EP3043929A1 - Classification de polysilicium - Google Patents

Classification de polysilicium

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Publication number
EP3043929A1
EP3043929A1 EP14752593.5A EP14752593A EP3043929A1 EP 3043929 A1 EP3043929 A1 EP 3043929A1 EP 14752593 A EP14752593 A EP 14752593A EP 3043929 A1 EP3043929 A1 EP 3043929A1
Authority
EP
European Patent Office
Prior art keywords
silicon
less
screen
size
fraction
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.)
Granted
Application number
EP14752593.5A
Other languages
German (de)
English (en)
Other versions
EP3043929B1 (fr
Inventor
Andreas Schneider
Peter Gruebl
Rainer Hauswirth
Reiner Pech
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.)
Wacker Chemie AG
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Wacker Chemie AG
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Filing date
Publication date
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Publication of EP3043929A1 publication Critical patent/EP3043929A1/fr
Application granted granted Critical
Publication of EP3043929B1 publication Critical patent/EP3043929B1/fr
Active legal-status Critical Current
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
    • B07B1/28—Moving screens not otherwise provided for, e.g. swinging, reciprocating, rocking, tilting or wobbling screens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
    • B07B1/46—Constructional details of screens in general; Cleaning or heating of screens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B1/00—Sieving, screening, sifting, or sorting solid materials using networks, gratings, grids, or the like
    • B07B1/46—Constructional details of screens in general; Cleaning or heating of screens
    • B07B1/4609—Constructional details of screens in general; Cleaning or heating of screens constructional details of screening surfaces or meshes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
    • B07B13/14—Details or accessories
    • B07B13/18—Control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B2201/00—Details applicable to machines for screening using sieves or gratings
    • B07B2201/04—Multiple deck screening devices comprising one or more superimposed screens

