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US20100300495A1 - Method for purifying polycrystalline silicon - Google Patents

Method for purifying polycrystalline silicon Download PDF

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Publication number
US20100300495A1
US20100300495A1 US12/675,297 US67529708A US2010300495A1 US 20100300495 A1 US20100300495 A1 US 20100300495A1 US 67529708 A US67529708 A US 67529708A US 2010300495 A1 US2010300495 A1 US 2010300495A1
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United States
Prior art keywords
fragments
purifying
polysilicon
nozzles
pptw
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.)
Abandoned
Application number
US12/675,297
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English (en)
Inventor
Hanns Wochner
Christian Gossmann
Herbert Lindner
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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Assigned to WACKER CHEMIE AG reassignment WACKER CHEMIE AG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GOSSMANN, CHRISTIAN, LINDER, HERBERT, WOCHNER, HANNS
Publication of US20100300495A1 publication Critical patent/US20100300495A1/en
Abandoned legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • 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
    • 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
    • C01B33/037—Purification
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H01L21/67028—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
    • H01L21/6704—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing
    • H01L21/67057—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing with the semiconductor substrates being dipped in baths or vessels

Definitions

  • the invention relates to a method for purifying polycrystalline silicon with an improved flow of the purifying solutions in the process.
  • High-purity semiconductor material is required for the production of solar cells or electronic components, such as memory elements or microprocessors for example.
  • the dopants introduced in a targeted manner are the only impurities that a material of this type should have in the most expedient case. Therefore, endeavors are made to keep the concentrations of harmful impurities as low as possible. It is often observed that semiconductor material that has already been produced with high purity is contaminated again in the course of further processing to form the target products. Therefore, complicated purifying steps repeatedly become necessary in order to restore the original purity.
  • contamination by metal atoms should be regarded as critical since the latter can alter the electrical properties of the semiconductor material in a harmful manner. If the semiconductor material that is to be comminuted is comminuted, in the manner that has predominantly been customary heretofore, by means of mechanical tools, such as crushers made of steel, for example, then the fragments have to be subjected to surface purifying prior to melting.
  • the surface of the mechanically processed polycrystalline silicon is etched using a mixture of nitric acid and hydrofluoric acid.
  • the metal particles are attacked to a great extent by the acid mixture during the preliminary purifying.
  • Metal carbide residues remain, and are dissolved to the greatest possible extent during the HF/HNO 3 main purifying.
  • the polysilicon fragments are usually dipped successively into different purifying solutions during purifying in baskets or basins.
  • EP 0905796 describes a purifying process comprising preliminary purifying by means of a mixture comprising HF/HCl/H 2 O 2 , main purifying by means of HF/HNO 3 and subsequent hydrophilization of the silicon surface by means of HCl/H 2 O 2 .
  • rinsing takes place in throughflow or dump tanks.
  • the silicon fragments are purified in a purifying machine on the basis of an up and down movement.
  • the basin loaded with polysilicon fragments can also move completely out of the liquid during the lifting/lowering movement, in order that the purifying solution can completely drain away from the silicon fragments.
  • a disadvantage that emerges is that spots having a gray appearance are found on the silicon fragments in the course of the process.
  • US 2006/0042539 describes an apparatus in which the tray in the container is caused to effect a regulated translational movement in a lateral direction during the treatment duration.
  • the translational movement leads to the same results as the lifting/lowering movement described in EP 0905 796.
  • the problem of the dead water zone at the contact points cannot be solved with an apparatus of this type either.
  • the object was to provide an improved method for purifying polysilicon fragments in which no dead water zones occur and the formation of spots on the polysilicon fragments is thus prevented.
