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WO2017110967A1 - Dispositif de test de creuset, procédé de test de creuset, creuset en verre de silice, procédé de fabrication d'un creuset en verre de silice, procédé de fabrication d'un lingot de silicium et procédé de fabrication d'une tranche homoépitaxiale - Google Patents

Dispositif de test de creuset, procédé de test de creuset, creuset en verre de silice, procédé de fabrication d'un creuset en verre de silice, procédé de fabrication d'un lingot de silicium et procédé de fabrication d'une tranche homoépitaxiale Download PDF

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Publication number
WO2017110967A1
WO2017110967A1 PCT/JP2016/088285 JP2016088285W WO2017110967A1 WO 2017110967 A1 WO2017110967 A1 WO 2017110967A1 JP 2016088285 W JP2016088285 W JP 2016088285W WO 2017110967 A1 WO2017110967 A1 WO 2017110967A1
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WIPO (PCT)
Prior art keywords
crucible
silica glass
glass crucible
wave
single crystal
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.)
Ceased
Application number
PCT/JP2016/088285
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English (en)
Japanese (ja)
Inventor
俊明 須藤
忠広 佐藤
賢 北原
江梨子 北原
山崎　亨
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Sumco Corp
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Sumco Corp
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Publication date
Application filed by Sumco Corp filed Critical Sumco Corp
Priority to JP2017558244A priority Critical patent/JP6692526B2/ja
Publication of WO2017110967A1 publication Critical patent/WO2017110967A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon

Definitions

  • the present invention relates to a crucible inspection apparatus, a crucible inspection method, a silica glass crucible, a silica glass crucible manufacturing method, and a silicon ingot manufacturing method, and more particularly to a crucible inspection apparatus, a crucible inspection method, and a silica glass crucible for inspecting crucible fragility.
  • the present invention relates to a method for producing a silica glass crucible, a method for producing a silicon ingot, and a method for producing a homoepitaxial wafer.
  • a silicon single crystal (silicon ingot) is manufactured by the Czochralski method (CZochralski) using a silica glass crucible.
  • CZochralski Czochralski
  • first, polycrystalline silicon is filled into a silica glass crucible.
  • the polycrystalline silicon is melted into the silicon melt by heating with a carbon heater or the like disposed around the silica glass crucible.
  • a silicon single crystal seed crystal is brought into contact with the molten silicon melt and gradually pulled up while rotating.
  • the silicon single crystal is grown by using the seed crystal of the silicon single crystal as a nucleus.
  • the pulling of the silicon single crystal is performed at a temperature of about 1450 to 1500 ° C. This is a temperature exceeding 1200 to 1300 ° C. which is the softening point of the silica glass crucible.
  • a silica glass crucible used in manufacturing the silicon single crystal includes a cylindrical side wall, a curved bottom, and a corner having a higher curvature than the bottom by connecting the side and the bottom. It is a shape and the upper end surface of the side wall part of the silica glass crucible is formed as an annular flat surface. Further, the silica glass crucible includes, for example, a transparent layer in which bubbles cannot be observed based on visual observation or image data, and a bubble-containing layer in which bubbles are observed, from the inner surface to the outer surface of the silica glass crucible. It is comprised with the layer of. Silica glass crucibles are manufactured in various sizes such as 28 inches (about 71 cm), 32 inches (about 81 cm), 36 inches (about 91 cm), and 40 inches (about 101 cm) in diameter.
  • the pulling of the silicon single crystal is performed at a temperature exceeding the softening point of silica glass. Therefore, when the silicon single crystal is pulled, the silica glass crucible is deformed. Therefore, generally, a silica glass crucible is used for every pulling of a silicon single crystal. That is, the silica glass crucible needs to be prepared separately for each pulling of the silicon single crystal.
  • the silica glass crucible as described above is manufactured by using, for example, a rotational mold method. That is, the silica glass crucible is formed by depositing silica powder on the inner surface of a rotating mold (made of carbon) to form a silica powder layer, and arc melting the deposited silica powder layer while reducing the pressure. To manufacture. When performing arc melting, the silica glass crucible having a transparent layer and a bubble-containing layer can be produced by strongly reducing the pressure of the silica powder in the initial stage of arc melting and then reducing the pressure reduction.
  • the silica glass crucible is manufactured by the rotational mold method as described above. Due to such a manufacturing method, the silica glass crucible cannot be manufactured as designed. Therefore, the shape of the manufactured silica glass crucible and the characteristics of the inner surface may be deviated from the design drawing. In addition, as described above, it is necessary to prepare a silica glass crucible separately for each pulling of the silicon single crystal. However, if there is a defect in the manufactured silica glass crucible, the single crystal ratio is reduced when the silicon single crystal is pulled. May cause deterioration. Thus, the silica glass crucible cannot be manufactured as designed, and the manufactured silica glass crucible may have defects that cause deterioration of the single crystal ratio. Therefore, the manufactured silica glass crucible is inspected.
  • Patent Document 1 As a technique for inspecting a silica glass crucible, for example, there is Patent Document 1.
  • Patent Document 1 at least one of an infrared absorption spectrum and a Raman spectrum is measured at a measurement point on the inner surface of a silica glass crucible, and whether or not an abnormal site such as a brown ring is generated based on the obtained spectrum.
  • a method for inspecting a silica glass crucible comprising a step of judging is described. According to Patent Document 1, with the above-described configuration, it is possible to grasp a silica glass crucible where an abnormal site is likely to occur before shipment.
  • Patent Document 2 includes a step of measuring a three-dimensional shape of the inner surface of a silica glass crucible with an internal distance measuring unit, a step of (1) measuring a three-dimensional shape of a foreign object, and (2) a step of measuring a three-dimensional distribution of strain. A method for evaluating a silica glass crucible having any of the steps is described.
  • Patent Document 3 discloses an inspection method for a silica glass crucible in which ultraviolet light having a wavelength of 365 nm is irradiated on a side surface of a silica glass crucible, and the number of fluorescent spots having a wavelength within a range of 420 nm to 600 nm generated on a silica glass crucible wall surface is measured. Is described. According to Patent Document 4, with the above configuration, impurities localized in the silica glass crucible can be easily detected.
  • Patent Document 4 discloses a method for manufacturing a glass substrate that can reduce breakage of the glass substrate while increasing the production efficiency of the glass substrate.
  • the method for manufacturing a glass substrate includes a heat treatment step for the glass substrate formed by the downdraw method.
  • the glass substrate is suspended by holding the upper end portion of the glass substrate with a holding member, and the glass substrate is heat-treated while being transported along the transport direction.
  • the glass substrate has a main surface that is curved so as to protrude along the transport direction.
  • Patent Document 5 discloses a method for producing a glass substrate for a magnetic recording medium that can sufficiently reduce the surface waviness of a short wavelength and the surface waviness of a medium wavelength on the main surface of the glass substrate for a magnetic recording medium.
