WO2012004968A1 - 多結晶シリコン棒および多結晶シリコン棒の製造方法 - Google Patents

多結晶シリコン棒および多結晶シリコン棒の製造方法 Download PDF

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WO2012004968A1
WO2012004968A1 PCT/JP2011/003800 JP2011003800W WO2012004968A1 WO 2012004968 A1 WO2012004968 A1 WO 2012004968A1 JP 2011003800 W JP2011003800 W JP 2011003800W WO 2012004968 A1 WO2012004968 A1 WO 2012004968A1
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polycrystalline silicon
silicon rod
frequency
peak frequency
rod
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English (en)
French (fr)
Japanese (ja)
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祢津　茂義
史高 久米
岡田　淳一
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Shin Etsu Chemical Co Ltd
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Shin Etsu Chemical Co Ltd
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Priority to AU2011275287A priority Critical patent/AU2011275287B2/en
Priority to CN201180033481.0A priority patent/CN102971624B/zh
Priority to EP11803307.5A priority patent/EP2594933A4/en
Priority to US13/808,404 priority patent/US9006002B2/en
Publication of WO2012004968A1 publication Critical patent/WO2012004968A1/ja
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P74/00—Testing or measuring during manufacture or treatment of wafers, substrates or devices
    • H10P74/20—Testing or measuring during manufacture or treatment of wafers, substrates or devices characterised by the properties tested or measured, e.g. structural or electrical properties
    • H10P74/203—Structural properties, e.g. testing or measuring thicknesses, line widths, warpage, bond strengths or physical defects
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M7/00—Vibration-testing of structures; Shock-testing of structures
    • G01M7/08—Shock-testing
    • 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
    • G01N29/045—Analysing solids by imparting shocks to the workpiece and detecting the vibrations or the acoustic waves caused by the shocks
    • 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
    • G01N29/12—Analysing solids by measuring frequency or resonance of acoustic waves
    • 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
    • G01N29/44—Processing the detected response signal, e.g. electronic circuits specially adapted therefor
    • G01N29/4409—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison
    • G01N29/4418—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison with a model, e.g. best-fit, regression analysis
    • 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
    • G01N29/44—Processing the detected response signal, e.g. electronic circuits specially adapted therefor
    • G01N29/4454—Signal recognition, e.g. specific values or portions, signal events, signatures
    • 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
    • G01N29/44—Processing the detected response signal, e.g. electronic circuits specially adapted therefor
    • G01N29/46—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by spectral analysis, e.g. Fourier analysis or wavelet analysis
    • 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
    • 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
    • G01N2291/26—Scanned objects
    • G01N2291/262—Linear objects
    • G01N2291/2626—Wires, bars, rods
    • 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
    • G01N2291/26—Scanned objects
    • G01N2291/269—Various geometry objects
    • G01N2291/2697—Wafer or (micro)electronic parts
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W72/00—Interconnections or connectors in packages
    • H10W72/071—Connecting or disconnecting
    • H10W72/072—Connecting or disconnecting of bump connectors
    • H10W72/07251—Connecting or disconnecting of bump connectors characterised by changes in properties of the bump connectors during connecting
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W72/00—Interconnections or connectors in packages
    • H10W72/20—Bump connectors, e.g. solder bumps or copper pillars; Dummy bumps; Thermal bumps