  • the rinsing capacity is intended to be high enough that acid residues are no longer detectable on the polysilicon fragments.
  • the invention relates to a method for purifying polysilicon fragments, characterized in that the flow of the purifying liquid in at least one of the process steps has a flow velocity of greater than 100 mm/sec, which impinges on the surface of the polysilicon fragments from more than two different directions.
  • the method according to the invention has made it possible to improve the substance exchange during the residence times of the polysilicon fragments in the purifying baths in such a way that no dead water zones arise in the bulk material and so spots no longer arise on the polysilicon fragments. It has become possible to significantly increase the etching removal with the same acid concentration.
  • the improvement in the flow conditions between the contact points of the individual fragments is obtained by means of non-directional, diffuse injection of the purifying liquid into the etching tank, by means of alternately active nozzles ( FIG. 1 ).
  • a plurality of nozzles for introducing the purifying liquid ( 2 ) are situated in the etching tank ( 1 ), said nozzles being fitted to the base and to the side walls.
  • the bulk material is suspended on the sides and on the base in a basin ( 3 ) having openings ( 4 ) in the etching tank. Numbers of nozzles of between 1 and 1000 are preferred in this case. 10 to 100 nozzles are particularly preferred.
  • the etching mixture emerges from said nozzles at a velocity of greater than 100 mm/sec. Flow velocities of 100 to 200 mm/sec are preferred, particularly preferably 150 mm/sec.
  • the nozzles can be opened in a temporally staggered manner in an alternating cycle with a temporal delay of 0.1 to 60 sec for a time of 0.1 to 60 sec. Temporal delays of 1 to 4 sec and an adjustable opening time of 0.2 to 1 sec are preferred.
  • the nozzles have an opening of 0.01 to 5 mm. An opening of 0.5 to 2 mm is preferably used. 50 nozzles having an exit diameter of 1 mm are particularly preferred.
  • the alternate incident flow on the individual fragments prevents dead water zones from arising at the contact points between the poly fragments. A uniform flow velocity prevails at all points in the bulk material.
  • the improvement in the flow conditions between the contact points of the individual fragments is produced by one or more moved nozzle rings in the etching tank ( FIG. 2 ).
  • moved, rotating nozzle rings ( 5 ) are arranged around the process basin ( 3 ).
  • the nozzle rings preferably contain between 5 and 500 nozzles having an opening of 0.01 to 5 mm.
  • the nozzles can also additionally be actuated with a temporal delay and an adjustable opening time.
  • the times as described in the first embodiment are likewise preferred here. 10 to 100 nozzles having an opening of 0.01 to 5 mm are preferred. An opening of 0.5 to 2 mm is preferably used. 50 nozzles having an exit diameter of 1 mm are particularly preferred.
  • the improvement in the flow conditions between the contact points of the individual fragments is produced by a so-called “principle of the rotating acid” ( FIG. 3 ).
  • a plurality of nozzles ( 6 ) having an opening of 0.01 to 5 mm are arranged at the base of the etching tank ( 1 ) in such a way that the acid mixture is cause to effect a rotational movement.
  • the etching mixture emerges from the nozzles at a velocity of greater than 100 mm/sec. Preference is given to nozzles having an opening of 0.5 mm to 4 mm, particularly preferably of 1 mm, and an exit velocity of 100 mm/sec.
  • the process basin ( 3 ) can rest in the rotating acid ( 7 ) or be moved by means of an additional lifting/lowering movement. Preference is given to an additional lifting/lowering movement in the case of which the process basin completely enters and exits from the liquid during each lifting/lowering movement.
  • the improvement in the flow conditions between the contact points of the individual fragments is produced by the application of a turntable which rotates in a horizontal plane and on which the process basin is situated ( FIG. 4 ).
  • the rotational movement of the process basin ( 3 ) on the turntable ( 8 ) is preferably between 1 and 500 revolutions per minute.
  • a sufficient incident flow on the polysilicon fragments from different directions is thus produced in the etching tank ( 1 ).
  • a rotational speed of 20 to 100 revolutions per minute is particularly preferred, especially preferably 50 revolutions per minute.
  • the setting of the suitable rotational speed of the horizontal rotatary movement produces an incident flow from different directions onto the surface of the individual silicon fragments at a velocity of greater than 100 mm/sec.
  • the improvement in the flow conditions between the contact points of the individual fragments can also be achieved by additional, non-directional injection of air through the base of the basin ( FIG. 5 ).
