EP4472925A1 - Dispositif et procédé destinés à la production de carbure de silicium - Google Patents

Dispositif et procédé destinés à la production de carbure de silicium

Info

Publication number
EP4472925A1
EP4472925A1 EP23702455.9A EP23702455A EP4472925A1 EP 4472925 A1 EP4472925 A1 EP 4472925A1 EP 23702455 A EP23702455 A EP 23702455A EP 4472925 A1 EP4472925 A1 EP 4472925A1
Authority
EP
European Patent Office
Prior art keywords
silicon carbide
precursor
interior
heating
reactor
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.)
Pending
Application number
EP23702455.9A
Other languages
German (de)
English (en)
Inventor
Siegmund Greulich-Weber
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.)
Yellow Sic Holding GmbH
Original Assignee
Yellow Sic Holding GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yellow Sic Holding GmbH filed Critical Yellow Sic Holding GmbH
Publication of EP4472925A1 publication Critical patent/EP4472925A1/fr
Pending legal-status Critical Current

Links

Classifications

    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/12—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by gravity in a downward flow
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087—Heating or cooling the reactor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C01B32/963—Preparation from compounds containing silicon
    • C01B32/97—Preparation from SiO or SiO2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B1/00—Shaft or like vertical or substantially vertical furnaces
    • F27B1/005—Shaft or like vertical or substantially vertical furnaces wherein no smelting of the charge occurs, e.g. calcining or sintering furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B1/00—Shaft or like vertical or substantially vertical furnaces
    • F27B1/10—Details, accessories or equipment specially adapted for furnaces of these types
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B1/00—Shaft or like vertical or substantially vertical furnaces
    • F27B1/10—Details, accessories or equipment specially adapted for furnaces of these types
    • F27B1/20—Arrangements of devices for charging
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D3/00—Charging; Discharging; Manipulation of charge
    • F27D3/0033—Charging; Discharging; Manipulation of charge charging of particulate material
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/0053—Controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00769—Details of feeding or discharging
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00823—Mixing elements
    • B01J2208/00831—Stationary elements
    • B01J2208/0084—Stationary elements inside the bed, e.g. baffles
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00938—Flow distribution elements