Definitions

  • the invention relates to a method for classifying polysilicon.
  • Polycrystalline silicon (polysilicon in short) serves as a starting material for the production of monocrystalline silicon for semiconductors according to the Czochralski (CZ) or zone melt (FZ) process, and for the production of monocrystalline or multicrystalline silicon after various drawing and casting processes.
  • CZ Czochralski
  • FZ zone melt
  • Polycrystalline silicon is usually produced by means of the Siemens process.
  • carrier bodies usually thin filament rods made of silicon
  • a reaction gas comprising hydrogen and one or more silicon-containing components is introduced 3 , TCS) or a mixture of trichlorosilane with dichlorosilane (SiH 2 Cl 2 , DCS) and / or with tetrachlorosilane (SiCl 4 , STC), but silane (SiH 4 ) is used more rarely but also on an industrial scale
  • Filament rods are placed vertically in electrodes located at the bottom of the reactor, where they are connected to the power supply.
  • the heated filament rods and the horizontal bridge deposit high-purity polysilicon, which increases in diameter over time.
  • the reactor bell is opened the bars are made by hand or with the help of special Vo taken from so-called development aids for further processing or for temporary storage.
  • polycrystalline silicon rods are
  • Polycrystalline silicon granules or polysilicon granules for short is an alternative to the polysilicon produced in the Siemens process. While the polysilicon produced in the Siemens process as a cylindrical silicon rod, the time-consuming and costly crushed into fragments prior to further processing and may need to be cleaned again, polysilicon granules has bulk material properties and can directly as raw material for example for single crystal production for the photovoltaic and electronics industry be used.
  • Polysilicon granules are produced in a fluidized bed reactor. This is done by fluidization of silicon particles by means of a gas flow in a fluidized bed, which is heated by a heater to high temperatures. By addition of a silicon-containing reaction gas a pyrolysis reaction takes place on the hot particle surface.
  • silicon-containing starting gas used may be silicon-halogen compounds (eg chlorosilanes or bromosilanes), monosilane (SiH 4 ), as well as mixtures of these gases with hydrogen.
  • the polycrystalline silicon granules are divided after its preparation by means of a sieve plant into two or more fractions.
  • the smallest sieve fraction (Siebunterkorn) can then be processed in a grinding plant to seed particles and added to the reactor.
  • US 2009081108 A1 discloses a workbench for manual sorting of polycrystalline silicon according to size and quality.
  • An ionization system is implemented to neutralize electrostatic charges by active air ionization. Ionizers penetrate the clean room air with ions in such a way that static charges on insulators and ungrounded conductors are dissipated.
  • a screening machine is generally a machine for sifting, ie the separation (separation) of solid mixtures according to grain sizes.
  • planing vibrating screens According to the movement characteristics, a distinction is made between planing vibrating screens and throwing machines.
  • the drive of the screening machines is usually electromagnetic or by unbalance motors or gearbox.
  • the movement of the Siebbelags serves the further transport of the feedstock in Siebleksscardi and the passage of the fine fraction through the mesh openings.
  • the sieve tower completes a horizontal circular movement in one plane.
  • the particles on the screen fabric largely retain their orientation.
  • Planeting machines are preferably used for needle-shaped, platelet-shaped, elongated or fibrous screening goods in which throwing up the sample good is not necessarily advantageous.
  • a special type is the Mehrdecksiebmaschine, which can fractionate several grain sizes simultaneously. They are designed for a multitude of sharp separations in the middle of the finest grain range.
  • the drive principle is based on two-deck planer on two counter-rotating unbalance motors that produce a linear vibration.
  • the screen material moves in a straight line over the horizontal separating surface.
  • the machine works with low vibration acceleration.
  • US 8021483 B2 discloses an apparatus for sorting polycrystalline silicon pieces comprising a vibratory motor assembly and a step bottom classifier attached to the vibratory motor assembly.
  • the vibratory motor assembly causes the pieces of silicon to move over a first bottom containing grooves.
  • dust is removed by a stream of air through a perforated plate.
  • the pieces of silicon settle in holes of grooves or remain on ridges of the grooves.
  • pieces of silicon smaller than a gap fall through it onto a conveyor belt. Larger pieces of silicon move across the gap and fall to the second floor.
  • the parts of the device that come in contact with the polycrystalline silicon pieces are made of materials that minimize contamination of silicon. Examples are tungsten carbide, PE, PP, PFA, PU, PVDF, PTFE, silicon and ceramics.
  • US 2007235574 A1 discloses a device for crushing and sorting polycrystalline silicon, comprising a polysilicon rough-cut feeder in a crusher, the crusher, and a polysilicon-collapse classifier, the device being provided with a controller comprising a allows variable adjustment of at least one crushing parameter in the crusher and / or at least one sorting parameter in the sorting system.
  • the sorting plant consists of a multi-stage mechanical screening plant and a multi-stage optoelectronic separation plant.
  • Preference Schwingsiebmaschinen that are driven by an unbalance motor used. As Siebbelag mesh and perforated sieves are preferred.
  • the screening levels can be successively or in another structure, such.
  • B. a tree structure be arranged.
  • the sieves are arranged in three stages in a tree structure.
  • the freed from fines polysilicon fraction is preferably sorted by means of optoelectronic separation plant. Sorting of polysilicon fracture can be done according to all criteria that are state of the art in image processing. It is preferably carried out according to one to three of the criteria selected from the group length, area, shape, morphology, color and weight of polysilicon fragments, particularly preferably length and area.