  • This measure results in an increase in the flow velocity at the critical contact points of greater than 100 mm/sec.
  • 5 to 100 nozzles ( 9 ) are fitted to the base of the etching tank ( 1 ), from which nozzles the air is injected into the etching tank from below in the direction of the process basin ( 3 ) with the polysilicon fragments ( 9 ).
  • the size of the opening of the nozzle outlets is preferably 0.01 to 5 mm.
  • the pressure of the injected air is preferably between 0.1 and 200 bar. 20 to 100 nozzles having an opening of 0.1 to 1 mm nozzle opening are particularly preferred.
  • the nozzles can additionally also be actuated with a temporal delay and an adjustable opening time. Preference is given to the temporal delays and the opening times analogously to the embodiments already described. As a result of the additional turbulence produced by the injected air into the purifying solution, the acid can flow through unimpeded at all the contact points between the poly fragments.
  • the improvement in the flow conditions between the contact points of the individual fragments is produced by a process basin that moves on a vertical axis ( FIG. 6 ).
  • the process basin ( 3 ) used is equipped with lateral holes ( 10 ) and is led through the etching bath on a vertical circular path.
  • a circular movement with a frequency of 1 to 200 revolutions per minute is preferred, and a rotational speed of 5 to 50 revolutions per minute is particularly preferred, especially preferably 10 revolutions per minute.
  • the circular movement can be carried out within the purifying liquid or else partially outside the purifying liquid. If a circular movement is performed in the course of which dipping into and out of the liquid takes place, the process basin can in this case be moved wholly or partly out of the liquid.
  • the improvement in the flow conditions between the contact points of the individual fragments is produced by applying ultrasound.
  • ultrasound having an operating frequency range of 10 kHz to 5 GHz the attack on silicon in the HF/HN03 etchant is surprisingly considerably increased.
  • An operating frequency of 500 kHz to 2 GHz is preferred.
  • An operating frequency of 1 GHz is particularly preferred.
  • the ultrasound has a positive effect on the etching process and on the dissolution of the metal particles. The metal surface values can be significantly reduced and it was thus possible to obtain the same effect as at flow velocities of greater than 100 mm/sec.
  • Purifying solution used 5% by weight HF, 55% by weight HNO 3 and 8% by weight H 2 SiF 6 ; temperature in the etching bath 20° C.
  • Purifying solution used 5% by weight HF, 55% by weight HNO 3 and 8% by weight H 2 SiF 6 ; temperature in the etching bath 20° C.
  • the table shows that with a lifting/lowering apparatus, at a flow of greater than 50 mm/sec onto the polysilicon surface, the etching removal no longer appreciably increases.
  • a lifting/lowering apparatus With a lifting/lowering apparatus, flow velocities up to a maximum 100 mm/sec are possible on an industrial scale for production installations with a tenable financial outlay. At flow velocities up to 100 mm/sec, however, gray spots are obtained as a result of the excessively small substance exchange in the dead water zones.
  • the purified poly fragments contained the following analysis values from ion chromatography or CE measurements: fluoride 2 pptw, nitrate 5 pptw, nitrite 0.1 pptw and chloride 3 pptw.
  • a polysilicon rod was comminuted and classified by means of a device comprising a comminuting tool and a screening device. 5 kg of poly fragments were treated in a process basin using the following 3-stage purifying process analogously to EP 0 905 796.
  • the polysilicon fragments were purified for 20 minutes in a mixture comprising HF/HCl/H 2 O 2 at a temperature of 25° C.
  • the polysilicon fragments were etched for 5 minutes at 8° C. in a mixture of HF/HNO 3 . This was followed by rinsing for 5 minutes in ultrapure water with 18 megohms at a temperature of 22° C.
  • hydrophilization was effected for 5 minutes in a mixture comprising HCl/H 2 O 2 at a temperature of 22° C. and drying was effected for 60 minutes using ultrapure air of class 100 at 80° C.
  • the basket containing a weighed-in quantity of 5 kg carried out an up and down movement with the poly fragments with a stroke frequency of 5 strokes per minute.
  • the main purifying took place in an etching bath with 500 l of acid, in which 50 nozzles were situated.
  • the HF/HNO 3 etching mixture emerged from the nozzles at a velocity of 150 mm/sec.
  • the nozzles were opened in temporally staggered fashion in an alternating cycle with a temporal delay of 2 sec for a time of 0.5 sec.
  • the nozzles had an opening of 1 mm.
