gas RG.
  • the reaction gas RG may be efficiently discharged to the outside of the container 105 through the plurality of openings 105c provided in the sidewall 105b of the container 105.
  • the supply of the reaction gas RG onto the base substrate 200 may be smooth.
  • the first source S1 may be continuously supplied into the vessel 105 by the first source supply unit 110, so that the production amount of the reaction gas RG may be maintained substantially constant. have. As a result, a change in the amount of the reaction gas RG supplied onto the base substrate 200 may be minimized.
  • the reaction gas RG may not be smoothly discharged to the outside of the container 105.
  • the first source supply unit 110 is omitted so that the first source S1 is not additionally supplied into the container 105, the first source received in the container 105 as the reaction proceeds. Since the amount of S1) is reduced, the amount of generation of the reaction gas RG can be reduced.
  • the growth rate of the film 210 decreases.
  • the amount of the reaction gas RG eg, GaCl
  • the third source S3 eg, NH 3
  • the reaction gas RG and the third source are reduced.
  • Defects are increased in the film 210 generated by the reaction of S3, and the film 210, for example, is caused by a large amount of the second source S2 (for example, HCl) remaining unreacted.
  • GaN is etched to deteriorate the quality of the film 210, and there is a limit to manufacturing the film 210 thickly in a single crystal state.
  • the container 105 has the plurality of openings 105c for smoothly discharging the reaction gas RG into the container 105,
  • the first source S1 may be continuously supplied to the container 105 by the first source supply unit 110.
  • a film production apparatus can be provided, which reduces processing time and manufacturing cost, improves production yield, and can produce a single bulk film in the form of a thick bulk.
  • FIG. 3 a film manufacturing method using a film manufacturing apparatus according to an embodiment of the present invention described with reference to FIGS. 1 and 2 will be described.
  • FIG. 3 is a flowchart illustrating a film production method using a film production apparatus according to an embodiment of the present invention.
  • the base substrate 200 is prepared on the support part 160 in the reactor 100 (S110).
  • the base substrate 200 may be a sapphire substrate.
  • the base substrate 200 may be any one of a semiconductor substrate, a compound semiconductor substrate, a glass substrate, a metal substrate, and a plastic substrate.
  • the base substrate 200 may be flexible.
  • An upper surface of the base substrate 200 may be nitrided (S120). As described with reference to FIG. 1, when the third source S3 includes nitrogen and the carrier gas CG is nitrogen gas, the upper surface of the base substrate 200 is the third surface. Nitriding may be performed by the source supply unit 130 and the third source S3 and the carrier gas CG provided by the carrier gas supply unit 140.
  • a reaction gas RG and the third source S3 are provided on the upper surface of the base substrate 200 to form a film 210. It may be (S130). As described with reference to FIG. 1, when the reaction gas RG includes gallium and the third source S3 includes nitrogen, the film 210 may be a gallium nitride film.
  • the upper portion of the base substrate 200 before the film 210 is formed on the upper surface of the base layer 200 by the reaction of the reaction gas RG and the third source S3.
  • the surface may be nitrided to improve the quality of the film 210.
  • the reaction gas RG is generated in the vessel 105 as described with reference to FIGS. 1 and 2, and through the plurality of openings 105c of the vessel 105, the base substrate ( 200 may be provided to the upper surface.
  • the reaction gas RG is generated by the reaction of the first source S1 accommodated in the vessel 105 and the second source S2 provided by the second source supply unit 120, the reaction gas RG is generated.
  • the amount of the first source S1 contained in the vessel 105 can be reduced.
  • the first source supply unit 110 may be configured to supply the first source S1.
  • the container 105 can be continuously supplied.
  • a sapphire substrate was prepared as a base substrate, and gallium (Ga) as a first source, HCl as a second source, ammonia gas as a third source, and nitrogen gas as a carrier gas were prepared.
  • Ga gallium
  • HCl HCl
  • ammonia gas as a third source
  • nitrogen gas as a carrier gas
  • the source region in which the quartz container is located is heated to 800 using the first heating unit, and the temperature of the growth region in which the sapphire substrate is located is heated to 1030 using the second heating unit. It was. After pretreatment of the top surface of the sapphire substrate with nitrogen gas at 1030 for 10 minutes, nitriding treatment was performed on the top surface of the sapphire substrate by flowing 2500 sccm of ammonia gas together with the nitrogen gas.
  • Ga gallium
  • GaCl gas was generated by flowing HCl gas into the quartz container, and a gallium nitride film was grown by reacting ammonia gas and the produced GaCl gas on a sapphire substrate.
  • the ratio of ammonia gas and GaCl gas was properly adjusted, and at the same time, nitrogen gas as a carrier gas was also provided.
  • the amount of gas provided was adjusted so that the growth rate was between 50 ⁇ m / hr and 150 ⁇ m / hr to produce a gallium nitride film having a thickness of 0.3 mm and 1.0 mm.
  • the amount of gallium (Ga) reduced during the growth of gallium nitride was measured. Specifically, the amount of gallium (Ga) consumed for growth was measured by measuring the amount of gallium (Ga) contained in the quartz container before and after growth. Thereafter, the amount of gallium (Ga) consumed was divided by the growth time, and the amount of gallium (Ga) used for growth per minute was measured as shown in Table 1 below.
  • Ga amount consumed (g) Growth time (hrs) Ga amount used per minute (g / min.) 146 43 0.057 142 41 0.058 140 40 0.058
  • gallium nitride When gallium nitride was grown for 40 to 43 hours, the amount of gallium consumed was 140 to 146g, and the average amount of gallium used to grow per minute was 0.058g. This shows that in order to maintain a constant gallium (Ga) level in a constant quartz container during gallium nitride growth, it is necessary to additionally and continuously supply gallium (Ga) per minute.
  • a gallium nitride single crystal film according to an embodiment of the present invention was prepared to a thickness of 1mm.
  • FIG. 4 is a photograph of a gallium nitride film prepared according to a comparative example of an embodiment of the present invention
  • Figure 5 is a photograph of a gallium nitride film prepared according to an embodiment of the present invention.
  • the 0.3 mm thick gallium nitride single crystal surface prepared according to the comparative example is clean, but the 1.0 mm thick gallium nitride single crystal has a number of defects on the surface. That is, as the growth of gallium nitride proceeds, the amount of gallium (Ga) is reduced, and accordingly, the amount of GaCl gas, which is a reaction gas, is reduced, and thus the quality of the gallium nitride film is deteriorated due to a different III / V ratio. . In other words, when the amount of GaCl which is the reaction gas is not controlled by the additional supply of gallium (Ga), it can be seen that it is not easy to manufacture a high quality bulk gallium nitride single crystal film.
  • the surface of the gallium nitride single crystal grown to a thickness of 1mm according to the embodiment of the present invention is clean and excellent in quality. That is, according to an embodiment of the present invention, by controlling the amount of gallium (Ga) constantly, supplying the reaction gas (GaCl) to the sapphire substrate smoothly and consistently, it is confirmed that an efficient method for improving the quality of the gallium nitride film Can be.
  • the film manufacturing apparatus and the film manufacturing method using the same according to an embodiment of the present invention may be used in various technical fields, such as a semiconductor, a display, a light emitting diode (LED), an organic light emitting diode (OLED), a secondary battery, and the like.
  • a semiconductor such as a semiconductor, a display, a light emitting diode (LED), an organic light emitting diode (OLED), a secondary battery, and the like.

