EP2001607B1 - Vorrichtung und verfahren zum flexiblen klassieren von polykristallinen silicium-bruchstücken - Google Patents

Vorrichtung und verfahren zum flexiblen klassieren von polykristallinen silicium-bruchstücken Download PDF

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Publication number
EP2001607B1
EP2001607B1 EP07727441A EP07727441A EP2001607B1 EP 2001607 B1 EP2001607 B1 EP 2001607B1 EP 07727441 A EP07727441 A EP 07727441A EP 07727441 A EP07727441 A EP 07727441A EP 2001607 B1 EP2001607 B1 EP 2001607B1
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Prior art keywords
fraction
sorting
optoelectronic
parameters
fractions
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German (de)
English (en)
French (fr)
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EP2001607A2 (de
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Marcus SCHÄFER
Reiner Pech
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Wacker Chemie AG
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Wacker Chemie AG
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    • 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
    • B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
    • 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
    • B07B13/003—Separation of articles by differences in their geometrical form or by difference in their physical properties, e.g. elasticity, compressibility, hardness
    • 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
    • B07B13/04—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices according to size

Definitions

  • the invention relates to an apparatus and method for flexibly classifying polycrystalline silicon fragments.
  • High purity silicon is produced by chemical vapor deposition of a high purity chlorosilane gas on a heated substrate.
  • the silicon is polycrystalline in the form of rods. These bars must be shredded for further use.
  • breaking tools for example made of metal baking or roll crushers, hammers or chisel are used.
  • the resulting fragments of polycrystalline silicon hereinafter referred to as Polybruch, are then classified according to defined breaking sizes.
  • a targeted separation according to length and / or surface can be achieved by optoelectronic sorting.
  • Such methods are for polysilicon z. B. off US 6,265,683 B1 .
  • the methods described herein are always limited to the separation of certain and previously known feed streams.
  • An optoelectronic separation of Polysilicon fragments is problematic when a high fines content (> 1 wt.% Fragments ⁇ 20mm) is present in the feedstock, as this significantly disturbs the image recognition of larger fragments. It is therefore not possible with the known devices, flexibly different input fractions into several grain classes in high accuracy after z. B. length and / or area to separate. In addition, no regulation is described, which leads to an even more accurate sorting result.
  • the object of the invention was to provide a device which allows a flexible classification of broken polycrystalline silicon (polysilicon), preferably according to the length and / or surface of the Polybruchs.
  • the length of a fragment is defined as the longest straight line between two points on the surface of a fragment.
  • the area of a fragment is defined as the largest shadow area of the fragment projected in a plane.
  • the invention relates to a device which is characterized in that it comprises a mechanical sieve and an optoelectronic sorting system, wherein the poly fraction is separated by the mechanical sieve into a silicon fines and a silicon remainder and the remaining silicon via an optoelectronic sorting is separated into further fractions.
  • the device allows a sorting of the poly rupture according to length, area, shape, morphology, color and weight in any combination.
  • the sorting plant consists of a multi-stage mechanical screening plant and a multi-stage optoelectronic sorting plant.
  • the mechanical and / or optoelectronic separation devices are arranged in a tree structure (see Fig. 1 ).
  • the arrangement of the screening and optoelectronic sorting system in a tree structure allows in comparison to a serial arrangement a more accurate sorting, as fewer separation stages must be run through and with each separation module, the rejection amount is lower.
  • the tree structure has shorter paths, whereby the wear of the system and the regrinding of large fragments are lower and there is a lower contamination of Polybruch. All this enhances the economy of the device and associated method.
  • the fine fraction of the polybrot to be classified is first separated by a mechanical sieve from the silicon residue and then separated by several mechanical sieving into other fractions.
  • any known mechanical screening machine can be used. Preference Schwingsiebmaschinen that are driven by an unbalance motor used. As Siebbelag mesh and perforated sieves are preferred.
  • the mechanical sieve system is used to separate fines in the product stream. The fine fraction contains grain sizes up to a maximum grain size of up to 25 mm, preferably of up to 10 mm.
  • the mechanical sieve therefore preferably has a mesh size which separates the mentioned grain sizes. Since the mechanical sieves therefore only have small holes at the beginning, in order to separate only the small breakage types ( ⁇ BG1), there is less blockage of the sieve, which increases the productivity of the system. The problematic large poly fragments can not settle in the small Siebmaschenweiten.
  • the fine fraction can be separated into further fractions.
  • the screening plants can successively or in another structure, such as. B. a tree structure, be arranged.