  • Fraction 0 fraction sizes with a distribution of about 0 to 3 mm
  • Fraction 1 fraction sizes with a distribution of about 1 mm to 10 mm
  • Fraction 2 fraction sizes with a distribution of about 10 mm to 40 mm
  • Fraction 3 fraction sizes with a distribution of about 25 mm to 65 mm
  • Fraction 4 fraction sizes with a distribution of about 50 mm to 1 10 mm
  • Fraction 5 fraction sizes with a distribution of approx.> 90 mm to 250 mm
  • US 5165548 A discloses an apparatus for size separation of silicon pieces suitable for semiconductor applications, comprising a cylindrical screen connected to a device for rotating the cylindrical screen, the surfaces of the screen contacting the silicon pieces in the screen
  • each first elongate member is greater than the mesh size of the first screen forming screen and the same length of the second particle or smaller than the mesh size.
  • EP 1454679 B1 describes a screening device with a first oscillating body, which is provided with first cross members, and a second oscillating body, which is provided with second cross members, which first and second cross members are arranged alternately and have clamping devices, so that elastic 5 Siebbeläge between each one the first and ever a second cross member are clamped, and a drive unit which is coupled directly to the first oscillating body and over which the first oscillating body is constrained, so that the clamped elastic Siebbeläge between a stretched and a compressed layer are moved back and forth, wherein the second oscillating body is forcibly guided relative to the first oscillating body.
  • a method for promoting silicon breakage in which the silicon fragments are guided over a conveying surface made of hyperpure silicon of a vibrating conveyor.
  • sharp-edged silicon pieces are rounded when they are conveyed on the vibrating conveyor surface of a vibrating conveyor.
  • the specific surfaces of the silicon fragments are reduced, superficial adhering contaminations are abraded.
  • the rounded by a first vibratory conveyor unit silicon break can via a second vibratory conveyor unit are performed.
  • Their conveying surface consists of parallel arranged hyperpure silicon plates, which are fixed by lateral fastening devices.
  • the hyperpure silicon plates have through openings, for example in the form of openings.
  • the conveyor edges which serve as a lateral boundary of the conveyor surfaces, are likewise made of hyperpure silicon plates and are fixed, for example, by hold-downs.
  • the conveyor surfaces made of hyperpure silicon slabs are supported by steel plates and optionally damping mats.
  • US 2012052297 A1 discloses a process for the production of polycrystalline silicon, comprising breaking into thin pieces of polycrystalline silicon deposited on thin rods in a Siemens reactor, classifying the fragments in size classes from about 0.5 mm to greater than 45 mm, treating the silicon fragments using compressed air or dry ice to remove silicon dust from the debris without chemical wet cleaning.
  • the polycrystalline silicon is classified as follows: Breakage size 0 (BG0) in mm: approx. 0.5 to 5; Break size 1 (BG1) in mm: approx. 3 to 15; Fracture size 2 (BG2) in mm: approx. 10 to 40; Crack size 3 (BG3) in mm: approx.
  • US 2009120848 A1 describes a device which enables a flexible classification of broken polycrystalline silicon, characterized in that it comprises a mechanical screening plant and an optoelectronic sorting plant, wherein the poly-fraction through the mechanical screening plant into a silicon fines and a silicon remainder is separated and the silicon residue is separated via an optoelectronic sorting in further fractions.
  • the mechanical screen is preferably a vibrating screen, which is driven by an unbalance motor.
  • the overlap between a fraction 1 and a fraction 0 is also max. 2mm. Especially in the fraction with smaller fragment sizes of 30 mm or less, such an overlap is undesirable.
  • the object of the invention is achieved by a method for mechanically classifying polycrystalline silicon fracture or granules with a vibrating screen, wherein silicon fracture or granules are on one or more screens each comprising a screen lining, which are vibrated such that the silicon break or the silicon granules make a movement, whereby the silicon fraction or the silicon granules are separated into different size classes, characterized in that a Siebkennziffer greater than or equal to 0.6 and less than or equal to 9.0.
  • the sieve index is defined as the ratio of the acceleration generated by the sieve movement to the gravitational acceleration vertical to the sieve plane:
  • ⁇ angular velocity
  • the sieving index For a throwing motion, the sieving index must be> 1.
  • the screen index is greater than or equal to 0.6 and less than or equal to 5.0.
  • a sieve index of 0.6 to 5.0 By classifying with a sieve index of 0.6 to 5.0, a further improvement of the sieve results could be achieved.
  • the selectivity is better than with a Siebkennziffer of greater than 5.0.
  • the movement of silicon fracture or granulate is particularly preferably a throwing movement, the sieving index being 1, 6 to 3.0. It has been shown that this results in even improved sieving results, in particular an even higher selectivity between the different size classes.
  • the oscillation amplitude is preferably 0.5 to 8 mm, particularly preferably 1 to 4 mm.
  • the rotational speed ⁇ / 2 ⁇ is preferably 400 to 2000 rpm, more preferably 600 to 1500 rpm.
  • the throwing angle is preferably 30 to 60 °, particularly preferably 40 to 50 °.
  • the screen tilt angle with respect to the horizontal is preferably 0 to 15 °, particularly preferably 0 to 10 °.
  • the screening machine preferably comprises a feed area in which the screenings are fed and a discharge area in which classified screenings are removed.
  • the size of the sieve openings increases in the direction of discharge. Fractions / break sizes are preferably separated by successively arranged discharges.
