Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
  • B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
• • 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
  • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
  • C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
  • C23C16/24—Deposition of silicon only
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/56—After-treatment
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
  • G01N29/04—Analysing solids
  • G01N29/09—Analysing solids by measuring mechanical or acoustic impedance
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
  • H10F77/00—Constructional details of devices covered by this subclass
  • H10F77/10—Semiconductor bodies
  • H10F77/12—Active materials
  • H10F77/122—Active materials comprising only Group IV materials
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
  • H10F77/00—Constructional details of devices covered by this subclass
  • H10F77/10—Semiconductor bodies
  • H10F77/16—Material structures, e.g. crystalline structures, film structures or crystal plane orientations
  • H10F77/162—Non-monocrystalline materials, e.g. semiconductor particles embedded in insulating materials
  • H10F77/164—Polycrystalline semiconductors
  • H10F77/1642—Polycrystalline semiconductors including only Group IV materials
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N2291/00—Indexing codes associated with group G01N29/00
  • G01N2291/02—Indexing codes associated with the analysed material
  • G01N2291/023—Solids
  • G01N2291/0234—Metals, e.g. steel
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E10/00—Energy generation through renewable energy sources
  • Y02E10/50—Photovoltaic [PV] energy
  • Y02E10/546—Polycrystalline silicon PV cells
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E10/00—Energy generation through renewable energy sources
  • Y02E10/50—Photovoltaic [PV] energy
  • Y02E10/547—Monocrystalline silicon PV cells

Definitions

• the invention relates to a process for the production of polycrystalline silicon.
• Polycrystalline silicon (polysilicon for short) serves as
• Multicrystalline silicon after various drawing and casting processes for the production of solar cells for photovoltaics.
• Polycrystalline silicon is usually by means of the
• Siemens process produced in this method, in a bell-shaped reactor ("Siemens reactor") carrier body, usually thin filament rods made of silicon, heated by direct passage of current and containing a reaction gas
• silicon-containing component trichlorosilane (SiHCl 3 , TCS) or a mixture of trichlorosilane with
• SiH 2 Cl 2 Dichlorosilane (SiH 2 Cl 2 , DCS) and / or with tetrachlorosilane (SiCl 4 , STC) used.
• Silane (SiH 4 ) is used more rarely but also on an industrial scale.
• Diameter increases with time.
• the reactor bell After cooling the rods, the reactor bell is opened and the rods are made by hand or with the help of special Devices, so-called removal aids for further processing or for temporary storage taken.
• Both the storage and the further processing, especially a crushing of the rods, a classification and packaging of broken pieces, are usually carried out under special environmental conditions in air-conditioned rooms, which is a
• the deposited material is exposed to environmental influences, in particular dust particles.
• the morphology and microstructure of the growing rod are determined by the parameters of the deposition process.
• the morphology of the deposited rods can range from compact and smooth (as described, for example, in US 6,350,313 B2) to highly porous and fissured material (such as in U.S. Pat
• the concentration of the silicon-containing component is too high, it may be more homogeneous
• Morphology of the deposited silicon rods is not compact enough to that with the growing rod diameter
• silicon rods are required, such as cracks, pores, joints, joints, etc.
• silicon rods are broken into small pieces, which are usually subsequently classified by size.
• Sorting of polysilicon is described for example in US 2007/235574 AI.
• US 2009081108 AI discloses a workbench for manual
• Ionization system is implemented to allow electrostatic charges by active air ionization
• Ionizers permeate the clean room air with ions in such a way that static charges on insulators and
• US 2007235574 AI discloses a device for crushing and sorting polycrystalline silicon, comprising
• Feeding device for a polysilicon coarse fracture in a crusher, the crusher, and a sorting system for classifying the polysilicon fracture characterized in that the device is provided with a control, the variable setting at least one crushing parameter in the crusher and / or at least one Sorting parameters in the sorting system allows.
• a polysilicon rod is placed on the breaker table of the pre-shredder. On the break table there is a visual quality control of the bar
• EP 2479142 A1 discloses a method for producing a polycrystalline silicon piece
• the fragments obtained by comminution of the residual bar have a low content of chromium, iron, nickel, copper and cobalt.