  • the sieves are preferably arranged in more than one stage, particularly preferably in three stages in a tree structure. For example, in an intended split of the poly-break into four grain fractions (eg, fraction 1, 2, 3, 4), in a first stage, fractions 1 and 2 are separated from fraction 3 and 4. In a second stage then fraction 1 of fraction 2 and a parallel third stage fraction 3 of fraction 4 are separated.
  • the sorting of the residual polysilicon content can be carried out according to all criteria that are state of the art in image and sensor technology.
  • an optoelectronic sorting is used. It preferably takes one or more, more preferably one to three, of the criteria selected from the group length, area, shape, morphology, color and weight of the polysilicon fragments. It is particularly preferably carried out according to the length and area of the polysilicon fragments.
  • the residual silicon content is separated by one or more optoelectronic sorting into further fractions.
  • 2, 3 or more optoelectronic sorting systems which are arranged in a tree structure, are used.
  • the optical image recognition of the optoelectronic sorting system has the advantage that "real" lengths or areas are measured. This allows a comparison with conventional mechanical screening method more accurate separation of the fragments according to the particular desired parameters.
  • an optoelectronic sorting system is preferably a device, as in US 6,265,683 B1 or in US 6,040,544 A is described. Reference is therefore made to these documents with regard to the details of the optoelectronic sorting system.
  • This optoelectronic sorting system comprises a device for separating the poly-break and a sliding surface for the poly-fracture, wherein the angle of the sliding surface is adjustable to the horizontal, and a radiation source through the beam path of the poly break falls and a shape detection device, which forwards the shape of the Klassierguts to a control unit, which controls a deflection device.
  • the product stream is separated via an integrated vibrating conveyor trough and passed over a slide in free fall one or more CCD Farzeilenmentss, the classification of one or more sorting parameters selected from the group length, area, volume (weight), shape , Morphology and color makes.
  • CCD Farzeilenments the classification of one or more sorting parameters selected from the group length, area, volume (weight), shape , Morphology and color makes.
  • all known in the art electronic sensor techniques can be used for the parameter recognition of the fragments.
  • the measured values are transmitted to the higher-level control and regulating device and z. B. evaluated by microprocessor. It is decided by comparison with the stored in the recipe sort criterion, whether a fragment is discharged from the product stream or transmitted.
  • the discharge preferably takes place via nozzles by compressed air pulses, wherein the pressure on the recipe in the higher-level control is adjustable.
  • the pressure on the recipe in the higher-level control is adjustable.
  • via a arranged under the image recognition valve strip separating channels (compressed air strips) are controlled and metered with compressed air pulses, which are dependent on the grain size.
  • the device according to the invention is therefore provided with a higher-level control, which makes it possible, the Sorting parameters, according to which the poly-break is sorted and / or the system parameters that influence the promotion of the Polybruchs (eg the conveying speed), flexibly adjust to the individual parts of the devices.
  • the sorting parameters by which the polybranch is sorted are preferably the abovementioned parameters, more preferably selected from the group length, area, morphology, color or shape of the fragments.
  • the sizes of the sorting parameters, according to which the poly-break is sorted, are preferably stored in the form of recipes in the higher-level control, and a variation of the selection criteria in the mechanical screening device and / or the opto-electronic sorting takes place via the selection of a recipe, which then selects the associated sorting parameters in the individual parts of the device according to the invention causes.
  • the device according to the invention after the sorting system comprises scales for determining the weight yields of the classified fractions.
  • the device according to the sorting system comprises a fully automatic Kistenab spall- and box transport device.
  • a preferred embodiment of the device is characterized in that the mechanical screen and / or the optoelectronic sorting system is provided with a measuring device for defined parameters of classified polysilicon fracture and this measuring device is connected to a higher-level control and regulating device, which statistically the measured parameters evaluates and compares with predetermined parameters and in a deviation between measured parameters and predetermined parameters, the setting of the sorting parameters of the optoelectronic sorting system or the entire sorting system (eg frequency of the mechanical screen or conveyor speeds of the poly fragments) or the selection of recipes can change in that the parameter then measured adjusts to the given parameter.
  • the mechanical screen and / or the optoelectronic sorting system is provided with a measuring device for defined parameters of classified polysilicon fracture and this measuring device is connected to a higher-level control and regulating device, which statistically the measured parameters evaluates and compares with predetermined parameters and in a deviation between measured parameters and predetermined parameters, the setting of the sorting parameters of the optoelectronic sorting system or the entire sort
  • a parameter is measured from the group length, area, shape, morphology, color and weight of the polysilicon fragments.