  • the screening machine comprises mutually arranged screen decks.
  • This oil has the advantage that large fragments can not damage fine-meshed screen coverings.
  • fractions / break sizes are separated by discharges arranged one below the other.
  • the screening machine comprises a frame-sieve system. This allows a quick screen change. Also, the monitoring of any contamination is facilitated.
  • Such a frame-sieve system provides that screen coverings are screwed to the frame, glued, plugged or potted, that the frames made of wear-resistant 0 plastic (preferably PP, PE, PU), possibly with steel reinforcement, or at least with wear-resistant plastic are lined.
  • the frames are sealed by vertical clamping. This can avoid contamination and material loss.
  • screen linings made of particularly wear-resistant plastics, namely elastomers having a hardness greater than 65 Shore A, more preferably having a hardness greater than 80 Shore A.
  • the Shore hardness is specified in the DIN 53505 and DIN 7868 standards , In this case, one or more screen coverings or their surfaces may consist of such an elastomer.
  • Both one or more screen coverings or their surfaces as well as all product-contacting components and linings are preferably made of plastics with a total contamination (metals, dopants) of less than 2000 ppmw, preferably less than 500 ppmw and particularly preferably less than 100 ppmw.5
  • the maximum contamination of the plastics with the elements Al, Ca, P, Ti, Sn and Zn should be less than 100 ppmw, more preferably less than 20 ppmw.
  • the maximum contamination of the plastics with the elements Cr, Fe, Mg, As, Co, Cu, Mo, Sb and W should be less than 10 ppmw, more preferably less than 0.2 ppmw.
  • the screen coverings of plastics preferably comprise a reinforcement or filling of metals, glass fiber, carbon fiber, ceramic or composite materials for stiffening.
  • the screenings are dedusted.
  • the mechanical sieving mobilizes most of the fine dust adhering to the bulk material on the individual screen decks. This effect is used in the invention to dedust the bulk material during the screening process.
  • the gas flow can be generated either by a suction or by a gas purging.
  • Suitable visual gases are purified air, nitrogen or other inert gases.
  • a gas velocity of 0.05 to 0.5 m / s, more preferably 0.2 to 0.3 m / s should be present.
  • a gas velocity of 0.2 m / s can be set, for example, with a gas throughput or a suction capacity of about 720 NrrrVh per m 2 screen area. As fine dust particles are understood that are smaller than 10 pm.
  • dedusting by means of countercurrent air classification in the discharge lines of the individual sieve fractions is optionally carried out.
  • the classifying gas is fed into the lower area of the flue ducts and the dust-laden exhaust gas is discharged in the upper area immediately in front of the screening machine.
  • the above media come into question.
  • the advantage of this dedusting method is that the visual flow can be adapted to the particle size of the sieve fraction. With a coarse sieve fraction, for example, a high visual flow can be set without fine product being carried along. This gives a very good dedusting and the desired low particulate matter in the product.
  • the speed is temporarily increased up to 4000 rev / min, to free the screen coverings of Steckkorn.
  • the speed is temporarily increased up to 4000 rev / min, to free the screen coverings of Steckkorn.
  • the oscillation amplitude decreases towards the discharge.
  • the ratio of the vibration amplitude at the discharge is up to 50% less than at the inlet. It has been shown that both wear and product contamination can be further reduced.
  • a drive for the screening machine come linear, circular or elliptical oscillator in question.
  • the drive preferably provides a vertical acceleration component to reduce screen wear and to avoid pinch.
  • the screening tray and the Siebauslässe inside are completely lined with silicon or with a thermoplastic or elastomeric plastic.
  • Steel body of the screening machine are preferably provided with welded PP lining segments.
  • As side linings, steel-reinforced PU castings have proven to be particularly suitable.
  • silicon hole strips are used as the screen covering.
  • One or more screen coverings can be designed in this way. These are preferably perforated square rods made of hyperpure silicon. These preferably have at least in part a conical hole shape, i. the cross-sectional area is smaller at the top than at the bottom. This contributes to avoiding pinch.
  • the cone preferably has an angle of 1 to 20 °, particularly preferably 1 to 5 °.
  • an edge rounding of the holes with a radius of 0.1 to 2 mm is provided on the upper Sieboberseite to avoid breakouts and wear, which would lead to a deterioration of the selectivity.
  • only the lower part of the hole is conical and the upper part is cylindrical, so that the hole is not expanded too quickly due to wear.
  • plastic-coated metal support strips are provided for stabilizing the breakage of the Si strips, to avoid contamination and to secure against loosening of fragments in inguinal hernia.
  • individual Si strips are provided with hard metal end strips, which are braced horizontally or vertically.
  • the hard metal used is preferably WC, SiC, SiN or TiN.
  • the Si perforated screen is placed on a base, glued or screwed. This allows higher strength, larger areas and the use of thinner or thicker screens possible. Breakage is easier to avoid.
  • Si perforated sieves and sieves made of plastic or sieves with a plastic covering It is particularly preferred to use both Si perforated sieves and sieves made of plastic or sieves with a plastic covering.
  • An Si-hole sieve with a hole diameter of 5 mm to 50 mm is preferably used as the first sieve cut.
  • the large fragments can clean the sprue grains and thus prevent clogging.
  • one or more screens made of plastic or plastic coverings are used.
  • an additional pre-screen with a plastic coating and with a mesh ratio to the underlying screen deck of 1.5: 1 to 10: 1 is used.
  • the Vorsiebdeck preferably has a lower wire tension. This serves to minimize wear.