Definitions

  • the present invention relates to a polycrystalline silicon rod and a method of manufacturing a polycrystalline silicon rod, and more particularly to a technique for easily sorting hard polycrystalline silicon rods.
  • the Siemens method is known as a manufacturing method of the polycrystalline silicon used as the raw material of the single crystal silicon for semiconductor device manufacture, or the silicon for solar cell manufacture.
  • the Siemens method is a method of vapor phase growing polycrystalline silicon on the surface of a silicon core wire by using a CVD (Chemical Vapor Deposition) method by bringing a source gas containing chlorosilane into contact with a heated silicon core wire.
  • CVD Chemical Vapor Deposition
  • two silicon core wires are assembled in a vertical direction and one horizontal direction torii type in a reaction furnace of a vapor phase growth apparatus, and both ends of the torii type silicon core wire are paired It fixes to a pair of metal electrodes arrange
  • a source gas such as a mixed gas of trichlorosilane and hydrogen is introduced into the reactor from a gas nozzle.
  • silicon crystal-grows on the silicon core, and polycrystalline silicon having a desired diameter is formed in an inverted U shape.
  • both ends of the above-mentioned inverted U-shaped polycrystalline silicon are cut to obtain multiple pieces of desired length. It is adjusted to a crystalline silicon rod (cutting step), the outer periphery of this polycrystalline silicon rod is polished to make the diameter uniform in the longitudinal direction (cylindrical polishing step), and one end of this polycrystalline silicon rod is processed to sharpen it Finally, the surface of the polycrystalline silicon rod is etched to remove impurities and strains (etching step).
  • Such polycrystalline silicon rods are likely to have cracks formed inside and outside in the vapor phase growth process or the cooling process after growth along with the recent increase in diameter.
  • a crack is formed on the inside and the outside of the polycrystalline silicon rod, it may be broken in the cutting step, the cylindrical polishing step, the tip processing step, or the etching step described above.
  • the polycrystalline silicon rod may be broken during the growth process of the single crystal silicon ingot by the FZ method. If the polycrystalline silicon rod is broken during these processes, not only the previous process work is wasted, but also the equipment used in the process may be damaged.
  • the additional charge is to melt the silicon block filled in the crucible and then gradually dissolve the polycrystalline silicon rod suspended on the crucible into the melt to increase the amount of melt in the crucible.
  • Recharge means that after pulling up the CZ crystal, the polycrystalline silicon rod suspended on the crucible is gradually dissolved in the residual solution to increase the amount of melt in the crucible.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2001-21543
  • a polycrystalline silicon block is placed in water or other liquid, and a sound wave of 0.5 to 10 MHz is emitted while scanning the probe above it.
  • a flaw detection method for displaying an abnormal part immediately below a probe in a second order plane is used.
  • JP 2007-218638 A compares the image data of infrared ray transmitted light of a polycrystalline silicon wafer with the image data of infrared ray reflected light, and the difference of brightness or luminance corresponding to the same position.
  • a crack inspection method is disclosed which takes each pixel and determines whether there is a crack inside or outside.
  • the present invention has been made to solve such conventional polycrystalline silicon cracks, and the object of the present invention is to eliminate the need for a large-scale device and to be hard and difficult to break with high accuracy.
  • An object of the present invention is to provide a method for sorting polycrystalline silicon rods, and thus to provide high quality polycrystalline silicon rods.
  • polycrystalline silicon is grown by a vapor phase method, and the polycrystalline silicon is used as a polycrystalline silicon rod having a length of L (m).
  • the frequency analysis of the impact sound obtained by striking the polycrystalline silicon rod is performed to obtain the peak frequency f (Hz) of the impact sound, and the polycrystalline silicon rod satisfying f ⁇ 1471 / L is selected. It is characterized by
  • the upper limit value of the peak frequency f may be f ⁇ 1471 / L + 1000 as a selection criterion of the polycrystalline silicon rod.
  • the ratio R (f 0 / f) of the natural frequency f 0 to the peak frequency f obtained from the waveform of the striking sound is 0.9 ⁇ R ⁇ 1.1. You may do it.
  • the polycrystalline silicon rod of the present invention is a polycrystalline silicon rod having a length of L (m), and the striking sound of the polycrystalline silicon rod has a peak frequency f (Hz) obtained by frequency analysis of f It is characterized by satisfying ⁇ 1471 / L.
  • the peak frequency f may satisfy f ⁇ 1471 / L + 1000.
  • the ratio R (f 0 / f) of the natural frequency f 0 to the peak frequency f determined from the waveform of the striking sound of the polycrystalline silicon rod may be 0.9 ⁇ R ⁇ 1.1. .
  • the polycrystalline silicon rod is obtained, for example, by vapor phase growth by the Siemens method.
  • the present invention includes, for example, a hammer for striking a polycrystalline silicon rod, a voice recorder for recording striking sound, a software and PC (personal computer) used for frequency analysis, and a tape measure for measuring the length of a polycrystalline silicon rod.
  • a hammer for striking a polycrystalline silicon rod for example, a voice recorder for recording striking sound, a software and PC (personal computer) used for frequency analysis, and a tape measure for measuring the length of a polycrystalline silicon rod.
  • a software and PC personal computer
  • FIG. 1 is a schematic view for explaining one aspect of the method for sorting polycrystalline silicon rods of the present invention.
  • reference numeral 100 is a polycrystalline silicon rod to be sorted, and the polycrystalline silicon rod 100 exemplified here is obtained by vapor phase growth by the above-mentioned Siemens method, and has a diameter of about 110 mm, The length is about 1600 mm.
  • Reference numeral 110 denotes a roller for mounting the polycrystalline silicon rod 100
  • reference numeral 120 denotes a hammer for striking the polycrystalline silicon rod 100
  • reference numeral 130 denotes sound from the polycrystalline silicon rod 100 generated by striking with the hammer 120.