• the object is achieved by a method for producing polycrystalline silicon, comprising depositing
• Silicon rods are obtained, removal of the polycrystalline silicon rods from the at least one reactor, crushing the expanded polycrystalline silicon rods into fragments, characterized in that after the removal of the
• the rod-shaped polycrystalline silicon is classified by at least one feature in at least two quality classes, which at least two quality classes separate
• the invention therefore provides for a classification into at least two quality classes on the removed silicon rods. This classification is done before
• Fracture size 1 [mm] 4 to 15;
• Silicon rod for analysis purposes, in particular for the investigation of a classification feature, should not be considered in the context of the invention as comminution of the polycrystalline
• the classification into at least two quality classes can be made with respect to that taken from only one reactor
• the at least two different further processing steps lead to at least two
• Silicon e.g. from the three upper classes
• a further processing step "crushing to fraction size 5" For example, a further processing step "crushing to fraction size 5", another, different further processing step “crushing to fraction size 3" read.
• the classification may provide that whole bars are assigned to certain quality classes.
• the classification feature may be the feature "position of the silicon in the rod”.
• the classification feature may be the feature "position of the rod in the reactor".
• the classification feature may be an optical one
• the classification feature can be a measurable one
• It may be a mechanically measurable feature selected from the group consisting of hardness of the rods or rod parts, bending strength of the rods or rod parts,
• Rod parts sound of the rods or rod parts after mechanical excitation, natural vibration frequency of the rods or rod parts, fracture behavior of the rods or rod parts spontaneously or at
• act measurable feature selected from the group consisting of thermal conductivity of the rods or rod parts, electr.
• Rod parts absorption spectrum of the rods or rod parts
• Emission spectrum of the rods or rod parts after excitation e.g., thermal, electrical, optical
• the measurable feature may be further selected from the group consisting of spots on the surface of the bars or rod parts, surface deformations of the bars or rod parts, Surface structure of the bars or rod parts, thickness of the bars or rod parts, shape of the bars or rod parts, length of the bars, weight of the bars or rod parts, porosity of the bars or
• Rod parts density of the bars or rod parts and appearance of the bars or rod parts (visual personal impression of quality) and combinations of the features mentioned.
• the classification feature may be, for example, the rod diameter.
• Contamination of the surface of the bars or rod parts with dust e.g., silicon dust
• dust e.g., silicon dust
• classification features include air temperature and composition (including impurities) during rod assembly and in the time to classify, condition of
• the interface of the filament rods to the deposited silicon (color, shape, thickness and composition of a possibly.
• the invention preferably also provides for separating a part of a silicon rod in order to use this part on the basis of a
• Classify classification feature e.g. by removing the surface or breaking the rod into pieces.
• a classification of the fragments takes place on the basis of at least one classification feature selected from the group consisting of porosity, cracks, holes, spots,
• Suitable classification features before deposition are reaction gases (impurities with metals, non-metals and foreign gases) and the filament rods used (thickness, shape, length, contamination on the surface and in the volume).
• a classification feature selected from the group consisting of Selected reactor type, Selected equipment of the reactor (electrodes, nozzles,
• Rod parts are separated so that rod parts result that are only compact and rod parts that also contain porous parts.
• the rod parts, which also contain porous parts, are broken down into pieces for the solar industry
• a classification is carried out by position in the reactor.
• Position can be selected in the reactor during the deposition.
• the arrangement of the rods in the reactor has an influence on the
• Modern reactors include At least 20 filament rods, which serve as a carrier body for the deposition of polycrystalline silicon. A reactor also sees gas inlet openings for reaction gas in the
• Reactor chamber which are nozzles which are aligned vertically upwards relative to a bottom plate of the reactor chamber. It may also be provided a nozzle in the center of the bottom plate.
• One or more exhaust ports are preferably placed in the reactor center around or around the central nozzles around the central nozzles and / or placed between the reactor wall and the outer silicon rods.