  • the surface roughness Ra at a measurement wavelength of 2.5 to 80 ⁇ m is 0.40 to 1.40 ⁇ m
  • the surface roughness Ra at a measurement wavelength of 2.5 to 800 ⁇ m is 0.40 to 2.00 ⁇ m.
  • Patent Document 6 discloses a method for quantitatively evaluating the amount of corrosion of reinforcing steel in a reinforced concrete structure using acoustic emission.
  • a piezoelectric element sensor is installed in a reinforced concrete structure, and acoustic emission generated due to an external load received by the concrete structure is detected.
  • the peak frequency f obtained by processing the acoustic emission is a hit number Hlow satisfying f1 ⁇ f ⁇ f2 with respect to an arbitrary frequency f1, f2, f3, f4 (f1 ⁇ f2 ⁇ f3 ⁇ f4), Evaluation is performed in a ratio with the number of hits High that satisfies f3 ⁇ f ⁇ f4.
  • Patent Document 7 discloses a defect site detection apparatus using an acoustic emission method that can clarify the position information of a defect site by removing a heat insulating material only at a sensor installation location of an inspection object such as a pipe.
  • This apparatus includes a waveform analysis device having a time-frequency analysis unit, an analysis waveform storage unit, and a calculation unit.
  • the time-frequency analysis unit extracts the highest frequency component that can be extracted from the original sound waveform detected by the sensor using time-frequency analysis in a certain frequency band, and then sequentially extracts the frequency component in a lower frequency band. To separate the waveforms.
  • the analysis waveform storage unit stores the waveform of each frequency band component separated.
  • the calculation unit reads the propagation time of the stored waveform in each frequency band, and calculates the distance between the defect site serving as the sound source and the sensor based on the difference and the propagation speed in each frequency band.
  • Patent Document 8 discloses a rotating machine bearing diagnostic apparatus using AE that can perform any bearing diagnosis regardless of the magnitude of the load and the rotating mode of the rotating machine.
  • the detection signal of the AE sensor is amplified and detected, an effective value is calculated by an effective value circuit, and a gate signal for determining a constant speed period of the elevator hoisting machine is output from the comparator to the gate circuit.
  • the control unit calculates a threshold value based on the effective value calculated by the effective value circuit during a predetermined period in the gate signal period, and outputs the threshold value to the comparator via the D / A converter.
  • the comparator outputs a signal when there is a signal equal to or greater than the threshold value among the signals that have passed through the gate circuit, and a pulse is output from the waveform shaping circuit by this signal. Whether or not the bearing is possible is diagnosed by the number of pulses.
  • Patent Document 9 discloses a plate glass cutting method and apparatus capable of cutting plate glass at a high speed and preventing deterioration in plate glass quality. This method detects the pressing force of the cutter wheel without a time lag by detecting the pressing force of the cutter wheel by a detecting unit such as a piezoelectric element while processing the cutting line of the plate glass. Also, since the vertical movement of the cutter wheel is controlled so as to follow the unevenness of the plate glass by the operation of the pressing means such as a linear motor, the cutter wheel is moved up and down so as to respond at high speed to the control signal from the control unit. .
  • Patent Literature 10 discloses a composite container inspection method and inspection system.
  • This composite container inspection method is a composite container inspection method including a liner forming a container and a reinforcing layer formed by winding fibers around the liner.
  • This inspection method includes a signal acquisition step of acquiring an acoustic emission signal from an acoustic emission sensor attached to the composite container, and a first indication of a sign of fatigue failure of the liner based on the acoustic emission signal acquired by the signal acquisition step. And a first determination step for determining whether or not the above condition is satisfied.
  • the first condition is a condition determined based on the energy of acoustic emission.
  • ⁇ Problems with cracks> In a silica glass crucible, when stress is applied to a silica glass crucible having growing cracks, the cracks grow and eventually the silica glass crucible is broken. In particular, when pulling up a silicon single crystal, about 400 kg of polycrystalline silicon is filled in the silica glass crucible, and therefore, a force pushed by the polycrystalline silicon from the inside acts on the silica glass crucible. In the process of pulling up the silicon single crystal, the silica glass crucible may be cracked or cracked, and the silicon melt in the crucible may leak out. It is known that such glass breakage is caused by the presence of cracks as starting points of cracks.
  • the crack as the starting point of the crack as described above may be formed at the stage of filling the silica glass crucible with polycrystalline silicon, but may also be formed in the process of manufacturing the silica glass crucible. Therefore, in order to prevent the situation where the silica glass crucible is broken, the silica glass crucible is inspected at the stage where the silica glass crucible is manufactured, and the crack formed in the silica glass crucible. It is necessary to inspect for the presence or absence of this. In particular, it is very important to accurately find cracks (including microcracks) that lead to cracking of the silica glass crucible before the silicon single crystal is pulled (before use).
  • the planar glass substrate before the heat treatment has only a predetermined strength to be inspected by the AE method. Is not considered.
  • an AE sensor is merely used for inspecting whether or not the manufactured glass substrate (plane) for a magnetic recording medium has a predetermined quality.
  • the technologies described in Patent Documents 4 to 10 do not consider the shape and bubble layer peculiar to the crucible. Therefore, the AE occurs, for example, by changing the sensor position for the crucible and how to apply external pressure. The ease of crucible cracking cannot be evaluated taking into account the position.
  • an object of the present invention is to provide a crucible inspection apparatus, a crucible inspection method, a silica glass crucible, and a silica glass crucible that can solve the problem that it is impossible to inspect the presence of a crack that may become a starting point of a crack. It is providing the manufacturing method of this, the manufacturing method of a silicon ingot, and the manufacturing method of a homoepitaxial wafer.
  • the crucible inspection apparatus is Inspecting the ease of cracking of a silica glass crucible comprising a cylindrical side wall, a curved bottom, and a corner provided between the side wall and the bottom and having a curvature higher than the curvature of the bottom.
  • a silica glass crucible inspection device A configuration is adopted in which an AE wave detecting means is provided which is installed on the surface of the silica glass crucible and detects an AE (Acoustic Emission) wave generated when a predetermined external force is applied to the silica glass crucible.
  • the inspection object using the conventional AE is used at room temperature, but the inspection object silicon single crystal pulling temperature of the present invention is high (the silicon melt is 1400 ° C. or higher, the temperature of the silica glass crucible).
  • the silicon melt is 1400 ° C. or higher, the temperature of the silica glass crucible.
  • This silica glass crucible is used in a state of being fitted into a carbon susceptor in a pulling device. Therefore, even if it is 1600 degreeC, it does not fall outside by the carbon susceptor outside the silica glass crucible, and can be used as a crucible.
  • quartz glass alone is deformed at about 1200 ° C.
  • the silica glass crucible is used in a completely different environment from general quartz glass, and it is necessary to detect microcracks that are so small that they cannot be compared with an object used at room temperature.