Definitions

  • the invention relates to a device and a method for the production of silicon carbide, in particular for the production of silicon carbide powder.
  • Silicon carbide is an attractive material for many applications because of its high degree of hardness, its thermal conductivity and its special semiconductor properties. However, many of these properties are affected by contamination. High-purity silicon carbide is required above all for further processing in the semiconductor industry.
  • Silicon carbide is typically produced by carbothermal reactions in a reactor (furnace) at high temperatures from a precursor containing Si and C.
  • a precursor containing Si and C examples of the precursor are powders or granules made from SiO 2 and components containing carbon.
  • a well-known process for the production of silicon carbide is the Acheson process, in which the silicon carbide is obtained in batches from silicon dioxide in the form of quartz sand and from carbon in the form of coke in an electric resistance furnace at temperatures of more than 2000 °C.
  • EP 0476422 A1 discloses a method for producing silicon carbide from silicon dioxide powder and soot under argon in a crucible or rotary kiln at temperatures of 1200 to 2000° C. over a period of one hour. These methods are batch processes in which the SiC is produced in batches from a quantity of precursor previously loaded into the reactor. However, batch processes are unsatisfactory for the industrial production of SiC because the quantity in a batch is limited. Reloading the precursor is time-consuming and involves a loss of energy due to the cooling and reheating of the reactor, making it difficult to precisely control the process parameters over the entire production time.
  • the silicon carbide produced in a known manner is not pure enough for many applications, for example in the manufacture of electronics or semiconductors, and must be cleaned at great expense before further processing.
  • the object of the invention is therefore to create a device and a method for the production of silicon carbide that are more efficient than the prior art.
  • the invention allows a continuous production of silicon carbide in a reactor in which the precursor is transformed into silicon carbide while falling through the reactor.
  • the precursor and silicon carbide hardly come into contact with the reactor wall. Therefore there is practically no contamination of the produced silicon carbide in the reactor.
  • the relatively short residence time when falling through the reactor also limits the Ingestion of foreign matter by the precursor and the produced silicon carbide.
  • the invention is ideally suited for the efficient production of high-purity silicon carbide.
  • Nanoscale or microscale refers here to the size of the primary particles in the precursor, i.e. a particle size in the range from 5 to 1000 nm, typically around 20 to 200 or up to 1000 nm or a particle size in the range from 1 to 1000 ⁇ m, typically around 1 or 20 to 200 p.m.
  • the properties of the invention cannot be achieved with horizontal rotary kilns as in the prior art.
  • the purity required for high quality silicon carbide would require a high purity silicon carbide kiln to avoid incorporation of other materials into the product, which would be technically difficult and expensive.
  • the furnace chamber should be filled with inert gas and sealed off from the outside atmosphere.
  • the throughput times of the precursor through conventional rotary kilns for silicon carbide production are too long. None of these problems arise with the invention. From preferred embodiments of the invention are in
  • FIG. 1 shows a device for the production of silicon carbide according to the exemplary embodiments.
  • top and bottom refer to the orientation of the device when used as intended using the method for the production of silicon carbide.
  • the device for the production of silicon carbide shown in FIG. 1 comprises a furnace as a reactor 1 that can be heated.
  • the reactor 1 comprises a jacket 2 which surrounds an interior space 3 and has a feed opening 4 at the upper end of the interior space 3 on the upper side of the reactor 1 and an outlet opening 5 at the lower end of the interior space 3 on the underside of the reactor 1 .
  • the shell 2 is designed essentially as a vertical tube. Feed opening 4 and outlet opening 5 lie essentially one above the other in the vertical direction.
  • the interior 3 is preferably filled with an inert gas, for example argon.
  • a feed device 6 for feeding a precursor 7 through the feed opening 4 into the interior space 3 is arranged above the feed opening 4 .
  • the precursor trickles through the feed opening 4 into the interior space 3 due to gravity.
  • the feed opening 4 is provided with a divider 8 for dividing the stream of the supplied precursor 7 into several parallel streams and thus for distributing it over a large part of the cross-sectional area of the interior 3 without directing the precursor 7 against the jacket 2 unnecessarily .
  • the precursor 7 contains Si and C and is typically provided as a powder or granulate, for example as an SiCp powder with carbon-containing components such as graphite or soot.
  • a nanoscale or microscale precursor is suitable, i.e.
  • the precursor should have a purity corresponding to the required purity of the silicon carbide to be produced.
  • the collecting device 9 can be a container or a removal device for the silicon carbide 10 designed as a ramp or conveyor belt.
  • the reactor 1 Since the reactor 1 is static, it can be sealed in a simple manner so that the outside atmosphere does not penetrate into the inert gas-filled interior 3, for example by sealing between the feed opening 4 and the feed device 6 and between the outlet opening 5 and the collecting device 9 or by a shell around the reactor 1 (not shown).
  • the reactor 1 is heated and the jacket 2 has one or more heating devices 11 , 12 for this purpose.
  • An upper first heating device 11 for heating an upper first heating zone 13 of the interior 3 to a first temperature and a lower second heating device are preferably device 12 provided for heating a lower second heating zone 14 of the interior 3 to a second temperature.
  • the first temperature ranges from about 1600 to 1900°C, preferably about 1800°C
  • the second temperature is lower than the first and preferably ranges from about 1500 to 1700°C.
  • the precursor falling through the interior from the feed opening 4 is first exposed to the first temperature in the first heating zone 13, whereby the carbothermal reactions are set in motion and intermediate products are formed, which react at the second temperature in the second heating zone 14 to form silicon carbide 10 , which emerges from the outlet opening 5.
  • the particles of the precursor 7 are thus transformed into nano- or microcrystalline particles of silicon carbide 10.
  • the silicon carbide 10 is taken as a powder by the collecting device 9 .
  • the transport of the particles of the precursor 7 and the silicon carbide 10 from the feed opening 4 through the interior space 3 to the outlet opening 5 occurs essentially in free fall under gravity.
  • the particle size of the precursor and the lengths of the first zone 13 and the second zone 14 in the vertical direction are selected in such a way that the rate of descent of the particles for a residence time, i.e. heating time of about 100 to 200 ms, preferably about 150 ms, in the first heating zone 13 and a total dwell time of about 300 to 1000 ms, preferably about 400 ms, in both heating zones 13, 14 or the entire interior space 3.
  • Baffle plates 15 can optionally be present, which, as in the example shown, starting from the jacket 2 downwards protrude obliquely into the first and/or the second heating zone 13, 14 of the interior 3 and interrupt the fall of the particles of the precursor 7 and/or the silicon carbide 10 and thus the residence time of the particles in the zones 13, 14 compared to a continuous one extend free fall.
  • the angle of inclination of the baffle plates 15 can be adjustable in order to set the dwell time.
  • the dwell time can also be adjusted in that the inert gas in the inner space 3 is allowed to flow upwards to lengthen the dwell time and downwards to shorten the dwell time, for example by circulating the inert gas in a closed circuit which runs through the inner space 3 and a feed and the outlet opening 4 , 5 leads to a return line (not shown) that connects them to one another outside of the reactor 1 .
  • the precursor 7 and the silicon carbide 10 are transported in free fall, largely without contact with the jacket 2 and therefore largely without contact, apart from contact with impact plates 15 that may be provided. Therefore, the precursor 7 and silicon carbide 10 do not absorb any impurities, and the produced silicon carbide 10 can be highly pure, corresponding to the purity of the precursor used.
  • Casing 2 and any baffle plates 15 provided are preferably made of silicon carbide or coated with silicon carbide towards the interior 3 in order not to introduce any foreign matter into the silicon carbide 10 produced.
  • the device is very robust since it has hardly any moving parts.
  • the device allows an efficient, continuous production process for the silicon carbide 10.
  • the feed device 6 continuously feeds precursor 7 through the feed opening 4, which, as described, passes through the heated interior 3, i.e. in particular the first and second heating zones 13 , 14 falls and is thereby transformed into silicon carbide 10, which falls out through the outlet opening 5 and is also continuously collected by the collecting device 9.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne un dispositif servant à la production de carbure de silicium, comprenant un réacteur chauffant (1) qui est pourvu, au niveau de son côté supérieur, d'un orifice d'alimentation (4) destiné à l'alimentation continue en précurseur (7), au niveau de son côté inférieur, d'un orifice de sortie (5) destiné à la sortie continue du carbure de silicium (10) formé dans le réacteur (1) à partir du précurseur et, entre l'orifice d'alimentation (4) et l'orifice de sortie (5), d'un espace intérieur (1) disposé de telle sorte que le précurseur, notamment le carbure de silicium, peut traverser ledit espace intérieur (1) en tombant depuis l'orifice d'alimentation (4) jusqu'à l'orifice de sortie (5).
EP23702455.9A 2022-02-01 2023-01-27 Dispositif et procédé destinés à la production de carbure de silicium Pending EP4472925A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102022102320.6A DE102022102320A1 (de) 2022-02-01 2022-02-01 Vorrichtung und Verfahren zur Produktion von Siliziumkarbid
PCT/EP2023/052089 WO2023148108A1 (fr) 2022-02-01 2023-01-27 Dispositif et procédé destinés à la production de carbure de silicium