  • the alternate incident flow on the individual fragments prevented dead water zones from arising at the contact points between the poly fragments. A uniform flow velocity prevails at all points in the bulk material. After the hydrophilization and drying, poly fragments without spots on their lustrous surfaces were obtained.
  • the process basin in a 500 liter HF/HNO 3 etching mixture in the acid tank was moved with a lifting/lowering movement at a frequency of 5 strokes per minute.
  • Four nozzles having an exit opening of 1 mm were fitted at the base of the tank.
  • the acid emerged from said nozzles at a velocity of 150 mm/sec.
  • the basin continually completely emerged from the acid and entered it again.
  • the acid had a temperature of 8° C.
  • a uniform throughflow was achieved at all points in the bulk material. This made it possible to prevent dead water zones at the contact points between the poly fragments.
  • the process basin in a 500 liter HF/HNO 3 etching mixture in the acid tank was moved with a lifting/lowering movement at a frequency of 5 strokes per minute.
  • 50 nozzles having an opening of 0.1 mm were additionally fitted at the base of the tank. Through these nozzles, air was additionally injected through the base of the basin. This made it possible to achieve an increase in the flow velocity at the contact points.
  • the flow velocity was 150 mm/sec.
  • the nozzles were opened with a temporal delay of 2 sec for 0.5 sec. As a result of the additional turbulence produced by the injected air, the acid can flow through unimpeded at all contact points between the poly fragments.
  • the process basin in a 500 liter HF/HNO 3 etching mixture was moved with a vertical circular movement through the acid tank.
  • the frequency of the circular movement was 10 revolutions per minute.
  • the acid flows onto the poly surfaces at a velocity of 150 mm/sec from all directions.
  • the bath temperature was 8° C. and there was continuous circulation.
  • the time in the etching bath was 5 minutes.
  • the basin was completely immersed in the liquid and completely removed therefrom in each cycle. The circular movement results in uniform flow through the bulk material which prevents dead water zones from arising at the contact points of the poly fragments. After the hydrophilization and drying, poly fragments without spots on their lustrous surfaces were obtained.
  • a polysilicon rod was comminuted and classified by means of a device comprising a comminuting tool and a screening device. 5 kg of poly fragments were treated in a process basin using the following 3-stage purifying process analogously to EP 0 905 796.
  • the polysilicon fragments were purified for 20 minutes in a mixture comprising HF/HCl/H 2 O 2 at a temperature of 25° C.
  • the polysilicon fragments were etched for 5 minutes at 8° C. in a mixture of HF/HNO 3 . This was followed by rinsing for 5 minutes in ultrapure water with 18 megohms at a temperature of 22° C.
  • hydrophilization was effected for 5 minutes in a mixture comprising HCl/H 2 O 2 at a temperature of 22° C. and drying was effected for 60 minutes using ultrapure air of class 100 at 80° C.
  • the basket filled with 5 kg of poly fragments carried out an up and down movement with a stroke frequency of 5 strokes per minute.
  • An ultrasonic generator having an operating frequency of 1 GHZ was additionally incorporated in all purifying and rinsing steps.
  • Poly fragments with fewer particles in comparison with a process without an ultrasound bath and with a lower metal level on the poly surface were obtained after the end of the process.
  • the purified polysilicon fragments had no spots on their lustrous surfaces.
  • a polysilicon rod was comminuted and classified by means of a device comprising a comminuting tool and a screening device. 5 kg of poly fragments were treated in a process basin by means of the following purifying process.
  • the polysilicon fragments were purified for 20 minutes in a mixture comprising 5% by weight HF, 8% by weight HCl and 3% by weight H 2 O 2 at a temperature of 25° C.
  • the removal of the polysilicon surface was 0.02 p in this case.
  • rinsing was effected for 5 minutes at 3 m 3 /hr in an ultrasound bath with plastic lining at 3 GHZ at 22° C.
  • main purifying the polysilicon fragments were etched for 5 minutes at 8° C. in a mixture of HF/HNO 3 comprising 3% by weight HF, 65% by weight HNO 3 .
  • the etching removal was approximately 12 ⁇ m.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)
  • Cleaning By Liquid Or Steam (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
US12/675,297 2007-08-29 2008-08-08 Method for purifying polycrystalline silicon Abandoned US20100300495A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102007040851.1 2007-08-29
DE102007040851A DE102007040851A1 (de) 2007-08-29 2007-08-29 Verfahren zum Reinigen von polykristallinem Silicium
PCT/EP2008/060425 WO2009027200A2 (fr) 2007-08-29 2008-08-08 Procédé de purification de silicium cristallin

