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WO2011136570A2 - Appareil et procédé de fabrication de nanopoudre de silicium - Google Patents

Appareil et procédé de fabrication de nanopoudre de silicium Download PDF

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Publication number
WO2011136570A2
WO2011136570A2 PCT/KR2011/003110 KR2011003110W WO2011136570A2 WO 2011136570 A2 WO2011136570 A2 WO 2011136570A2 KR 2011003110 W KR2011003110 W KR 2011003110W WO 2011136570 A2 WO2011136570 A2 WO 2011136570A2
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WO
WIPO (PCT)
Prior art keywords
plasma
gas
silicon
antenna
baffle
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/KR2011/003110
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English (en)
Korean (ko)
Other versions
WO2011136570A3 (fr
Inventor
홍순일
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NEST CORP
Original Assignee
NEST CORP
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Filing date
Publication date
Application filed by NEST CORP filed Critical NEST CORP
Publication of WO2011136570A2 publication Critical patent/WO2011136570A2/fr
Publication of WO2011136570A3 publication Critical patent/WO2011136570A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0875—Gas
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • Embodiments of the present invention relate to a silicon nanopowder manufacturing apparatus and method. More specifically, the present invention relates to a silicon nanopowder manufacturing apparatus and method for supplying as high power as possible in forming a nanopowder using plasma to facilitate plasma generation and to form high quality nanoparticles.
  • ICP inductive coupled plasma
  • CCP capacitive coupled plasma
  • MEMS micro-electromechanical system
  • the crystals since the crystals must be formed as small nanoparticles, when the particles bonded to the substrate through the plasma are combined with the grains before the crystals are formed, the nanoparticles cannot be easily formed when the grains become large.
  • Embodiment of the present invention is to supply a high power as possible in forming the nano-powder using the plasma to facilitate the generation of plasma and to form high-quality nanoparticles.
  • a silicon nano powder manufacturing apparatus comprising: a synthetic container having a space formed therein; A plasma gas inlet for introducing a plasma gas into the synthesis vessel; A plasma antenna for supplying power to make the plasma gas into a plasma; A plasma gas inlet for introducing a silicon process gas into the synthesis vessel; A baffle having a plurality of holes through which the decomposed particles pass after the silicon process gas is decomposed by the plasma; And a stage for fixing the substrate through which the particles passing through the baffle are bonded to each other to form crystalline particles.
  • the plasma gas may be an inert gas.
  • the silicon nano-powder manufacturing apparatus may further include a coalescence prevention gas inlet for introducing a coalescence prevention gas between the baffle and the stage.
  • the plasma antenna has a shape in which the synthetic container is wound in a ring shape
  • the silicon nanopowder manufacturing apparatus may further include an antenna moving part including a member for moving the plasma antenna up and down.
  • the plasma antenna may have a hollow tube shape to fill a coolant therein to be cooled, and both ends of the plasma antenna may be open upward to inject coolant.
  • the baffle may include a conductive material and may be grounded to the ground of a power source that supplies the plasma power.
  • the silicon nano-powder manufacturing method may further include an agglomeration preventing gas inflow step of introducing agglomeration preventing gas between the baffle and the stage.
  • the silicon nanopowder manufacturing method may further include moving the plasma antenna.
  • FIG. 1 is a view showing a silicon nano powder manufacturing apparatus according to an embodiment of the present invention.
  • FIG 2 is a diagram illustrating the plasma antenna 130 and the antenna moving unit 180.
  • FIG 3 is a diagram illustrating a case in which the refrigerant is filled in the plasma antenna 130.
  • FIG. 4 is a diagram illustrating the shape of the baffle 150.
  • FIG. 5 is a flowchart illustrating a method of manufacturing silicon nanopowder according to another embodiment of the present invention.
  • first, second, A, B, (a), and (b) may be used. These terms are only for distinguishing the components from other components, and the nature, order or order of the components are not limited by the terms. If a component is described as being “connected”, “coupled” or “connected” to another component, that component may be directly connected to or connected to that other component, but there may be another configuration between each component. It is to be understood that the elements may be “connected”, “coupled” or “connected”.