Publications (1)

Publication Number Publication Date
EP4472925A1 true EP4472925A1 (fr) 2024-12-11

Family

ID=85132906

Family Applications (1)

Application Number Title Priority Date Filing Date
EP23702455.9A Pending EP4472925A1 (fr) 2022-02-01 2023-01-27 Dispositif et procédé destinés à la production de carbure de silicium

Country Status (8)

Country Link
US (1) US20250135425A1 (fr)
EP (1) EP4472925A1 (fr)
JP (1) JP2025503261A (fr)
KR (1) KR20240140955A (fr)
AU (1) AU2023214706A1 (fr)
DE (1) DE102022102320A1 (fr)
IL (1) IL314480A (fr)
WO (1) WO2023148108A1 (fr)

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2744636A1 (de) * 1977-10-04 1979-05-17 Wolfgang Dipl Ing Boecker Verfahren und vorrichtung zur herstellung von hochreinem siliciumcarbidpulver und seine verwendung
JPS55113609A (en) 1979-02-21 1980-09-02 Ibiden Co Ltd Manufacturing apparatus for beta crystallbase silicon carbide
US4529575A (en) * 1982-08-27 1985-07-16 Ibiden Kabushiki Kaisha Process for producing ultrafine silicon carbide powder
EP0476422B1 (fr) 1990-09-07 1994-07-27 H.C. Starck GmbH & Co. KG Procédé de fabrication de carbure de silicium beta pulverulent
JPH06505955A (ja) * 1991-03-22 1994-07-07 ザ・ダウ・ケミカル・カンパニー 非酸化物セラミック粉末の移動床炭熱合成方法
JPH05208900A (ja) 1992-01-28 1993-08-20 Nisshin Steel Co Ltd 炭化ケイ素単結晶の成長装置
US5437708A (en) * 1994-05-04 1995-08-01 Midrex International B.V. Rotterdam, Zurich Branch Iron carbide production in shaft furnace
DE102007034912A1 (de) 2006-08-03 2008-02-07 General Electric Co. Verfahren zur Erzeugung solartauglichen Siliziums

Also Published As

Publication number Publication date
WO2023148108A1 (fr) 2023-08-10
KR20240140955A (ko) 2024-09-24
JP2025503261A (ja) 2025-01-30
DE102022102320A1 (de) 2023-08-03
US20250135425A1 (en) 2025-05-01
AU2023214706A1 (en) 2024-08-22
IL314480A (en) 2024-09-01

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