• the reactor chamber has a round or one adapted to the number of filament rods and optimal use of space, for example, hexagonal cross-section.
• each silicon rod (with the exception of rods, which stand next to the reactor wall) at a distance of 150 to 450 mm has three more silicon rods and one to three Switzerlandasdüsen. Those three other silicon rods are referred to as adjacent rods or neighboring rods.
• the distance to nozzles and neighboring bars is between 200 and 350 mm.
• the individual distances between the adjacent silicon rods or nozzles can be
• a difference in the distances to the individual adjacent silicon rods and nozzles is less than 50%
• Reactor wall have at the same distance only 1 to 3 three more silicon rods and 1 to 3 gas inlet openings.
• the angles between the directions of silicon rod to the neighboring rods and from the silicon rod to the adjacent nozzles are preferably between 90 and 150 °, more preferably between 105 and 135 °, most preferably around 115-125 °.
• rods in the middle of the reactor can reach higher temperatures and thus grow faster and more porous than the rods located outside, close to the reactor wall.
• a classification according to morphological expression takes place.
• a classification based on the morphology of the bars can be made immediately after the bars have been removed: either whole bars or even parts of these bars (e.g., peeled surface) are classified into separate quality classes.
• the ultrasound coupling means Bubble-free demineralized water in water jet technology, the ultrasonic waves after passing through the polysilicon molding of an ultrasonic receiver
• 20080053232 AI to take By the method can be sorted for defects with a projection area greater than 0.03 mm 2 .
• One possible classification feature is the presence or absence of defects of this size. Accordingly, it is sorted into two quality classes.
• the polysilicon shaped body investigated can be a polycrystalline silicon rod or a separate rod part.
• classification may also be made for other abnormalities.
• Further abnormalities may be, for example, deposits or stains that may occur even on a single bar of a batch.
• the fragments are classified on the basis of at least one feature into at least two quality classes, wherein those at least two quality classes are supplied to at least two different further processing steps, wherein those at least two different Further processing steps lead to at least two product classes.
• This classification of fragments can also be done after a wet chemical treatment. Just after one
• wet-chemical treatment often causes stains on individual fragments.
• a suitable wet-chemical treatment is described in EP 0 905 796 B1. It is particularly preferred to give the employee of the cleaning line a spot catalog in the hand, in the
• Another classification feature is the
• Dopant content is.
• the measurement can be done at different staff locations by a sample is taken.
• Silicon rod were generated (eg by drilling), placed in a Siliziumgef ß and with the silicon vessel to a Single crystal processed. Here, however, must by the
• Dopants B, P, As, Al
• SEMI MF 1398 an FZ single crystal
• a disk (wafer) is separated from the monocrystalline rod produced from a polycrystalline silicon rod or polycrystalline silicon fragments by means of FZ, etched with HF / HNO 3 , rinsed with 18MOH of water and dried. At this disc, the photoluminescence measurements
• Treatment is supplied while the other quality class is processed without such a cleaning step.
• Rod or CZ break, which may be cleaned or unpurified.
• a product class looks ahead of a polycrystalline
• a silicon rod having a diameter of at least 150 mm comprising a core (A) having a porosity of 0 to less than 0.01 ⁇ m around a thin rod (support body, filament) and at least two subsequent regions B and C which differ in their porosity by one Differ from 1.7 to 23, wherein the outer region C is less porous than the region B.
• a portion of the silicon rod having a porosity of less than 0.01 is considered compact within the scope of the invention.
• the core of the silicon rod is therefore compact in this product class.
• a range with a porosity of 0.01 to 0.1 is referred to as "dense material" or "dense layer”.
• Area C is dense material.
• core A extends over one
• the thin rod on which core A is deposited typically has a dimension of a few mm to 12 mm.
• core A typically starts e.g. with a diameter of 9 mm and extends up to a maximum diameter of 60 mm.
• Core A preferably extends to a maximum diameter of 50 mm, particularly preferably a maximum of 40 mm.
• the region B following the core A has the largest porosity of 0.06 to 0.23 and extends over a diameter range of 15% to 90% of the diameter of the silicon rod.