  • the process according to the invention leads to polycrystalline silicon fragments with a sharp particle size distribution without large overlap or with a high selectivity classified polycrystalline silicon granules, which was previously not feasible in the prior art.
  • the invention therefore also relates to Classified polycrystalline silicon fragments, characterized by a particle size classification in fractional size classes 2, 1, 0 and F, wherein it applies to the fragments that at fraction size 2 max. 5 wt .-% less than 1 1 mm and max. 5% by weight greater than 27 mm; at fraction size 1 max. 5% by weight smaller than 3.7 mm and max. 5% by weight greater than 14 mm; at fraction size 0 max. 5% by weight less than 0.6 mm and max. 5 wt% greater than 4.6 mm; at fraction size F max. 5 wt .-% less than 0.1 mm and max. 5 wt .-% are greater than 0.8 mm.
  • BG 2 in mm 1 1 to 27.
  • Breakage size 2 to breakage size 1 max. 3 mm;
  • Break size 1 to breakage size 0 max. 0.9 mm;
  • Fraction size 0 to fraction size F max. 0.2 mm.
  • the polycrystalline silicon fragments having the improved grain size classification preferably have a very low surface contamination: Tungsten (W):
  • Fraction size 0 ⁇ 1000000 pptw, more preferably ⁇ 200000 pptw;
  • Fraction size 2 ⁇ 5000 pptw, more preferably ⁇ 500 pptw;
  • Fracture size 1 ⁇ 50,000 pptw, more preferably ⁇ 5,000 pptw;
  • Fraction size 0 ⁇ 500,000 pptw, more preferably ⁇ 50,000 pptw;
  • Fraction size F ⁇ 5000000 pptw, more preferably ⁇ 500000 pptw;
  • Fraction size 1 ⁇ 500,000 pptw, more preferably e 10000 pptw;
  • Fraction size 0 ⁇ 5000000 pptw, more preferably ⁇ 100000 pptw;
  • Fraction size F ⁇ 50,000,000 pptw, more preferably ⁇ 1,000,000 pptw;
  • Fraction size 2 ⁇ 1 ppmw, more preferably ⁇ 0.2 ppmw; Fraction size 1 ⁇ 10 ppmw, more preferably ⁇ 2 ppmw;
  • Fraction size 0 ⁇ 100 ppmw, more preferably ⁇ 20 ppmw;
  • Fraction size F ⁇ 1000 ppmw, more preferably ⁇ 200 ppmw; Cr, Ni, Na, Zn, Al, Cu, Mg, Ti, K, Ag, Ca, Mo per single element:
  • Fraction size F ⁇ 100000 pptw, more preferably e 10000 pptw;
  • Particulate matter (silicon particles less than 10 pm in size):
  • Fraction size 0 ⁇ 25 ppmw, more preferably ⁇ 10 ppmw;
  • Fraction size F ⁇ 50 ppmw, more preferably ⁇ 20 ppmw.
  • the invention also relates to classified polycrystalline silicon granules, classified at least in the two size classes Siebzielkorn and Siebunterkorn, wherein a selectivity between Siebzielkorn and Siebunterkorn is more than 0.86.
  • Classified polycrystalline silicon granules preferably have the following impurities with metals on the surface: Fe: ⁇ 800 pptw, more preferably ⁇ 400 pptw; Cr: ⁇ 100 pptw, more preferably ⁇ 60 pptw; Ni: ⁇ 100 pptw, more preferably ⁇ 50 pptw; Na: ⁇ 100 pptw, more preferably ⁇ 50 pptw; Cu: ⁇ 20 pptw, more preferably ⁇ 10 pptw; Zn: ⁇ 2000 pptw, more preferably ⁇ 1000 pptw.
  • Classified polycrystalline silicon granules preferably have a surface carbon contamination of less than 10 ppmw, more preferably less than 5 ppmw.
  • Classified polycrystalline silicon granules preferably have a surface particulate contamination of less than 10 ppmw, most preferably niger than 5 ppmw, on. Fine dust is defined as silicon particles with a size of less than 10 [im.
  • Example 1 and Comparative Example 2 relate to the classification of polycrystalline silicon fragments in fractions of 2, 1, 0 and F.
  • Example 3 and Comparative Example 4 relate to classifying polycrystalline silicon granules (sieve grain size 0.75 - 4 mm).
  • example 1
  • Table 1 a shows the essential parameters of the screening machine.
  • Table 1 b shows which sieve set was used in the example. Three sieve decks with different sieve mesh sizes were used. Table 1 b
  • Table 1 c shows the composition of the screen coverings.
  • Table 1f shows the contaminants of the classified fragments with surface metals, carbon, dopants and particulate matter.
  • Table 2a shows the essential parameters of the screening machine used for this purpose.
  • Table 2b shows which sieve set was used in Comparative Example 2. Three sieve decks with different sieve mesh sizes were used.
  • Table 2c shows the composition of the screen coverings used.
  • the impurities are consistently higher than in Example 1. This shows the influence of the composition of the screen coverings on the surface contamination of the fragments after classification.
  • Table 3a shows the essential parameters of the screening machine.
  • Table 3b shows which sieve set was used in Example 3. Three sieve decks with different sieve mesh sizes were used. Table 3b
  • Table 3c shows the composition of the screen coverings.
  • Table 3f shows the contaminants of the sized granules with surface metals, carbon, dopants and particulate matter.
  • Table 4a shows the essential parameters of the screening machine.
  • Table 4b shows which sieve set was used in Comparative Example 4. Three sieve decks with different sieve mesh sizes were used.
  • Table 4b Table 4c shows the composition of the screen coverings used.
  • Table 4e The selectivity of Siebzielkorn / Siebunterkorn is worse than in Example 3. This is due to the comparison with Example 3 lower Siebkennziffer.
  • Table 4f shows the contaminants of the sized granules with surface metals, carbon, dopants and particulate matter.
  • the impurities are consistently higher than in example 3.
  • the following measuring methods were used to determine the specified parameters.
  • the determination of carbon contamination is carried out by means of an automatic analyzer. This is described in detail in the not yet published US application with the application number 13 / 772,756 and in the German application with the file number 102012202640.1.
  • the determination of the dopant concentrations (boron, phosphorus, As) is carried out according to ASTM F1389-00 on monocrystalline samples.
  • the determination of the metal impurities is carried out according to ASTM 1724-01 with ICP-MS.
  • the fine dust measurement is carried out as described in DE 10 2010 039 754 AI.
  • the particle sizes are determined by means of dynamic image analysis according to ISO 13322-2 (measuring range: 30 m - 30 mm, type of analysis: dry measurement of powders and granules).