  • FIG. 1 is a view showing a silicon nano powder manufacturing apparatus according to an embodiment of the present invention.
  • the apparatus for manufacturing silicon nanopowder may include a synthetic container 110, a plasma gas inlet 120, a plasma antenna 130, a process gas inlet 140, and a baffle ( 150, a stage 160, agglomeration preventing gas inlet 170, an antenna moving unit 180, and a pump unit 190.
  • Synthetic container 110 is formed a space where the nano-powder is made inside.
  • the plasma gas inlet unit 120 introduces plasma gas into the synthesis vessel 110.
  • the plasma antenna 130 supplies power for making plasma gas introduced into the synthesis container 110 into plasma.
  • the process gas inlet 140 introduces the silicon process gas into the synthesis vessel 110.
  • the baffle 150 has a plurality of holes through which the decomposed particles pass after the silicon process gas is decomposed by the plasma.
  • the stage 160 has a substrate where particles passing through the baffle 150 are bonded to each other to form crystalline particles.
  • the aggregation preventing gas inlet 170 introduces the aggregation preventing gas between the baffle 150 and the stage 160.
  • the antenna moving unit 180 allows the plasma antenna 130 to move up and down.
  • the pump unit 190 adjusts the degree of vacuum inside the synthesis container 110.
  • Synthetic vessel 110 may be manufactured in the form of a tube so that a space in which the reaction is made to produce the nano-powder is formed.
  • the synthetic container 110 may be made of a material of quartz or ceramic, and may be made transparent so that the inside is visible.
  • the pump unit 190 may include two low vacuum pumps and a high vacuum pump to adjust the degree of vacuum of low or high vacuum according to working conditions. According to the embodiment, it may be configured only with a low vacuum pump.
  • the low vacuum pump may use a dry pump, and the high vacuum pump may use a turbo pump.
  • the plasma gas inlet unit 120 introduces a gas for plasma formation into the synthesis vessel 110.
  • An inert gas may be used as the gas for plasma, and argon (Ar), helium (He), krypton (Kr), xenon (Xe), or the like may be used.
  • Inflow of inert gas is about 100 sccm (Standard Cubic Centimeter per Minute) ⁇ 10,000sccm.
  • the plasma gas inlet 120 may be located on the upper surface of the synthesis vessel 110, but the present invention is not limited thereto.
  • the plasma antenna 130 supplies electric power to make the plasma gas introduced into the synthesis container 110 into plasma.
  • the plasma antenna 130 may have a shape in which the synthetic container 110 is wound in a ring shape as shown in FIG. 1.
  • an RF antenna is used as the plasma antenna 130 and plasma of an inert gas is generated by a force of a magnetic field or an electric field inside the synthesis vessel 110 induced by an applied RF power.
  • the internal pressure is controlled by the pump unit 190 and the pressure maintains 10mt ⁇ 10torr.
  • the supplied high frequency power can use 100W ⁇ 10KW.
  • FIG 2 is a diagram illustrating the plasma antenna 130 and the antenna moving unit 180.
  • the antenna moving unit 180 may be fixed to the synthesis container 110, and the plasma antenna 130 may be fixed by the antenna support unit.
  • the antenna support is coupled to the antenna moving part 180 to move up and down.
  • the antenna support part is provided with a tubular connection part while supporting the antenna to maintain the inserted shape with the antenna moving part 180, but the external force is increased by making enough friction force between the tubular connection part and the antenna moving part 180. Do not move unless it is applied.
  • a hole may be formed in the connecting portion and the plasma antenna 130 may be fixed by using a fastening chain in the portion.
  • the method of allowing the plasma antenna 130 to be coupled to the antenna moving unit 180 to move may be implemented in various ways.
  • FIG 3 is a diagram illustrating a case in which the refrigerant is filled in the plasma antenna 130.
  • the plasma antenna 130 may generate a lot of heat when applying RF power. There may be a problem in that a lot of power cannot be applied because heat is generated in the plasma antenna 130.
  • the plasma antenna 130 may have a hollow tube shape so that a refrigerant is filled therein to enable cooling.
  • both ends of the plasma antenna 130 may be open upward to inject the refrigerant, and any refrigerant may be used as a material used as a water-cooled refrigerant such as water.