  • stress may be concentrated in the curved portion in the silica glass crucible, and it is necessary to detect minute microcracks in order to withstand the stress.
  • conventional inspection objects using AE waves are composed of simple materials such as blocks and pipes, but silica glass crucibles have side walls, corners, and bottoms, and are composed of curved surfaces. In addition, it has a layer structure of a transparent layer and a bubble layer. For this reason, the conventional method cannot be applied as it is.
  • non-destructive silica glass crucibles that are actually used for pulling up silicon single crystals at high temperatures for a long time are inspected without cutting sample pieces from the silica glass crucible. Can be selected. Thereby, it is possible to prevent troubles such as high temperature silicon melt leaking into the silicon single crystal pulling furnace (CZ furnace) due to cracking or opening of the silicon single crystal.
  • CZ furnace silicon single crystal pulling furnace
  • AE wave inspection means for inspecting AE waves is installed on the surface of the silica glass crucible, Apply a predetermined external force to the silica glass crucible, AE (Acoustic Emission) wave generated when the predetermined external force is applied to the silica glass crucible is detected. The structure is taken.
  • the silica glass crucible which is another embodiment of the present invention, A configuration is adopted in which the number of defects that generate AE waves when an external force is applied is equal to or less than a predetermined threshold.
  • An AE wave inspection means for inspecting the AE wave is installed on the surface of the silica glass crucible, a predetermined external force is applied to the silica glass crucible, and an AE (Acoustic Emission) wave generated when the predetermined external force is applied to the silica glass crucible. It has a configuration of having a detecting step.
  • the method for producing a silicon ingot according to another embodiment of the present invention A configuration is adopted in which the method includes the step of pulling up the silicon single crystal using the silica glass crucible manufactured by the silica glass crucible manufacturing method described above.
  • a homoepitaxial wafer according to another embodiment of the present invention includes a step of forming a substrate portion by a wafer formed by cutting out a silicon ingot manufactured by the above method, and a silicon single crystal homoepitaxial layer on the substrate portion Forming a step.
  • the present invention is configured as described above, and can solve the problem that the presence of a crack that may be a starting point of a crack cannot be inspected. By this, even if it is a microcrack that cannot be seen by visual inspection or image inspection, or a microcrack that exists inside the crucible wall, the inside surface and wall portion of these silica glass crucibles can be inspected using AE waves. Internal microcracks can be found.
  • FIG. 1 It is a figure which shows an example of a structure of the silica glass crucible used as the test object in the 1st Embodiment of this invention. It is a figure which shows an example of a structure of the crucible inspection apparatus in the 1st Embodiment of this invention. It is a figure which shows an example of a structure of the AE sensor shown in FIG. It is a figure which shows an example of a mode at the time of installing the AE sensor shown in FIG. 2 in a silica glass crucible. It is a figure which shows an example of a structure of the AE wave analysis apparatus shown in FIG. It is a figure for demonstrating an example of the measurement by the AE wave intensity measurement part shown in FIG.
  • FIG. 1 is a diagram illustrating an example of the configuration of the silica glass crucible 1.
  • FIG. 2 is a diagram illustrating an example of the configuration of the crucible inspection apparatus 2.
  • FIG. 3 is a diagram illustrating an example of the configuration of the AE sensor 21.
  • FIG. 4 is a diagram illustrating an example of a state when the AE sensor 21 is installed in the silica glass crucible 1.
  • FIG. 5 is a diagram illustrating an example of the configuration of the AE wave analyzer 23.
  • FIG. 6 is a diagram for explaining an example of measurement by the AE wave intensity measurement unit 231.
  • FIG. 7 is a diagram for explaining an example of AE wave measurement by the AE wave generation number measurement unit 232.
  • FIG. 8 is a diagram for explaining an example of calculation of the AE wave generation position by the AE wave generation position calculation unit 233.
  • FIG. 9 is a flowchart showing an example of the operation of the crucible inspection apparatus 2.
  • the crucible inspection apparatus 2 in the first embodiment of the present invention, a crucible inspection apparatus 2 that inspects and evaluates the fragility of the silica glass crucible 1 will be described.
  • the crucible inspection apparatus 2 in the present embodiment has an AE (Acoustic Emission) sensor 21 and detects an AE wave generated when a predetermined external force is applied to the silica glass crucible 1.
  • the crucible inspection apparatus 2 inspects and evaluates the ease of cracking of the silica glass crucible 1 based on the detection result of the AE wave by the AE sensor 21.
  • a silica glass crucible 1 to be inspected / evaluated by the crucible inspection apparatus 2 in this embodiment includes a cylindrical side wall portion 11, a curved bottom portion 12, a side wall portion 11 and a bottom portion 12. And a corner portion 13 having a higher curvature than the bottom portion 12. Moreover, the upper end surface of the side wall part 11 of the silica glass crucible 1 is formed as an annular flat surface.
  • the silica glass crucible 1 includes a transparent layer 111 in which bubbles are not observed and a bubble-containing layer 112 in which bubbles are observed from the inner surface toward the outer surface of the silica glass crucible 1 based on visual observation or image data.
  • the silica glass crucible 1 has various sizes such as 28 inches (about 71 cm), 32 inches (about 81 cm), 36 inches (about 91 cm), and 40 inches (about 101 cm) in diameter.
  • Such a silica glass crucible 1 is manufactured using, for example, a rotational mold method. That is, the silica glass crucible 1 forms a silica powder layer by depositing silica powder on the inner surface of a rotating mold (made of carbon), and arc-melting the deposited silica powder layer while reducing the pressure. Manufactured by. When performing arc melting, silica powder is strongly depressurized in the initial stage of arc melting, and then the pressure is weakened, whereby the silica having the transparent layer 111 on the inner surface side and the bubble-containing layer 112 on the outer surface side. A glass crucible 1 can be manufactured.
  • the silica glass crucible 1 is manufactured by the method as described above, for example, unmelted silica powder is attached to the outer surface layer of the silica glass crucible 1. That is, the outer surface layer of the silica glass crucible 1 has a rough roughness.
  • Silica powder used for the production of the silica glass crucible 1 includes natural silica powder produced by pulverizing natural quartz and synthetic silica powder produced by chemical synthesis. Natural silica powder contains impurities, but synthetic silica powder has high purity. On the other hand, synthetic silica glass obtained by melting synthetic silica powder has a lower viscosity at high temperature than silica glass obtained by melting natural silica powder. Thus, natural silica powder and synthetic silica powder have a plurality of differences in their properties. When manufacturing the silica glass crucible 1, natural silica powder and synthetic silica powder can be used properly.
  • the crucible inspection apparatus 2 in the present embodiment includes an AE sensor 21 (AE wave detection means), an amplifier 22, and an AE wave analysis apparatus 23.
  • the AE sensor 21 and the amplifier 22 are connected so that an electric signal can be transmitted.
  • the amplifier 22 and the AE wave analyzer 23 are also connected so as to be able to transmit electrical signals.