  • the length or the area of the polysilicon fragments within the respective fraction is particularly preferably measured and evaluated in the form of lengths or area distributions (eg 5%, 50% or 95% quantile).
  • the weight yields of the individual sieve fractions are determined by the scales at the sieve sheds.
  • Another measuring parameter is the mass and particle throughput determined at the individual optoelectronic sorting plants.
  • the conveying speed can be adjusted, for example, on the basis of the measured number of particles so as not to overload the system and / or to select a different sorting recipe.
  • the sorting parameters (for example length average value of a fraction) of the classified polysilicon fraction determined in the optoelectronic sorting system as part of the on-line monitoring according to the sorting criteria (eg length distribution, weight distribution) are transmitted to the higher-level control and regulating device and compared there with predetermined setpoints.
  • the variable sorting parameters (for example the separation limits between two fractions or the driving mode through the modules) are changed by the control and regulating device in such a way that the measured parameter adjusts to the predetermined parameter.
  • control device regulates the separation boundaries between the fractions, the flow rate through the conveyor troughs or the pressure at the outlet nozzles.
  • magnetic separators for example plate magnets, drum magnets or strip magnets
  • plate magnets for example plate magnets, drum magnets or strip magnets
  • the control and regulating device preferably consists of a control system in the form of a programmable logic controller (PLC) via which the controls of all units (eg mechanical and optoelectronic sorting system, automated box handling with recipe management and management of the control logic) are managed and controlled.
  • PLC programmable logic controller
  • the cross-plant visualization and operation is carried out by a higher-level control system.
  • the fault and operating messages of all units are evaluated and visualized together in a fault or operating message database.
  • the device according to the invention allows a flexible separation with different particle size distribution of the feed material. Both very small (length ⁇ 45 mm) and very large cubic fraction (length> 45 - 250 mm) can be classified without mechanical modifications by simple software control.
  • the inventive device allows a higher separation accuracy with respect to length and / or area of the fragments in comparison to a purely mechanical screening.
  • the device can be regulated by feedback of the sorting parameters (eg mean value of the grain fraction (BG) measured in the optoelectronic screening plant) as reference variables for the sorting plants (eg separation limits at the individual optoelectronic sorting stages).
  • the control and regulation can also be adapted via the recipes.
  • the device according to the invention enables on-line monitoring of the quality of the feed material (eg via the statistical evaluation of the particle size distribution after breaking) in accordance with the sorting criteria (eg length distribution, weight distribution).
  • the sorting criteria eg length distribution, weight distribution.
  • the invention further relates to a method in which a poly-fracture is classified by means of a device according to the invention.
  • the poly-break is separated by a mechanical sieve in a sieved fine and a residual fraction, wherein the screened fine fraction by means of another mechanical sieve is separated into a target fraction 1 and a target fraction 2 and the residual fraction is separated by means of an optoelectronic sorting into two fractions, these two fractions are divided by means of a further optoelectronic sorting into 4 other target fractions (target fractions 3 to 6) ,
  • the inventive method has a high productivity, since the set-up times are lower than in known classifiers and it is less likely to become clogged as mechanical sieves.
  • the screened fine fraction has a particle size of less than 20 mm
  • the residual fraction has a particle size of greater than 5 mm
  • the target fraction 1 has a particle size of less than 10 mm
  • the target fraction 2 has a particle size of from 2 mm to 20 mm
  • the Target fraction 3 has a particle size of 5 mm to 50 mm
  • the target fraction 4 has a particle size of 15 mm to 70 mm
  • the target fraction 5 has a particle size of 30 mm to 120 mm
  • the target fraction 6 has a particle size of greater than 60 mm.
  • the input of the sorting parameters of the desired target fractions into a higher-level control and regulating device which causes a corresponding adjustment of the parameters of the sorting systems to achieve the desired target fractions of Polybruch.
  • the setting of the parameters of the sorting systems is carried out as described for the device according to the invention.
  • the fraction with the larger number of particles with respect to the respective sorting parameter is preferably rejected or blown out in each case.
  • a preset recipe is selected at the higher-level controller of the device according to the invention.
  • the recipes contain all the parameters of the sorting system and the manipulated variables of the control system.
  • the measurement of the product parameters as well as the classification of the polysilicon fracture is preferably carried out as described below:
  • the oversize grain of the first mechanical screening stage is fed to a multi-stage optoelectronic separation plant.
  • the product stream is separated via an integrated vibrating conveyor trough and passed over a slide in free fall one (or more) CCD color line camera (s), the classification according to one or more of the parameters length, area, volume, shape, morphology and color in any combination.