  • a refrigerant pump (not shown) and a heat exchanger (not shown) are further provided to connect the refrigerant pump to one end of the plasma antenna 130, and then connect the refrigerant pump and the heat exchanger, and then heat exchange again. By connecting the other end of the plasma antenna 130 to circulate the refrigerant to circulate the refrigerant to maximize the cooling effect.
  • the process gas inlet unit 140 introduces the silicon process gas into the synthesis container 110.
  • Silane SiH 4
  • the flow rate of silane may be set to 1sccm ⁇ 1,000sccm.
  • the process gas inlet 140 and the plasma gas inlet 120 may be configured separately, but by forming an integrated gas inlet, the integrated gas inlet may be used for both inlet and plasma gas inlet.
  • the integrated case is illustrated.
  • FIG. 4 is a diagram illustrating the shape of the baffle 150.
  • the baffle 150 has a plurality of holes through which the decomposed particles pass after the silicon process gas is decomposed by the plasma. If the structure of the baffle 150 is absent, the area where the particles decomposed by the plasma descends increases, so that a thin film may be formed of particles decomposed by the plasma on the substrate (for example, a wafer) on the stage 160. Big. Therefore, a baffle 150 having a plurality of holes is used so that the thin film is not formed but is formed in powder form. The nanoparticles formed may reach the lower stage 160 through the baffle 150 having a hole having a uniform diameter of 3 mm to 10 mm.
  • the baffle 150 may include a conductive material and may be grounded with the ground of the power source for supplying plasma power.
  • grounding is performed by being connected to the ground acid of the RF power source, thereby preventing the plasma formed between the upper antenna regions from descending.
  • the intended process conditions may not be changed by initially fixing the position of the plasma antenna 130. Therefore, there is an effect of enabling high quality nano powder formation.
  • the silicon nanopowder manufacturing apparatus of the present invention may include an agglomeration preventing gas inlet 170 for introducing an agglomeration preventing gas between the baffle 150 and the stage 160.
  • an inert gas may be used, and the aggregation preventing gas may be introduced in a side direction in which particles decomposed by the plasma descend.
  • the agglomeration prevention gas serves to cool down the decomposition particles that are decomposed by the plasma. As such, by cooling the decomposition particles, the particles are prevented from sticking together before the crystals are formed to maintain the decomposition particles in a small state, thereby forming high quality nanopowders.
  • the stage 160 has a substrate where particles passing through the baffle 150 are bonded to each other to form crystalline particles.
  • the size of the nanoparticles formed in the substrate can be controlled by the ratio of the amount of the gas and the process gas flowing in.
  • the ratio of the amount of plasma gas and process gas may be set between 10: 1 and 10,000: 1.
  • the power can vary between 100W and 10,000W.
  • Si particles in which the process gas is decomposed by plasma may be bonded to each other to form crystalline particles having a lattice structure on the substrate.
  • the size of the crystalline particles formed may have a size of several nm to several hundred nm, which is called silicon nanoparticles (nano powder).
  • the in-situ clean can be performed using a gas containing NF 3 or other Flourine without exposing the synthetic vessel (reactor) to the outside.
  • the gas inflow is 10sccm ⁇ 1,000 sccm
  • the pressure is 10mt ⁇ 5torr
  • the power can be used 100W ⁇ 5,000W. It can also be mixed with an inert gas and used.
  • FIG. 5 is a flowchart illustrating a method of manufacturing silicon nanopowder according to another embodiment of the present invention.
  • Silicon nanopowder manufacturing method the step of introducing a plasma gas into the synthesis vessel (S502), the step of supplying power to make the plasma gas into a plasma using a plasma antenna (S504)
  • the silicon process gas is introduced into the synthesis vessel, in which the silicon process gas is decomposed by plasma (S508), and the decomposed particles pass through the holes of the baffle to form crystalline particles on the substrate ( S510) is made.
  • the anti-aggregation gas inflow step of introducing an anti-agglomeration gas between the baffle and the stage may be further included.
  • the method may further include a step of moving the plasma antenna before the gas for plasma is introduced.
  • Figure 7 is a photograph observing the formed nanoparticles with a transmission electron microscope.
  • the present invention is a useful invention for generating the nanopowder using plasma to generate the effect of supplying as high power as possible to facilitate the generation of plasma and the formation of high quality nanoparticles.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