  • FIG. 2 shows a case where the crucible inspection apparatus 2 has one AE sensor 21 as an example of the configuration of the crucible inspection apparatus 2.
  • the number of AE sensors 21 included in the crucible inspection apparatus 2 is not limited to one.
  • the crucible inspection apparatus 2 may have an arbitrary number of AE sensors 21 of two or more.
  • the AE sensor 21 is installed on the surface of the silica glass crucible 1 and detects an AE wave generated when a predetermined external force is applied to the silica glass crucible 1.
  • the AE sensor 21 can be configured to detect the AE wave so that the time when the AE wave is detected can be discriminated.
  • the AE sensor 21 includes, for example, a piezoelectric element 211, a receiving plate 212, and a connector 213.
  • a piezoelectric element 211 is provided on one surface of the receiving plate 212, and the piezoelectric element 211 and the connector 213 are connected so that a current can flow.
  • the receiving plate 212 is in contact with the silica glass crucible 1 on the other surface (the surface opposite to the side on which the piezoelectric element 211 is provided).
  • the AE sensor 21 in the present embodiment is installed on the inner surface of the silica glass crucible 1. That is, the receiving plate 212 of the AE sensor 21 is installed on the inner surface of the silica glass crucible 1 so as to be in contact with the transparent layer 111 of the silica glass crucible 1.
  • the outer surface layer of the silica glass crucible 1 has a rough roughness. In order to increase the detection accuracy of the AE wave, it is desirable that the installation surface does not have roughness. Therefore, by installing the AE sensor 21 on the inner surface of the silica glass crucible 1 as described above, Compared with the case where it is installed on the outer surface of the silica glass crucible 1, it is possible to detect the AE wave with higher accuracy.
  • the piezoelectric element 211 converts a force applied to itself into a voltage. Specifically, the piezoelectric element 211 in the present embodiment detects distortion of the silica glass crucible 1 due to propagation of AE waves and converts the distortion into a voltage. That is, the piezoelectric element 211 detects an AE wave and generates an electric signal (AE signal) corresponding to the AE wave.
  • the piezoelectric element 211 in the present embodiment is, for example, a piezoelectric ceramic, and is made of, for example, lead zirconate titanate (Pb (Zr, Ti) O3).
  • the receiving plate 212 is provided with a piezoelectric element 211 on one surface, and comes into contact with the silica glass crucible 1 on the other surface.
  • the receiving plate 212 is distorted by AE waves propagating through the silica glass crucible 1. As the receiving plate 212 is distorted in this way, the AE wave generated in the silica glass crucible 1 is transmitted to the piezoelectric element 211.
  • the receiving plate 212 is ceramics, for example.
  • Connector 213 connects piezoelectric element 211 and amplifier 22 which is an external device. As described above, the piezoelectric element 211 is connected to the connector 213, and the AE signal generated by the piezoelectric element 211 is transmitted to the amplifier 22 via the connector 213.
  • at least three AE sensors 21 described above are installed in the silica glass crucible 1. As will be described later, by using at least three AE sensors 21, it is possible to specify the position of the AE occurrence position on the plane when the three-dimensional silica glass crucible 1 is developed on the plane.
  • At least three AE sensors 21 are installed on the side wall part 11, the bottom part 12, and the corner part 13, for example.
  • a plurality of AE sensors 21 are arranged at equal intervals in the circumferential direction of the cylinder.
  • the AE sensor 21 is applied to the corner portion 13 where internal residual stress is likely to be accumulated in the silica glass crucible 1 and the bottom portion 12 where pressure is easily applied when filling a material (polycrystalline silicon) for pulling up the silicon single crystal. Is preferably arranged.
  • the silica glass crucible 1 is likely to break when the silicon single crystal is pulled. Therefore, it is desirable to inspect the ease of cracking of the silica glass crucible 1 by installing the AE sensor 21 around the connection portion between the corner portion 13 and the bottom portion 12.
  • the amplifier 22 amplifies the AE signal received from the AE sensor 21.
  • the AE signal amplified by the amplifier 22 is transmitted to the AE wave analyzer 23.
  • the configuration of the amplifier 22 is not particularly limited.
  • the AE wave analyzer 23 receives the AE signal amplified by the amplifier 22. Then, the AE wave analysis device 23 measures the strength of the AE wave based on the received AE signal, counts the number of times the AE wave is detected, and is easy to break the silica glass crucible 1 based on the detection result. Or evaluate.
  • the AE wave analysis device 23 includes, for example, a filter, an in-device amplifier, an envelope detection unit, and the like (not shown).
  • the AE wave analyzer 23 removes a signal having a frequency unnecessary for the inspection from the AE signal received from the amplifier 22 using a filter. Then, the AE wave analyzing device 23 amplifies the removed AE signal with an in-device amplifier. Thereafter, the AE wave analyzer 23 performs processing such as measurement using the amplified AE signal. Further, the AE wave analysis device 23 extracts the envelope of the amplified AE signal by the envelope detection means (specifically, for example, after half-rectifying the negative portion of the AE signal, the envelope detection is performed). Do). The AE wave analyzer 23 can also perform processing such as measurement using the extracted envelope.
  • FIG. 5 shows an example of the main configuration of the AE wave analyzer 23.
  • the AE wave analysis device 23 includes, for example, an AE wave intensity measurement unit 231, an AE wave generation frequency measurement unit 232, an AE wave generation position calculation unit 233 (position specifying unit), and a crucible evaluation unit. 234 (crucible evaluation means) and a measurement result storage unit 235.
  • the AE wave analysis device 23 includes a central processing unit (CPU: Central Processing Unit) (not shown) and a storage device, and the CPU executes a program stored in the storage device, thereby realizing the above-described units.
  • CPU Central Processing Unit
  • the AE wave analysis device 23 may have a configuration other than the above-exemplified examples, or may be configured by a part of the above-exemplified examples (for example, the AE wave analysis device 23 has an AE wave strength). And a measuring unit 231 and a crucible evaluating unit 234.
  • the AE wave intensity measurement unit 231 measures the intensity of the AE wave detected by the AE sensor 21.
  • the AE wave intensity measurement unit 231 measures the intensity of the AE wave based on the AE signal waveform amplified by the in-device amplifier.
  • FIG. 6 is an example of an AE signal waveform after amplification by the in-device amplifier.
  • the AE wave intensity measurement unit 231 measures the maximum amplitude, which is the largest amplitude among the AE signal waveforms, as the intensity of the AE wave.
  • the maximum amplitude represents the energy level (dB) of the AE wave.
  • the AE wave intensity measurement unit 231 may be configured to measure the AE average value as the AE wave intensity instead of the maximum amplitude.
  • the AE average value can be calculated by, for example, averaging the envelope waveform extracted by envelope detection.
  • the AE wave intensity measuring unit 231 may be configured to measure the AE effective value (effective value, root mean square value, RMS) as the AE wave intensity.