  • a microphone for picking up, and a code 140 is a recorder for recording the striking sound picked up by the microphone 130.
  • the polycrystalline silicon rod 100 is struck with a hammer 120, and the frequency of the impact sound generated thereby is analyzed to determine the hardness of the polycrystalline silicon rod 100. For this reason, in order to obtain the original hitting sound of the polycrystalline silicon rod 100, it is desirable that the polycrystalline silicon rod 100 is not in contact with other members as much as possible. That is, in order to perform accurate frequency analysis, it is desirable to hold the polycrystalline silicon rod 100 in a state in which the contact area with other members is as narrow as possible. Therefore, in the example shown in FIG. 1, the polycrystalline silicon rod 100 is placed on the two rollers 110.
  • the hammer 120 used to hit the polycrystalline silicon rod 100 is preferably made of a material that hardly causes heavy metal contamination on the polycrystalline silicon rod 100 at the time of impact.
  • a plastic hammer or a tungsten hammer it is desirable to use a plastic hammer or a tungsten hammer.
  • the impact sound from the polycrystalline silicon rod 100 is picked up by the microphone 130 and recorded in the recorder 140.
  • a digital voice recorder for example, is used as the recorder 140, an acoustic signal is converted from analog to digital and recorded.
  • FIG. 2 is a flow chart for explaining the procedure for frequency analysis of the impact sound from the polycrystalline silicon rod in the present invention.
  • the length of the polycrystalline silicon rod 100 is measured with a tape measure (S101).
  • the polycrystalline silicon rod 100 is struck using the hammer 120 (S102), and the impact sound is recorded on the recorder 140 via the microphone 130 (S103).
  • S104 by analyzing the impact sound to calculate the natural frequency f 0 (S104), further, a fast Fourier transform acoustic signals of impact sound (Fast Fourier Transform: FFT) to display the frequency distribution (S105).
  • FFT fast Fourier transform acoustic signals of impact sound
  • FIGS. 3A and 3B respectively show an example of an acoustic signal of a striking sound and an example of a frequency distribution obtained by subjecting the acoustic signal to fast Fourier transform.
  • free software for performing fast Fourier transform on the acoustic signal converted into digital is available on the Internet.
  • the waveform of the striking sound produced when hitting the crack free part of polycrystalline silicon rod 100 with hammer 120 is close to a sine wave, and one or two frequencies showing large loudness observed in the frequency distribution after fast Fourier transform is there.
  • the hammering sound may be obtained as if hitting a plurality of polycrystalline silicon rods with slightly different lengths at once. Will occur. Specifically, a large number of sound waves having slightly different frequencies are formed, and the waveform of the striking sound is a whirlpool having many peaks and valleys in one cycle. For this reason, the period of the waveform becomes long, the frequency becomes low, and the hitting sound can be heard low.
  • the acoustic signal of such a striking sound is subjected to fast Fourier transformation, a frequency distribution in which a large number of frequencies have a relatively large volume is obtained.
  • the peak frequency f showing the largest volume is detected in the frequency distribution after the fast Fourier transform (S106).
  • the peak frequency f is a main frequency that forms the striking sound. If the waveform of the striking sound is formed by a single sine wave, the peak frequency f and the natural frequency f 0 completely match. On the other hand, when a large number of sound waves overlap to form the waveform of the striking sound, the peak frequency f and the natural frequency f 0 are shifted.
  • the natural frequency f 0 is the peak frequency f because the waveform of the striking sound is such that the period of the sine wave is slightly longer. Slightly smaller.
  • the frequency of the beat becomes the peak frequency f.
  • the natural frequency f 0 is larger than the peak frequency f because the period of the beat is longer than the period of the striking sound.
  • the natural frequency f 0 and the peak frequency f were measured for a total of 31 polycrystalline silicon rods, and the relationship with the cracks was investigated. There were 21 polycrystalline silicon rods without cracks. Further, the value (R) obtained by dividing the natural frequency f 0 by the peak frequency f for each of these polycrystalline silicon rods was 0 or more and 2 or less.
  • the R value range is limited to 0.9 or more and 1.1 or less, there are 19 crack-free polycrystalline silicon rods in this R value range, and it is only two less than the total number (21). is there. That is, it can be seen that most of polycrystalline silicon rods without cracks have an R value in the range of 0.9 or more and 1.1 or less. On the other hand, the number of cracked polycrystalline silicon rods in the R value range of 0.9 or more and 1.1 or less is only one, and most of polycrystalline silicon rods with cracks have an R value of 0. Either less than 9 or greater than 1.1.
  • FIG. 4 is a diagram showing the result of finding the relationship between the R value and the peak frequency f for a population of polycrystalline silicon rods other than those summarized in Table 1. Black circles indicate the values of polycrystalline silicon rods without cracks, and white circles indicate the values of polycrystalline silicon rods with cracks.
  • FIG. 5 is a graph showing the relationship between the length (L) and the peak frequency for polycrystalline silicon rods having an R value of 0.9 or more and 1.1 or less.
  • the horizontal axis is the reciprocal (unit m ⁇ 1 ) of the length (L) of the polycrystalline silicon rod, and the vertical axis is the peak frequency (f: unit Hz).
  • the peak frequency of the polycrystalline silicon rod belonging to the A region is f ⁇ 1471 / L.
  • the peak frequency of the polycrystalline silicon rod belonging to the A region is in the range of f ⁇ 1471 / L + 1000.
  • the peak frequency of the polycrystalline silicon rod belonging to the B region is lower than the peak frequency of the polycrystalline silicon rod belonging to the A region, and the polycrystalline silicon rod belonging to the B region is struck with a hammer And can be split relatively easily.