La présente invention concerne un appareil et un procédé de fabrication de nanopoudre de silicium. La présente invention concerne un appareil et un procédé de fabrication de nanopoudre de silicium, caractérisés en ce que l'appareil comprend : un récipient de synthèse ayant un espace intérieur ; une partie d'alimentation de gaz plasma permettant au gaz plasma d'être amené dans le récipient de synthèse ; une antenne de plasma amenant l'énergie pour convertir le gaz plasma en plasma ; une partie d'alimentation de gaz plasma permettant au gaz de procédé de silicium d'être amené dans le récipient de synthèse ; un baffle ayant une pluralité d'ouvertures à travers lesquelles les particules, produites par la décomposition du gaz de procédé de silicium au moyen du plasma, passent ; et un étage dans lequel un substrat, sur lequel des particules cristallines sont formées en combinant les particules passant à travers le baffle, est fixé.
PCT/KR2011/003110 2010-04-30 2011-04-27 Appareil et procédé de fabrication de nanopoudre de silicium Ceased WO2011136570A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2010-0041089 2010-04-30
KR1020100041089A KR101240422B1 (ko) 2010-04-30 2010-04-30 실리콘 나노분말 제조장치 및 방법

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WO2011136570A2 true WO2011136570A2 (fr) 2011-11-03
WO2011136570A3 WO2011136570A3 (fr) 2012-04-12

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108910889A (zh) * 2018-07-16 2018-11-30 新疆泰宇达环保科技有限公司 提高金属硅加工效率的实现方法

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KR101320969B1 (ko) * 2012-02-08 2013-10-29 주식회사 정화나노엔지니어링 나노 입자 제조 장치
KR101436409B1 (ko) * 2013-01-11 2014-09-01 후성정공 주식회사 나노복합소재 제조용 복합 가스 제조장치
US9802826B2 (en) * 2013-11-25 2017-10-31 Korea Institute Of Energy Research Apparatus for producing silicon nanoparticle using inductive coupled plasma
KR102833123B1 (ko) * 2023-02-06 2025-07-11 한국표준과학연구원 플라즈마를 이용한 나노입자 합성, 집속 및 수집 장치 및 방법

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JP5309426B2 (ja) 2006-03-29 2013-10-09 株式会社Ｉｈｉ 微結晶シリコン膜形成方法及び太陽電池
US20090130337A1 (en) 2006-10-12 2009-05-21 Ovshinsky Stanford R Programmed high speed deposition of amorphous, nanocrystalline, microcrystalline, or polycrystalline materials having low intrinsic defect density
KR101468730B1 (ko) * 2007-08-31 2014-12-09 최대규 다중 무선 주파수 안테나를 갖는 유도 결합 플라즈마반응기
JP5321468B2 (ja) 2007-10-30 2013-10-23 日新電機株式会社 シリコンドット形成方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108910889A (zh) * 2018-07-16 2018-11-30 新疆泰宇达环保科技有限公司 提高金属硅加工效率的实现方法

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KR101240422B1 (ko) 2013-03-08
KR20110121484A (ko) 2011-11-07
WO2011136570A3 (fr) 2012-04-12

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