  • the AE wave generation number measurement unit 232 measures the number of detections of the AE wave detected by the AE sensor 21. For example, the AE wave generation frequency measurement unit 232 measures the number of detections of the AE wave based on the envelope waveform extracted by envelope detection and a predetermined threshold value (a value larger than the noise signal). .
  • FIG. 7 is an example of an envelope waveform extracted by envelope detection. As illustrated in FIG. 7, for example, the AE wave generation number measurement unit 232 measures the number of detections of the AE wave by counting the number of times exceeding the threshold value in the envelope waveform. For example, in the case of FIG. 7, the AE wave generation number measurement unit 232 measures that the AE wave has been detected twice.
  • the AE wave generation frequency measurement unit 232 may be configured to calculate, for example, the AE wave generation frequency per unit time obtained by dividing the measured frequency by the measurement time.
  • the AE wave generation position calculation unit 233 calculates the generation position of the AE wave. For example, the AE wave generation position calculation unit 233 calculates the generation position of the AE wave based on the difference in detection time when the plurality of AE sensors 21 installed in the silica glass crucible 1 detect the AE wave. Specifically, the AE wave generation position calculation unit 233 determines the generation position of the AE wave based on the difference in detection time when each AE sensor 21 detects the AE wave and the sound velocity V in the silica glass crucible 1. Is calculated.
  • FIG. 8 is a diagram for explaining an example of the calculation of the AE wave by the AE wave generation position calculation unit 233.
  • FIG. 8 shows one example when calculating the generation position of the AE wave in one dimension as an example for explaining the calculation method of the generation position of the AE wave.
  • the AE sensor 21-1 and the AE sensor 21- 2 is set at a known coordinate, and an AE wave generated from a crack 3 existing on an unknown coordinate x is detected. As shown in FIG. 8, for example, it is assumed that the AE sensor 21-1 is installed at the coordinate k1, and the AE sensor 21-2 is installed at the coordinate k2.
  • the AE sensor 21-1 detects an AE wave generated from the crack 3 at time t1
  • the AE sensor 21-2 detects an AE wave generated from the crack 3 at time t2.
  • the speed of sound waves in the silica glass crucible 1 is about 5700-5900 m / s for longitudinal waves and about 3700 m / s for transverse waves.
  • the AE wave generation position calculation unit 233 uses the three AE sensors 21 to calculate the two-dimensional position of the crack 3 based on the positional relationship between the three AE sensors and the difference in detection time. I can do it.
  • the two-dimensional position is a coordinate on a plane when the three-dimensional silica glass crucible 1 is developed on the plane.
  • the actual silica glass crucible 1 has a three-dimensional shape (a cylindrical side wall portion 11, a curved bottom portion 12, a corner portion 13 provided between the side wall portion 11 and the bottom portion 12 and having a higher curvature than the bottom portion 12). It is.
  • the AE wave generation position calculation unit 233 returns (reversely converts) the calculated two-dimensional position of the crack 3 to the actual three-dimensional shape of the silica glass crucible 1 to calculate the three-dimensional position of the crack 3. Also good. Thereby, the three-dimensional shape of the silica glass crucible 1 and the position of the crack 3 can be accurately grasped.
  • the crucible evaluation unit 234 evaluates the ease of cracking of the silica glass crucible 1 based on the measurement, measurement, and calculation results by the AE wave intensity measurement unit 231, the AE wave generation frequency measurement unit 232, and the AE wave generation position calculation unit 233. To do.
  • the crucible evaluation unit 234 compares the value of the measurement result obtained by the AE wave intensity measurement unit 231 with a strength threshold value (arbitrarily adjusted value) stored in advance. And when the value of a measurement result exceeds the strength threshold, crucible evaluation part 234 evaluates that silica glass crucible 1 is easy to break. Thus, the crucible evaluation unit 234 evaluates the ease of cracking of the silica glass crucible 1 based on the strength of the AE wave generated when a predetermined external force is applied to the silica glass crucible 1, for example.
  • a strength threshold value arbitrarily adjusted value
  • the silica glass crucible 1 When the result of measurement by the AE wave intensity measurement unit 231 is equal to or greater than a preset threshold, if the silicon single crystal is actually pulled up using the silica glass crucible 1, the silica glass crucible 1 may be broken in the middle. Becomes stronger.
  • the crucible evaluation unit 234 compares the value of the measurement result obtained by the AE wave generation frequency measurement unit 232 with a frequency threshold value (arbitrarily adjusted value) stored in advance. And when the value of a measurement result exceeds the frequency threshold, crucible evaluation part 234 evaluates that silica glass crucible 1 is easy to break. Thus, the crucible evaluation part 234 evaluates the ease of cracking of the silica glass crucible 1 based on the number of AE waves generated when a predetermined external force is applied to the silica glass crucible 1, for example.
  • the AE wave generation frequency measuring unit 232 As a result of measurement by the AE wave generation frequency measuring unit 232, when AE waves of a preset number of times or more are measured, when the silicon single crystal is actually pulled up using the silica glass crucible 1, the silica glass crucible 1 breaks along the way. The risk of getting stronger.
  • the crucible evaluation unit 234 can evaluate the ease of cracking of the silica glass crucible 1 based on the calculation result by the AE wave generation position calculation unit 233. For example, it is conceivable that the ease of cracking of the silica glass crucible 1 changes depending on the position of a crack generated in the silica glass crucible 1. Therefore, the crucible evaluation unit 234 evaluates the ease of cracking of the silica glass crucible 1 based on the calculation result by the AE wave generation position calculation unit 233.
  • the crucible evaluation unit 234 evaluates the easiness of cracking of the silica glass crucible 1 based on whether or not there is a curved corner portion 13 or bottom portion 12 or a connection portion microcrack between the corner portion 13 and the bottom portion 12. It is desirable to do.
  • the crucible evaluation unit 234 can be configured to evaluate the ease of cracking of the silica glass crucible 1 by combining a plurality of the above-exemplified methods. For example, the crucible evaluation unit 234 determines the target when the result of the measurement by the AE wave intensity measurement unit 231 is equal to or greater than a predetermined threshold value and more than a predetermined number of AE waves are measured. It can be evaluated that the silica glass crucible 1 is easily broken. Also, the crucible evaluation unit 234 may change the threshold value to be compared with the value of the measurement result obtained by the AE wave intensity measurement unit 231 according to the generation position of the AE wave, for example.
  • the crucible evaluation unit 234 may change the number of AE waves that are allowable for each location of the silica glass crucible 1.
  • the crucible evaluating unit 234 may evaluate the ease of cracking of the silica glass crucible 1 by a combination other than those exemplified above.
  • the measurement result storage unit 235 is a storage device such as a semiconductor memory or a hard disk.