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  • Silicon Compounds (AREA)
  • Combined Means For Separation Of Solids (AREA)

Abstract

L'invention concerne un procédé permettant la classification mécanique d'un fragment ou d'un granulé polycristallin au moyen d'un tamiseur vibrant. Le fragment ou le granulé de silicium se situe sur un ou plusieurs tamis comprenant chacun une garniture de tamis, lesquelles sont amenées à vibrer de telle manière que le fragment de silicium ou le granulé de silicium exécute un mouvement, le fragment de silicium ou le granulé de silicium étant séparé en différentes catégories de taille. Un coefficient de tamisage, lequel est défini comme le rapport entre l'accélération produite par le mouvement de tamisage et l'accélération gravitationnelle perpendiculairement au plan de tamisage, et lequel est caractérisé par la formule Kv = r * ω2 * sin(α+ β)/(g*cos(ß)), où : r : amplitude des vibrations ; ω : vitesse angulaire ; α : angle de projection ; β : angle d'inclinaison du tamis ; g : constante gravitationnelle, est supérieur ou égal à 0,6 et inférieur ou égal à 9,0.
EP14752593.5A 2013-09-09 2014-08-07 Classification de silicium polycristallin Active EP3043929B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102013218003.9A DE102013218003A1 (de) 2013-09-09 2013-09-09 Klassieren von Polysilicium
PCT/EP2014/067032 WO2015032584A1 (fr) 2013-09-09 2014-08-07 Classification de polysilicium