  • the polycrystalline silicon rod belonging to the A region is hard and does not break easily even if struck with a hammer. That is, by performing frequency analysis of the impact sound and knowing which of the A region and the B region the peak frequency f belongs to, it can be determined whether the polycrystalline silicon rod is hard and hard to break.
  • the peak frequency with respect to the length of the polycrystalline silicon rod is confirmed based on the principle as described above (S108), and the hardness of the polycrystalline silicon rod and hence the resistance to cracking are judged (S109).
  • FIG. 6 is a flow chart showing an example of steps for selecting hard polycrystalline silicon rods.
  • FIG. 7 is a schematic view showing a configuration example of an apparatus used to manufacture polycrystalline silicon.
  • the polycrystalline silicon manufacturing apparatus 50 is an apparatus for vapor phase growing polycrystalline silicon on the surface of a silicon core wire by the Siemens method, and is roughly configured by the base plate 1 and the reaction vessel 10 and obtained.
  • the polycrystalline silicon 100 is composed of a straight body portion 100a which is vapor grown on the vertical portion 5a of the silicon core wire 5 assembled in a torii type, and a bridge portion 100b which is vapor grown on the horizontal portion (bridge portion 5b).
  • the base plate 1 is provided with a metal electrode 2 for supplying an electric current to the silicon core wire 5, a gas nozzle 3 for supplying a process gas such as nitrogen gas, hydrogen gas or trichlorosilane gas, and an exhaust port 4 for discharging exhaust gas.
  • a metal electrode 2 for supplying an electric current to the silicon core wire 5
  • a gas nozzle 3 for supplying a process gas such as nitrogen gas, hydrogen gas or trichlorosilane gas
  • an exhaust port 4 for discharging exhaust gas.
  • the metal electrode 2 is connected to another metal electrode (not shown) or to a power source disposed outside the reactor, and receives an external power supply.
  • An insulator 7 is provided on the side surface of the metal electrode 2 and penetrates the base plate 1 in a state of being sandwiched by the insulator 7.
  • core wires of two (5a) in the vertical direction and one (5b) in the horizontal direction are formed in a toriiary manner in the reaction furnace 10.
  • the silicon core wire 5 is assembled, and both ends of the vertical direction portion 5a of the silicon core wire 5 are fixed by the core wire holder 20 respectively held by the carbon electrode 30, and the external power supplied to the metal electrode 2 is through the carbon electrode 30.
  • the silicon core wire 5 is energized.
  • the metal electrode 2, the base plate 1 and the reaction furnace 10 are cooled using a refrigerant. Further, both the core holder 20 and the carbon electrode 30 are made of graphite.
  • reverse U-shaped polycrystalline silicon is vapor-phase grown by the Siemens method (S201).
  • the inverted U-shaped polycrystalline silicon is taken out from the reaction furnace 10 and divided into a straight body portion 100a and a bridge portion 100b. However, since cracks often remain at both ends of the polycrystalline silicon rod 100, both ends of the polycrystalline silicon rod 100 are cut (S202).
  • the polycrystalline silicon rod 100 is placed on the roller 110 and struck with a hammer 120, and an impact sound is recorded through the microphone 130. Then, the frequency analysis of the above-mentioned impulsive sound is performed in the same manner as described with reference to FIG. 2, and a value obtained by dividing the natural frequency f 0 by the peak frequency f (S203).
  • the entire polycrystalline silicon rod 100 may be struck with a hammer 120, and only a tapping sound in a relatively low sound area may be recorded and subjected to frequency analysis.
  • a value obtained by dividing the natural frequency f 0 by the peak frequency f is less than 0.9 or more than 1.1, it is considered that a crack is present inside and outside, so the area is cut and removed (S 204 ). In this case, after the cracked area is cut and removed, frequency analysis is performed again (S205). Also, if necessary, repeat steps S204 and S205 multiple times and finally confirm that the value obtained by dividing the natural frequency f 0 by the peak frequency f is 0.9 or more and 1.1 or less in all regions. (S206).
  • the length L of the polycrystalline silicon rod 100 is measured with a tape measure or the like, and with respect to the reciprocal 1 / L of the length L of the polycrystalline silicon rod 100, whether the above peak frequency belongs to the above-mentioned A region or B region It is checked whether it belongs to (S207).
  • the polycrystalline silicon rod 100 belonging to the A region is harder and less likely to break than the one belonging to the B region. That is, by sorting the polycrystalline silicon rods belonging to the A region from the polycrystalline silicon rods belonging to the B region, it is possible to obtain a polycrystalline silicon rod hard and hard to break (S208).
  • Example 1 Both ends of polycrystalline silicon obtained by vapor deposition according to the Siemens method were cut into polycrystalline silicon rods 100 having a length of 1.2 m and a diameter of 121 mm.
  • the polycrystalline silicon rod 100 was struck with a tungsten carbide hammer 120 and the impact sound was recorded on a digital voice recorder 140 attached with a microphone 130.
  • the natural frequency of the recorded impact sound was 1563 Hz.
  • the peak frequency was 1636.5 Hz.
  • a value obtained by dividing the natural frequency by the peak frequency is 0.96.
  • the above-mentioned peak frequency (1636.5 Hz) is higher than this boundary peak frequency. Therefore, the polycrystalline silicon rod 100 was selected as belonging to the A region.
  • Comparative Example 1 The natural frequency and peak frequency of a polycrystalline silicon rod having a length of 1.5 m and a diameter of 122 mm obtained by the Siemens method were measured in the same manner as in Example 1 described above. As a result, the natural frequency was 147 Hz, the peak frequency was 75.4 Hz, and the value obtained by dividing the natural frequency by the peak frequency was 1.96.
  • the above mentioned peak frequency (75.4 Hz) is much lower than this boundary peak frequency. Therefore, this polycrystalline silicon rod was classified as belonging to the B region.
  • the present invention it is possible to easily detect the hardness of the polycrystalline silicon rod, and hence the hardness of the crack, and based on this method, it is possible to sort out the polycrystalline silicon rod which is hard to be cracked to obtain high quality. It is possible to manufacture various polycrystalline silicon rods.