  • the measurement result storage unit 235 stores the measurement, measurement, and calculation results obtained by the AE wave intensity measurement unit 231, the AE wave generation frequency measurement unit 232, and the AE wave generation position calculation unit 233. Further, the measurement result storage unit 235 stores the evaluation result obtained by the crucible evaluation unit 234. In the measurement result storage unit 235, for example, measurement, measurement, calculation result, and evaluation result for each silica glass crucible 1 are stored.
  • the AE wave is generated by the generation or growth of cracks in the silica glass crucible 1 due to external force applied to the silica glass crucible 1 or internal force fluctuations. Therefore, in order to detect the AE wave by the crucible inspection apparatus 2, it is necessary to apply an external force to the silica glass crucible 1 or cause an internal force fluctuation.
  • generation of AE waves is induced by applying an external force to the silica glass crucible 1 using air or water pressure.
  • the compressed air is hit against the silica glass crucible 1 and the AE wave generated when the compressed air is hit is detected by the crucible inspection device 2.
  • the crucible inspection apparatus 2 detects an AE wave generated using water pressure.
  • the silica glass crucible 1 includes a cylindrical side wall part 11, a curved bottom part 12, and a container part that connects the side wall part 11 and the bottom part 12 and has a corner part 13 having a higher curvature than the bottom part 12. It has the shape of For this reason, the inside of the silica glass crucible 1 can be filled with water (liquid). By filling with water, an external force (force directed outward from the center inside the crucible) can be uniformly applied to the inner surfaces of the cylindrical side wall portion 11, the curved bottom portion 12, and the corner portion 13 having a predetermined curvature. it can.
  • the position where the external force on the inner surface of the crucible is to be applied can be easily selected depending on the amount of water to be filled. For example, if only the bottom portion 12 is filled with water, an external force can be applied only to the bottom portion 12, and if water is filled up to the corner portion 13, an external force can be applied from the bottom portion 12 to the corner portion 13. Moreover, if water is filled to the predetermined height of the side wall part 11, external force can be given to the height with which the water of the bottom part 12, the corner part 13, and the side wall part 11 was filled.
  • the AE wave can be inspected while continuously changing the position where the external force is applied to the inner surface of the crucible.
  • the use of the crucible inspection apparatus 2 is not limited to the case of inspecting the silica glass crucible 1 nondestructively.
  • the crucible inspection apparatus 2 may be configured to detect an AE wave generated by a destructive inspection of the silica glass crucible 1.
  • the AE sensor 21 of the crucible inspection apparatus 2 in the present embodiment is installed on the surface of the silica glass crucible 1. Specifically, the AE sensor 21 is installed on the inner surface of the silica glass crucible 1, for example. Then, an AE wave is generated in the silica glass crucible 1 by applying a predetermined external force to the silica glass crucible 1.
  • the AE sensor 21 of the crucible inspection apparatus 2 detects an AE wave generated when a predetermined external force is applied to the silica glass crucible 1 (step S001). Specifically, the AE sensor 21 detects an AE wave and generates an AE signal according to the AE wave. The AE signal generated by the AE sensor 21 is amplified by the amplifier 22, and the amplified AE signal is received by the AE wave analyzer 23.
  • the AE wave analyzer 23 evaluates the ease of cracking of the silica glass crucible 1 based on the received AE signal (step S002). Specifically, the AE wave intensity measurement unit 231 of the AE wave analyzer 23 measures the intensity of the AE wave based on the received AE signal. In addition, the AE wave generation frequency measurement unit 232 of the AE wave analyzer 23 measures the number of AE wave generations based on the received AE signal. Further, the AE wave generation position calculation unit 233 of the AE wave analysis device 23 calculates the generation position of the AE wave.
  • the crucible evaluation unit 234 of the AE wave analysis device 23 uses the silica glass based on the measurement, measurement, and calculation results of the AE wave intensity measurement unit 231, the AE wave generation frequency measurement unit 232, and the AE wave generation position calculation unit 233. The ease of cracking of the crucible 1 is evaluated.
  • the crucible inspection apparatus 2 in the present embodiment includes the AE sensor 21 and the AE wave analysis apparatus 23.
  • the crucible inspection apparatus 2 can detect an AE wave generated when an external force is applied to the silica glass crucible 1.
  • the crucible inspection apparatus 2 can evaluate the ease of cracking of the silica glass crucible 1 based on the detection result.
  • the ease of extension of microcracks can be evaluated from the number of times the AE wave is detected. It is possible to evaluate whether or not it affects the cracking and deformation of the crucible from the ease of extension of microcracks.
  • the size of the microcrack can be estimated from the strength of the AE wave.
  • the position of the microcrack can be estimated from the generation position of the AE wave. Considering the position where the pressure is applied by filling the raw material in the crucible and the position of the liquid surface during the pulling of the silicon single crystal, it can be evaluated whether the position where the microcracks are present affects the cracking and deformation of the crucible. Further, by evaluating these in combination, it is possible to grasp the ease of extension, size, and position of the microcracks in the crucible. Thereby, it is possible to evaluate whether the microcrack affects the crucible crack and the deformation during the pulling in consideration of the pulling condition of the silicon single crystal (the length of pulling time, the raw material filling amount, etc.).
  • the AE sensor 21 includes the piezoelectric element 211, the receiving plate 212, and the connector 213.
  • the configuration of the AE sensor 21 is not limited to the above case.
  • the AE sensor 21 may have a damper material.
  • the AE sensor 21 is installed on the inner surface of the silica glass crucible 1.
  • the AE sensor 21 may be installed on a surface other than the inner surface such as the outer surface of the silica glass crucible 1.
  • a crucible inspection method using the crucible inspection apparatus 2 described in the present embodiment can be performed.
  • an AE wave generation source such as a crack exists in the produced silica glass crucible 1.
  • the silica glass crucible 1 in which the number of defects such as cracks that generate AE waves when an external force is applied is equal to or less than a predetermined threshold value can be realized.
  • the silica glass crucible 1 in which the strength of the AE wave generated when an external force is applied is equal to or less than a predetermined threshold value. Further, by using the silica glass crucible 1 manufactured by the method for manufacturing the silica glass crucible 1 described above, for example, by pulling up the silicon ingot by the Czochralski method, cracks are not generated during the pulling. Can raise the silicon ingot.
  • FIGS. 10A to 10C are schematic views for explaining a method for producing a silicon single crystal using the silica glass crucible according to the present embodiment.
  • the silica glass crucible 1 when pulling up the silicon single crystal, the silica glass crucible 1 is filled with polycrystalline silicon, and in this state, the polycrystalline silicon is heated by a heater disposed around the silica glass crucible 1. And melt. Thereby, the silicon melt 230 is obtained.
  • the silica glass crucible of the present invention the crucible during filling can be prevented from being damaged.