Publications (2)

Publication Number Publication Date
EP3043929A1 true EP3043929A1 (fr) 2016-07-20
EP3043929B1 EP3043929B1 (fr) 2017-10-04

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EP14752593.5A Active EP3043929B1 (fr) 2013-09-09 2014-08-07 Classification de silicium polycristallin

Country Status (11)

Country Link
US (2) US10589318B2 (fr)
EP (1) EP3043929B1 (fr)
JP (1) JP6290423B2 (fr)
KR (1) KR101789607B1 (fr)
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Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015206849A1 (de) * 2015-04-16 2016-10-20 Wacker Chemie Ag Vorrichtung und Verfahren zur Klassierung und Entstaubung von Polysiliciumgranulat
BR102016017233B1 (pt) * 2015-07-23 2021-06-22 Cnh Industrial America Llc sistema de limpeza para uma colheitadeira-debulhadora agrícola
US9682404B1 (en) * 2016-05-05 2017-06-20 Rec Silicon Inc Method and apparatus for separating fine particulate material from a mixture of coarse particulate material and fine particulate material
US20230011307A1 (en) * 2019-12-17 2023-01-12 Wacker Chemie Ag Method for producing and classifying polycrystalline silicon
CN111359869A (zh) * 2020-02-26 2020-07-03 江苏鑫华半导体材料科技有限公司 电子级多晶硅筛分装置和方法
WO2022123077A1 (fr) 2020-12-11 2022-06-16 Zadient Technologies SAS Procédé et dispositif de production d'un matériau solide du type sic
CN116234759A (zh) 2021-03-24 2023-06-06 瓦克化学股份公司 用于硅块的运输容器
WO2023222787A1 (fr) 2022-05-18 2023-11-23 Zadient Technologies SAS Procédé de fabrication d'au moins une pièce de sic sans fissure
WO2024061466A1 (fr) 2022-09-22 2024-03-28 Wacker Chemie Ag Production de particules de silicium à teneur réduite en métaux de surface
DE102023102854B3 (de) 2023-02-06 2024-05-02 Alztec GmbH Vorrichtung und Verfahren zur flexiblen Klassierung von poly- und/oder monokristallinem Silizium