  • CCD color line camera Alternatively, all known in the art electronic sensor techniques can be used for the parameter recognition of the fragments.
  • the measured values are transmitted to the higher-level control and regulating device and z. B. evaluated by microprocessor. It is decided by comparison with the stored in the recipe sort criterion, whether a fragment is discharged from the product stream or transmitted.
  • the discharge is preferably carried out by compressed air pulses, wherein the pressure on the recipe in the higher-level control is adjustable.
  • the pressure on the recipe in the higher-level control is adjustable.
  • the discharge can also be done hydraulically or mechanically. Surprisingly, it has been found that a higher sorting accuracy is achieved when the smaller fraction in terms of length is blown out, although this Fraction has a higher number of particles.
  • the recognition by means of a sensor preferably by means of an optical image recognition, has the advantage that "real" lengths, areas or shapes of the fragments are measured. This allows for a comparison with conventional mechanical screening method more accurate separation, z. B. regarding. The length of the fragments. The overlap between two fractions to be separated is less.
  • the cut-off limits can be set as required via the specified parameters (the recipe) of the higher-level control without making any changes to the machine itself (such as changing the screen coverings).
  • the inventive combination of mechanical sieve and optoelectronic sorting system for the first time a separation in both small and large fraction size range, regardless of the composition of the feed, possible.
  • the entire plant can be controlled via the "on-line measurement", in which, for example, the separation limits are directly corrected according to the feedstock.
  • the optoelectronic sorting in the device according to the invention offers the advantage that a more precise separation of the fragments according to the respective requirements (eg high cubicity of the fragments) is possible due to the combination of area and length.
  • the lengths refer to the maximum length of the fragments, with 85% by weight of the fragments having a maximum length within the specified limits.
  • Polysilicon was deposited by the Siemens method in the form of rods.
  • the rods were removed from the Siemens reactor and crushed by methods known in the art (eg, by manual comminution) to polysilicon coarse fracture.
  • This rough fracture with fragments of an edge length of 0 to 250 mm was emptied via a feeder, preferably a funnel, onto a conveyor trough which conveys the material to the device according to the invention.
  • the parameters for the fractions to be produced were entered into the higher-level measuring and control device. Since a particular desired particle size distribution in the different fractions is in each case given by the respective further use of the fracture to be produced, the fractions are usually stored as recipes in the higher-level measuring and control device and are selected accordingly. In the present example, the device was used for the production of 6 different fractions (BG 0, 1, 2, 3, 4 and 5).
  • the recipes contain all the parameters of the optoelectronic and mechanical sorting system and the conveyor system.
  • the fines (BG 0 and 1) of the Polybruchs was separated on a mechanical sieve with a mesh size of about 10 mm and then the separated portion with a further mechanical Sieve, or another sieve with a mesh size of approx. 4 mm, separated into BG 0 and 1.
  • the coarse fraction (BG 2, 3, 4 and 5) was conveyed via a conveyor trough whose conveying characteristics, such as, for example, B. Frequency, also stored in the recipe, fed to the optical sorting system and separated over two tree levels, or three optical stages as follows: In the first stage BG 3 & 2 was separated from BG 4 & 5. As a separation limit, the recipe has a maximum length of 55 mm. BG 3 & 2 was separated into BG 3 and 2 in a second stage or a separation limit of 27 mm stored in the recipe. The BG 4 & 5 in a third stage and a separation limit of 100 mm in the BG 4 and 5.
  • Fig. 2 shows the result of this classification compared to an optopneumatic separation with the same optopneumatic separator without prior sieving. It is clear that the feed material could be sorted into the selected length classes. The opposite to conventional screening more accurate separation (example length) is visible. So z.
  • BG2 / BG3 overlap in conventional separation it can be seen that the BG2 distribution ends at only about 45 mm, whereas the BG3 distribution already starts at 20 mm. The overlap is therefore 25 mm.
  • the BG2er distribution already ends at about 40 mm while the BG3er distribution starts only at 25 mm at the same time. The overlap is thus only 15mm and thus 40% less than in the prior art.
  • the software parameters were slightly varied with respect to separation limits of the individual fractions.
  • the values for the maximum or minimum permissible length of the fragments in the individual fractions have been changed by a few millimeters (see Fig. 3 ).
  • the separation limit for blow-out between BG 2 and 3 was changed from 27 mm to 31 mm and between BG 3 and 4 from 55 mm to 57 mm.
  • This program parameter change of just a few millimeters is already evident in the product properties (eg length distribution), ie the separation boundaries between the individual fractions can be flexibly adapted to the respective specification with high accuracy by simple recipe selection, or The online control system to achieve desired target values.