  • the volume of the silicon melt 230 is determined by the mass of polycrystalline silicon. Therefore, the initial height position H 0 of the liquid surface 23 a of the silicon melt 230 is determined by the mass of the polycrystalline silicon and the three-dimensional shape of the inner surface of the silica glass crucible 1. That is, when the three-dimensional shape of the inner surface of the silica glass crucible 1 is determined, the volume up to an arbitrary height position of the silica glass crucible 1 is specified, whereby the initial height of the liquid surface 23a of the silicon melt 230 is determined. The position H0 is determined.
  • the tip of the seed crystal 24 is lowered to the height position H0 and brought into contact with the silicon melt 230. Then, the silicon single crystal 25 is grown by slowly pulling up the wire cable 561 while rotating it. At this time, the silica glass crucible 1 is rotated opposite to the rotation of the wire cable 561.
  • the inner surface shape of the corner portion 13 can be known, and therefore how the descent speed Vm changes can be accurately predicted. it can. Based on this prediction, pulling conditions such as the pulling speed of the silicon single crystal 25 are determined. At this time, by using the silica glass crucible 1 of the present embodiment, since the deformation from the predicted shape is less, the prediction accuracy of the descent speed Vm is further improved. As a result, it is possible to prevent transition from occurring in the corner portion 13 and to automate the lifting.
  • the silica glass crucible 1 is prevented from being deformed by the heating of the silica glass crucible 1 when the silicon single crystal 25 is pulled up (such as falling of the side wall 11, distortion, rising of the bottom 12).
  • the deviation of the descending speed Vm of the liquid surface 23a obtained from the three-dimensional shape of the inner surface of the glass crucible 1 is suppressed, and the silicon single crystal 25 having a high crystallization rate can be manufactured with a high yield.
  • the silicon single crystal is pulled up in an argon atmosphere and under reduced pressure (about 660 Pa to 13 kPa).
  • a silicon ingot may be manufactured by setting the silica glass crucible 1 manufactured in the present embodiment to a pulling device and pulling up the silicon single crystal.
  • FIG. 11 is a schematic view illustrating a silicon single crystal silicon ingot.
  • the silicon single crystal ingot 600 is manufactured by setting the silica glass crucible 1 of the present invention in a pulling apparatus and pulling it up by the above-described silicon single crystal manufacturing method.
  • the ingot 600 has a shoulder 610 on the seed crystal 24 side, a straight body 620 continuous from the shoulder 610, and a tail 630 continuous from the straight body 620. Note that the seed crystal 24 is removed from the ingot 600.
  • the diameter of the shoulder portion 610 gradually increases from the seed crystal 24 side to the straight body portion 620.
  • the diameter of the straight body 620 is substantially constant.
  • the diameter of the tail 630 gradually decreases as the distance from the straight body 620 increases.
  • the quality of the ingot 600 is closely related to the quality of the silica glass crucible 1 to be pulled up.
  • contamination of the silica glass crucible 1 for example, an impurity metal element in the glass
  • foreign matters leads to dislocation of the silicon single crystal in the ingot 600.
  • the smoothness of the inner surface of the silica glass crucible 1 unevenness that can be seen visually
  • the amount and size of bubbles in the vicinity of the surface there is a minute amount into the silicon due to chipping of the crucible surface, cracking of the bubbles, or crushing.
  • debris particles peeled off from the crucible
  • the liquid level lowering speed Vm is determined by a function f of the crucible inner volume and the silicon single crystal growth speed Vg (see FIG. 12B).
  • the liquid level lowering speed Vm is obtained by calculation using this function f.
  • the inner shape of the crucible is deformed and the internal volume is changed due to exposure to high temperature (see FIG. 12C).
  • the silica glass crucible is inserted into the carbon susceptor. Therefore, the outer peripheral surface of the silica glass crucible is in a state of being fitted to the carbon susceptor. For this reason, the silica glass crucible is not deformed outward but deformed only inward.
  • the internal volume of the crucible changes, the calculation of the liquid level lowering speed Vm becomes inaccurate, and the silicon single crystal growth speed Vg cannot be determined accurately. This growth rate Vg is an important factor in the generation of crystal defects. Therefore, if the growth rate Vg cannot be accurately controlled, the quality of the ingot 600 is greatly affected.
  • Vg ⁇ L / ⁇ s ⁇ ( ⁇ R / r) 2 ⁇ Vm
  • Vg ⁇ 2 ⁇ ⁇ L / ⁇ s ⁇ ( ⁇ R / r) 2 ⁇ Vm ⁇
  • the thickness of the silicon wafer is 1 A pulling control of / 10 to 1/100 or less (pulling control for making COP substantially zero) is necessary. In this case, in order to control the decrease in the liquid level of the silicon melt, it is necessary to control the accuracy of 0.01 mm or less.
  • the growth rate Vg of the silicon single crystal fluctuates 2%.
  • the rate of decrease Vm of the silicon melt at the corner 13 of the silica glass crucible 1 is higher than the rate of decrease of the level of the silicon melt at the straight body of the silica glass crucible 1. Therefore, the influence of the variation in the inner diameter of the crucible on the variation in the liquid level is larger in the corner portion 13 than in the straight body portion of the crucible.
  • the relationship between the internal residual stress and the change in the inner diameter of the crucible after use (in terms of operation results) Based on the simulation of the fluctuation amount of the inner diameter of the crucible based on this, the inner diameter fluctuation amount of the crucible in use can be estimated at the stage of the silica glass crucible 1 before use (before the silicon single crystal is pulled up). This makes it possible to reduce the deviation from the target value of the growth rate Vg of the silicon single crystal compared to the case where the deformation of the crucible is not considered at all as in the conventional technique, and the entire length of the straight body portion 620 of the ingot 600 can be reduced. Defects can be suppressed (substantially zero).
  • FIG. 13 is a diagram showing a variation amount of the inner diameter of the crucible.
  • the horizontal axis indicates the amount of variation in the inner diameter of the crucible
  • the vertical axis indicates the height from the bottom of the crucible.
  • the plot of FIG. 13 is a measured value.
  • the line L connects the average of the measured value in each height. As shown by line L, it can be seen that fluctuations in the inner diameter of the crucible (that is, fluctuations in the crucible internal volume) occur on average.
  • the rising speed A of the silicon single crystal is changed based on the shape of the inner surface of the crucible, it is possible to control the growth rate Vg of the silicon single crystal so that the entire length of the silicon single crystal is within a defect-free range. become.
  • feedback control during CZ single crystal growth is performed only by a combination of ADC (automatic diameter control) and liquid level control. That is, in the prior art, the shape of the crucible in actual use is not taken into consideration at all, and the shape change of the crucible cannot be accurately grasped, so that the growth rate Vg is accurately controlled in pulling up the silicon single crystal. I can't.
  • the conventional technology does not correspond to the Vg control corresponding to the accuracy of the liquid level lowering velocity Vm of 0.01 mm or less as described above, and the performance of the semiconductor device, particularly the device of the three-dimensional structure is sufficient. It is not a silica glass crucible that can produce a silicon single crystal (ingot) to be drawn out.