Family Cites Families (32)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3857751A (en) * 1971-11-15 1974-12-31 Tufdura Ltd Composite sheet capable of withstanding impingement by particulate materials
US4107035A (en) * 1977-05-02 1978-08-15 The Young Industries, Inc. Three-plane balance gyro sifter
EP0094741B1 (fr) * 1982-04-09 1990-02-07 William F. Hahn Tamisage différentiel
US4544102A (en) * 1982-04-09 1985-10-01 Penn Virginia Corporation Differential rate screening
JPS59147679A (ja) 1983-02-10 1984-08-24 ユ−オ−ピ−・インコ−ポレイテツド 耐摩耗性スクリ−ン
JPS59166878A (ja) 1983-03-11 1984-09-20 Advantest Corp 撮像装置試験用光源
JPS59166878U (ja) * 1983-04-25 1984-11-08 近畿工業株式会社 振動式ふるい機
SE435585B (sv) * 1983-05-16 1984-10-08 Kmw Mekan Ab Sallanordning
DE3811091A1 (de) 1988-03-31 1989-10-12 Heliotronic Gmbh Verfahren zum kontaminationsarmen zerkleinern von massivem stueckigem silicium
US5165548A (en) 1990-04-23 1992-11-24 Hemlock Semiconductor Corporation Rotary silicon screen
DE4218283A1 (de) * 1992-05-27 1993-12-02 Wacker Chemitronic Verfahren zum kontaminationsfreien Zerkleinern von Halbleitermaterial, insbesondere Silicium
DE19719698A1 (de) * 1997-05-09 1998-11-12 Wacker Chemie Gmbh Optoelektronische Klassiervorrichtung
JP3189764B2 (ja) * 1997-09-29 2001-07-16 住友金属工業株式会社 シリコン単結晶原料の溶解方法
JP3603142B2 (ja) * 1997-12-17 2004-12-22 株式会社トクヤマ 選別装置
DE19914998A1 (de) 1999-04-01 2000-10-12 Wacker Chemie Gmbh Schwingförderer und Verfahren zur Förderung von Siliciumbruch
EP1553214B1 (fr) 2002-02-20 2011-11-23 Hemlock Semiconductor Corporation Copeaux sous forme fluide et procédés pour leur utilisation
US8021483B2 (en) 2002-02-20 2011-09-20 Hemlock Semiconductor Corporation Flowable chips and methods for the preparation and use of same, and apparatus for use in the methods
US6874713B2 (en) * 2002-08-22 2005-04-05 Dow Corning Corporation Method and apparatus for improving silicon processing efficiency
AT411874B (de) 2003-03-07 2004-07-26 Statec Anlagentechnik Gmbh Siebvorrichtung
DE102005039118A1 (de) * 2005-08-18 2007-02-22 Wacker Chemie Ag Verfahren und Vorrichtung zum Zerkleinern von Silicium
DE102006016324A1 (de) * 2006-04-06 2007-10-25 Wacker Chemie Ag Vorrichtung und Verfahren zum flexiblen Klassieren von polykristallinen Silicium-Bruchstücken
DE102006016323A1 (de) 2006-04-06 2007-10-11 Wacker Chemie Ag Verfahren und Vorrichtung zum Zerkleinern und Sortieren von Polysilicium
DE102007027110A1 (de) * 2007-06-13 2008-12-18 Wacker Chemie Ag Verfahren und Vorrichtung zum Verpacken von polykristallinem Siliciumbruch
EP2036856B1 (fr) 2007-09-04 2018-09-12 Mitsubishi Materials Corporation Banc stérile et procédé de production de matière première pour silicium monocristallin
DE102007052473A1 (de) 2007-11-02 2009-05-07 Schott Solar Gmbh Verfahren und Vorrichtung zum Aussieben von Partikeln
CN201300122Y (zh) * 2008-09-30 2009-09-02 鞍山重型矿山机器股份有限公司 振幅递加式椭圆香蕉筛
PL2277633T3 (pl) 2009-07-16 2012-11-30 Univ Freiberg Tech Bergakademie Sposób i urządzenie do selektywnego klasyfikowania cząstek według ich wielkości
DE102010039752A1 (de) 2010-08-25 2012-03-01 Wacker Chemie Ag Polykristallines Silicium und Verfahren zu dessen Herstellung
DE102010039754B4 (de) 2010-08-25 2013-06-06 Wacker Chemie Ag Verfahren zur Bestimmung der Konzentration an Feinstaub in Silicium-Schüttgütern
DE102012202640A1 (de) 2012-02-21 2013-08-22 Wacker Chemie Ag Polykristallines Siliciumbruchstück und Verfahren zur Reinigung von polykristallinen Siliciumbruchstücken
DE102012208473A1 (de) * 2012-05-21 2013-11-21 Wacker Chemie Ag Polykristallines Silicium
US9475095B2 (en) * 2012-10-26 2016-10-25 M-I L.L.C. Shaker with automatic motion

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JP6290423B2 (ja) 2018-03-07
CN105612011B (zh) 2018-10-26
US20180169704A1 (en) 2018-06-21
CA2923110C (fr) 2017-11-07
WO2015032584A1 (fr) 2015-03-12
CA2923110A1 (fr) 2015-03-12
EP3043929B1 (fr) 2017-10-04
KR101789607B1 (ko) 2017-10-25
MY188174A (en) 2021-11-24
DE102013218003A1 (de) 2015-03-12
US20160214141A1 (en) 2016-07-28
US10589318B2 (en) 2020-03-17
TWI577459B (zh) 2017-04-11
KR20160047580A (ko) 2016-05-02
NO2960429T3 (fr) 2017-12-23
CN105612011A (zh) 2016-05-25
TW201509548A (zh) 2015-03-16

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