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  • Sorting Of Articles (AREA)
  • Combined Means For Separation Of Solids (AREA)
  • Silicon Compounds (AREA)
EP07727441A 2006-04-06 2007-03-28 Vorrichtung und verfahren zum flexiblen klassieren von polykristallinen silicium-bruchstücken Active EP2001607B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006016324A DE102006016324A1 (de) 2006-04-06 2006-04-06 Vorrichtung und Verfahren zum flexiblen Klassieren von polykristallinen Silicium-Bruchstücken
PCT/EP2007/052969 WO2007115937A2 (de) 2006-04-06 2007-03-28 Vorrichtung und verfahren zum flexiblen klassieren von polykristallinen silicium-bruchstücken

Publications (2)

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EP2001607A2 EP2001607A2 (de) 2008-12-17
EP2001607B1 true EP2001607B1 (de) 2009-07-22

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US (1) US10478860B2 (ko)
EP (1) EP2001607B1 (ko)
JP (1) JP4988821B2 (ko)
KR (1) KR101068488B1 (ko)
CN (1) CN101415503B (ko)
CA (1) CA2647721C (ko)
DE (2) DE102006016324A1 (ko)
ES (1) ES2328295T3 (ko)
WO (1) WO2007115937A2 (ko)

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KR20080108273A (ko) 2008-12-12
JP2009532319A (ja) 2009-09-10
US20090120848A1 (en) 2009-05-14
CN101415503B (zh) 2012-11-14
WO2007115937A3 (de) 2007-11-29
CA2647721C (en) 2011-08-30
KR101068488B1 (ko) 2011-09-28
EP2001607A2 (de) 2008-12-17
CA2647721A1 (en) 2007-10-18
JP4988821B2 (ja) 2012-08-01
DE502007001136D1 (de) 2009-09-03
ES2328295T3 (es) 2009-11-11
DE102006016324A1 (de) 2007-10-25
CN101415503A (zh) 2009-04-22
US10478860B2 (en) 2019-11-19

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