• region B extends over a diameter range of 20-80%.
• the subsequent region C has a lower porosity of 0.01 to 0.1 and extends over a diameter range of 50% to 100% of the total diameter of the silicon rod.
• region C extends over a diameter range of 60-100%, more preferably over a range of 70-100%.
• the porosity in the region C is constant. It is particularly preferred if the porosity in the region C with
• a final layer Z is applied to the porous regions B and C, with a
• Diameter range from 90% to 100% of the total diameter.
• a particularly preferred diameter range is 95-100%.
• the Z-layer has a thickness of at least 7.5 mm.
• Silicon rod can produce polycrystalline Siliziumbruchstucke.
• the comminution of the rods is preferably carried out in accordance with EP 2 423 163 A1 with subsequent dedusting of the fragments by means of compressed air or dry ice. It is likewise preferred to break the rods into fragments analogously to US Pat. No. 3,874,905
• Classifying or sorting fragments of size classes from about 0.5 mm to 200 mm and then one
• Fragments of different porosities or fragments comprising regions of different porosities are included.
• the porosities of individual fragments vary from 0 to 0.25. There are two quality classes:
• Individual fragments have a porosity of 0 to less than 0.01 and come from the compact core of the silicon rod or from the optional Z-layer.
• fragments are more or less porous and have porosities of 0.01 to 0.25.
• the total porosity of a sample is composed of the sum of the voids communicating with each other and with the environment and unconnected Cavities.
• the total porosity ie the proportion of the total pore volume (open and closed pores) on the
• Total volume of polysilicon is determined according to DIN-EN 1936 from the calculation of raw and true density, i.
• the bulk density is defined as the density of the polysilicon including the pore space in the dry state according to DIN-EN 1936 (weighing volume-defined test specimens or measuring the buoyancy of the saturated sample in mercury with a hydrostatic balance).
• the compact core A of the polycrystalline silicon rod preferably has a bulk density of 2.329 (porosity 0).
• Region B preferably has a bulk density of 1.8 to 2.2.
• Region C preferably has a bulk density of 2.1 to 2.3.
• Layer Z preferably has a bulk density of 2.25 to 2.329. Another product class sees a polycrystalline
• Silicon rod comprising an outer layer
• polycrystalline silicon having a thickness of 0.01 to 20 mm, said outer layer includes crystallites having an average size of more than 20 ⁇ ago.
• the average size of the crystallites of the outer layer is at most 80 ⁇ .
• the average size of the crystallites of the outer layer is at most 80 ⁇ .
• the polycrystalline silicon rod below the outer layer has a porous or fissured structure.
• the structure in the interior of the polycrystalline silicon rod is similar (ie, has the same crystal structure, crystallite size, etc.) inside, including pores, joints, crevices, cracks, and fractures.
• the outer layer consists of crystallites having an average size greater than the average size of the krxstallites below the outer layer. The invention thus makes it possible to classify according to compact and porous proportions of polycrystalline silicon.
• Polysilicon production can be driven much more flexible. High quality material is also used for high quality use. Compact material produced in the manufacture of solar products can also be used for higher quality products (CZ).

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• Physics & Mathematics (AREA)
• Chemical Kinetics & Catalysis (AREA)
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• 2013
  • 2013-04-22 DE DE201310207251 patent/DE102013207251A1/de not_active Withdrawn
• 2014
  • 2014-03-24 JP JP2016509348A patent/JP6567501B2/ja active Active
  • 2014-03-24 US US14/785,918 patent/US10400329B2/en active Active
  • 2014-03-24 EP EP14714215.2A patent/EP2989052B1/de active Active
  • 2014-03-24 CN CN201480035722.9A patent/CN105339302A/zh active Pending
  • 2014-03-24 KR KR1020157032942A patent/KR101801757B1/ko active Active
  • 2014-03-24 ES ES14714215.2T patent/ES2677489T3/es active Active
  • 2014-03-24 WO PCT/EP2014/055837 patent/WO2014173596A1/de not_active Ceased
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• 2015
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