Related Parent Applications (1)

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PCT/EP2008/060425 A-371-Of-International WO2009027200A2 (fr) 2007-08-29 2008-08-08 Procédé de purification de silicium cristallin

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US14/535,975 Continuation US9421584B2 (en) 2007-08-29 2014-11-07 Method for purifying polycrystalline silicon

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US14/535,975 Expired - Fee Related US9421584B2 (en) 2007-08-29 2014-11-07 Method for purifying polycrystalline silicon

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US (2) US20100300495A1 (fr)
EP (1) EP2181068B1 (fr)
JP (1) JP5738592B2 (fr)
KR (1) KR101167597B1 (fr)
CN (1) CN101790493B (fr)
AT (1) ATE503723T1 (fr)
CA (1) CA2694012C (fr)
DE (2) DE102007040851A1 (fr)
WO (1) WO2009027200A2 (fr)

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US20150101642A1 (en) * 2013-10-11 2015-04-16 Cfa Properties, Inc. Produce washing system and methods
CN109158373A (zh) * 2018-11-09 2019-01-08 江苏德润光电科技有限公司 一种多晶硅片智能化清洗装置

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CN102344144A (zh) * 2011-09-30 2012-02-08 巨锋 一种废晶体硅的自动酸碱清洗反应设备
JP6184906B2 (ja) * 2014-06-20 2017-08-23 信越化学工業株式会社 多結晶シリコン塊の洗浄方法
US10345211B2 (en) * 2016-03-28 2019-07-09 Hemlock Semiconductor Operations Llc Method of determining a concentration of a material not dissolved by silicon etchants contaminating a product
EP3778480A4 (fr) * 2018-03-27 2022-01-05 Tokuyama Corporation Procédé de lavage, procédé de fabrication et dispositif de lavage pour silicium polycristallin
CN113357913B (zh) * 2021-06-29 2022-12-09 吉利硅谷(谷城)科技有限公司 一种用于多晶硅提纯的电磁加热炉

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CN109158373A (zh) * 2018-11-09 2019-01-08 江苏德润光电科技有限公司 一种多晶硅片智能化清洗装置

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CA2694012C (fr) 2012-03-06
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JP5738592B2 (ja) 2015-06-24
CA2694012A1 (fr) 2009-03-05
DE502008003032D1 (de) 2011-05-12
US20150075559A1 (en) 2015-03-19
US9421584B2 (en) 2016-08-23
KR20100049092A (ko) 2010-05-11
CN101790493A (zh) 2010-07-28
WO2009027200A2 (fr) 2009-03-05
EP2181068A2 (fr) 2010-05-05
WO2009027200A3 (fr) 2009-06-04
EP2181068B1 (fr) 2011-03-30
CN101790493B (zh) 2013-03-06
ATE503723T1 (de) 2011-04-15
JP2010536570A (ja) 2010-12-02

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