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PCT/JP2011/003800 2010-07-06 2011-07-04 多結晶シリコン棒および多結晶シリコン棒の製造方法 Ceased WO2012004968A1 (ja)

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AU2011275287A AU2011275287B2 (en) 2010-07-06 2011-07-04 Polycrystalline silicon rod and production method for polycrystalline silicon rod
CN201180033481.0A CN102971624B (zh) 2010-07-06 2011-07-04 多晶硅棒以及多晶硅棒的制造方法
EP11803307.5A EP2594933A4 (en) 2010-07-06 2011-07-04 Polycrystalline silicon rod and production method for polycrystalline silicon rod
US13/808,404 US9006002B2 (en) 2010-07-06 2011-07-04 Polycrystalline silicon rod and method for manufacturing polycrystalline silicon rod

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JP2010153828A JP5238762B2 (ja) 2010-07-06 2010-07-06 多結晶シリコン棒および多結晶シリコン棒の製造方法

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WO2014024388A1 (ja) * 2012-08-10 2014-02-13 信越化学工業株式会社 多結晶シリコン棒の選択方法、多結晶シリコン塊の製造方法、及び、単結晶シリコンの製造方法
CN108225955A (zh) * 2017-12-30 2018-06-29 洛阳阿特斯光伏科技有限公司 一种硅棒的硬度评估方法