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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

La présente invention concerne un appareil pour fabriquer un film. L'appareil pour fabriquer un film comprend : un contenant qui est disposé à l'intérieur d'un réacteur et dans lequel une première source est logée ; une unité d'alimentation de première source pour fournir la première source dans le contenant ; et une unité d'alimentation de seconde source pour fournir, dans le contenant, une seconde source qui réagit avec la première source. Le contenant peut comprendre : une surface inférieure ; une surface latérale qui s'étend vers le haut à partir de la surface inférieure ; et une pluralité d'ouvertures prévues sur la surface latérale.
PCT/KR2015/009824 2014-09-23 2015-09-18 Appareil pour fabriquer un film et procédé pour fabriquer un film utilisant ledit appareil WO2016047972A2 (fr)

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KR102536979B1 (ko) * 2021-11-10 2023-05-26 신정훈 질화갈륨 단결정 성장을 위한 하이드라이드 기상 증착 장비
KR102536978B1 (ko) * 2021-11-10 2023-05-26 신정훈 질화갈륨 단결정 성장을 위한 하이드라이드 기상 증착 장비
KR102489127B1 (ko) * 2021-11-10 2023-01-13 신정훈 질화갈륨 단결정 성장을 위한 하이드라이드 기상 증착 장비
KR102489015B1 (ko) * 2021-11-10 2023-01-13 신정훈 질화갈륨 단결정 성장을 위한 하이드라이드 기상 증착 장비
WO2024111688A1 (fr) * 2022-11-22 2024-05-30 신정훈 Appareil d'épitaxie en phase vapeur aux hydrures pour la croissance de monocristaux de nitrure de gallium

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WO2016047972A3 (fr) 2017-05-18

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