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* Cited by examiner, † Cited by third party
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JP5828795B2 (ja) 2012-04-04 2015-12-09 信越化学工業株式会社 多結晶シリコンの結晶配向度評価方法、多結晶シリコン棒の選択方法、および単結晶シリコンの製造方法
JP2014001096A (ja) 2012-06-18 2014-01-09 Shin Etsu Chem Co Ltd 多結晶シリコンの結晶配向度評価方法、多結晶シリコン棒の選択方法、多結晶シリコン棒、多結晶シリコン塊、および、単結晶シリコンの製造方法
DE102013207251A1 (de) * 2013-04-22 2014-10-23 Wacker Chemie Ag Verfahren zur Herstellung von polykristallinem Silicium
JP6181620B2 (ja) 2014-09-04 2017-08-16 信越化学工業株式会社 多結晶シリコン製造用反応炉、多結晶シリコン製造装置、多結晶シリコンの製造方法、及び、多結晶シリコン棒または多結晶シリコン塊
CN108168868A (zh) * 2017-12-29 2018-06-15 绍兴文理学院 一种检测型钢构件自振频率的方法
CN108732307A (zh) * 2018-05-04 2018-11-02 扬州连城金晖金刚线切片研发有限公司 一种金刚线切片的单、多晶硅棒检验方法
US11655541B2 (en) 2018-12-17 2023-05-23 Wacker Chemie Ag Process for producing polycrystalline silicon

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001021543A (ja) 1999-07-06 2001-01-26 Sumitomo Sitix Of Amagasaki Inc シリコン塊の探傷方法
JP2001294416A (ja) * 2000-04-07 2001-10-23 Mitsubishi Materials Polycrystalline Silicon Corp 多結晶シリコンの製造装置
JP2004149324A (ja) * 2002-10-28 2004-05-27 Sumitomo Mitsubishi Silicon Corp 多結晶シリコンロッド及びその製造方法、並びにそのロッドの製造に使用されるシリコン芯材
JP2007218638A (ja) 2006-02-14 2007-08-30 Sharp Corp 多結晶半導体ウエハの割れ検査装置および割れ検査方法
JP2008058314A (ja) * 2006-08-30 2008-03-13 Wacker Chemie Ag ポリシリコン成形体の汚染および破壊のない試験法および欠陥のないポリシリコン成形体

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4062229A (en) * 1977-02-22 1977-12-13 General Electric Company Method of testing the integrity of installed rock bolts
JP2001235451A (ja) * 2000-02-25 2001-08-31 Mitsubishi Electric Corp 試料の欠陥測定装置及び方法
JP4768927B2 (ja) 2001-05-11 2011-09-07 新日本製鐵株式会社 打音検査物の非破壊検査方法、及び品質管理方法
US6941811B2 (en) * 2003-08-04 2005-09-13 Nan Ya Technology Corporation Method and apparatus for detecting wafer flaw

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001021543A (ja) 1999-07-06 2001-01-26 Sumitomo Sitix Of Amagasaki Inc シリコン塊の探傷方法
JP2001294416A (ja) * 2000-04-07 2001-10-23 Mitsubishi Materials Polycrystalline Silicon Corp 多結晶シリコンの製造装置
JP2004149324A (ja) * 2002-10-28 2004-05-27 Sumitomo Mitsubishi Silicon Corp 多結晶シリコンロッド及びその製造方法、並びにそのロッドの製造に使用されるシリコン芯材
JP2007218638A (ja) 2006-02-14 2007-08-30 Sharp Corp 多結晶半導体ウエハの割れ検査装置および割れ検査方法
JP2008058314A (ja) * 2006-08-30 2008-03-13 Wacker Chemie Ag ポリシリコン成形体の汚染および破壊のない試験法および欠陥のないポリシリコン成形体

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2594933A4

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014024388A1 (ja) * 2012-08-10 2014-02-13 信越化学工業株式会社 多結晶シリコン棒の選択方法、多結晶シリコン塊の製造方法、及び、単結晶シリコンの製造方法
JP2014034506A (ja) * 2012-08-10 2014-02-24 Shin Etsu Chem Co Ltd 多結晶シリコン棒の選択方法、多結晶シリコン塊の製造方法、及び、単結晶シリコンの製造方法
CN108225955A (zh) * 2017-12-30 2018-06-29 洛阳阿特斯光伏科技有限公司 一种硅棒的硬度评估方法
CN108225955B (zh) * 2017-12-30 2024-01-12 洛阳阿特斯光伏科技有限公司 一种硅棒的硬度评估方法

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