  • the temperature gradient (G) in the pulling axis direction is higher on the melt side than on the solid side (in other words, lower on the solid side than on the melt side).
  • the temperature gradient in the plane (in the radial direction) perpendicular to the pulling axis (in the radial plane) is constant.
  • the silica glass crucible 1 of the present invention can stabilize the height H between the liquid surface of the silicon melt and the tip of the heat shielding member because the deformation and collapse of the silicon single crystal are suppressed.
  • the crystal defects in the straight body portion 620 are substantially zero.
  • COP Crystal Originated Particle
  • COP is one of crystal defects and is a fine defect in which silicon atoms are not present at lattice points of a single crystal (holes are collected). The presence of the COP causes deterioration of electrical characteristics (leakage current, resistance value distribution, carrier mobility, etc.) of the semiconductor device.
  • FIG. 14 is a schematic diagram for explaining a situation in which various defects occur based on the Boronkov theory.
  • V the pulling speed
  • G the temperature gradient in the pulling axis direction in the vicinity of the solid-liquid interface of the ingot (silicon single crystal)
  • V / G the temperature gradient in the pulling axis direction in the vicinity of the solid-liquid interface of the ingot (silicon single crystal)
  • the relationship between V / G and point defect concentration is schematically shown with the ratio V / G being the horizontal axis and the concentration of vacancy type point defects and the concentration of interstitial silicon type point defects being the same vertical axis. expressing. It is shown that there is a critical point that becomes a boundary between a region where a vacancy type point defect occurs and a region where an interstitial silicon type point defect occurs.
  • V / G falls below the critical point, a single crystal having a dominant interstitial silicon type point defect concentration is grown.
  • V / G is less than the critical point (V / G) I, the interstitial silicon type point defects are dominant in the single crystal, and the region where the aggregate of interstitial silicon point defects exists [I ] Appears.
  • V / G exceeds the critical point, a single crystal having a dominant vacancy point defect concentration is grown.
  • V / G is greater than the critical point (V / G) v, a region where vacancy type point defects are dominant in the single crystal and agglomerates of vacancy type point defects exist [V] Appears and COP occurs.
  • FIG. 15 is a schematic diagram showing the relationship between the pulling rate and the defect distribution during single crystal growth.
  • the defect distribution shown in FIG. 15 is obtained by growing a silicon single crystal while gradually lowering the pulling speed V, cutting the grown single crystal along the central axis (pickup axis) to form a plate-like specimen, It shows the occurrence of defects.
  • the defect distribution is a result of evaluating the occurrence of defects by decorating Cu on the surface of the plate-shaped specimen and performing heat treatment, then observing the plate-shaped specimen by the X-ray topograph method.
  • the OSF region appears in a ring shape from the outer peripheral portion of the single crystal.
  • the diameter of the OSF region gradually decreases as the pulling speed decreases, and disappears when the pulling speed becomes V1. Accordingly, a defect-free region [P] (region [PV]) appears instead of the OSF region, and the entire in-plane area of the single crystal is occupied by the defect-free region [P].
  • the fact that the COP shown above is substantially zero means that the number of detected COPs is substantially zero.
  • COP is detected by a particle counter.
  • the particle counter when the number of particles of 0.020 ⁇ m or more is detected only 30 or less on the wafer surface (semiconductor device forming surface), the number is substantially zero.
  • “0.020 ⁇ m COP” means, for example, 0.020 ⁇ m when measured with the SP series manufactured by Tencor or the particle counter device for semiconductors and silicon wafers having the same performance as this device.
  • the ingot 600 in which the COP of the straight body 620 is substantially zero is sliced into, for example, a diameter of 300 mm and a thickness of about 1 mm to become a silicon wafer.
  • electrical characteristics can be stabilized and deterioration can be suppressed.
  • the method of detecting COP may be other than the particle counter.
  • a method using a surface defect inspection apparatus after forming an oxide film of a predetermined thickness on the surface of a wafer, applying an external voltage to destroy the oxide film at the defective portion of the wafer surface and deposit copper
  • Examples include a method of detecting defects (COP) by observing the deposited copper with the naked eye, a transmission electron microscope (TEM), a scanning electron microscope (SEM), and the like. In the straight body 620 of the ingot 600, COP is not detected by such a detection method (substantially becomes zero).
  • a more preferable form of the ingot 600 according to the present invention is that all the straight body portions 620 do not have a region where point defects (voids) called vacancy are aggregated (V-Rich region where COP exists), and OSF (Oxidation Induced Stacking). Fault) is not detected, and there is no region (I-Rich region) where interstitial point defects called interstitials exist, that is, all of the straight body portion 620 is a neutral region.
  • the neutral region includes not only a region having no defects, but also a region that does not exist as an agglomerated defect or is so small that it cannot be detected even if a slight vacancy or interstitial is included.
  • the crystal defects in the straight body portion 620 are zero, the electrical characteristics of the semiconductor device manufactured using the wafer cut out from the ingot 600 can be stabilized and the deterioration can be suppressed.
  • a homoepitaxial wafer (hereinafter, also simply referred to as “epitaxial wafer”) may be configured by using a wafer cut out from the ingot 600 as a substrate portion.
  • FIG. 16 is a schematic cross-sectional view illustrating an epitaxial wafer.
  • the epitaxial wafer 700 includes a wafer substrate portion 710 cut out from the ingot 600, and a silicon single crystal epitaxial layer 720 provided on the substrate portion 710.
  • the epitaxial layer 720 is a silicon homoepitaxial layer.
  • the thickness of the epitaxial layer 720 is about 0.5 ⁇ m to 20 ⁇ m.
  • the substrate unit 710 is heated to about 1200 ° C. in an epitaxial furnace.
  • vaporized silicon tetrachloride (SiCl 4 ) and trichlorosilane (trichlorosilane, SiHCl 3 ) are flowed into the furnace.
  • trichlorosilane, SiHCl 3 trichlorosilane
  • the epitaxial layer 720 having substantially zero crystal defects can be formed.
  • a transistor called a Fin-type FET fin-type field effect transistor
  • a MOSFET Metal Oxide Semiconductor Field Effect Transistor
  • the source and drain are two-dimensionally configured.
  • the Fin-type FET has a channel region called FIN in the upper layer of the silicon surface and is in contact with the silicon wafer to form a three-dimensional MOSFET.
  • the planar type has been miniaturized by the gate length, but in the Fin type FET, the fin width is managed as the minimum dimension. There is also a Fin type FET having a fin width of about 20 nm, that is, about the same as COP. Therefore, it is required to reduce the size of the COP to the limit as the surface quality of the silicon wafer directly under the fin.
  • Such a three-dimensional structure is adopted not only in a Fin type FET but also in a three-dimensional NAND type flash memory.
  • a homoepitaxial wafer with improved quality is desired.
  • the size of the COP of the silicon wafer needs to be smaller and smaller.
  • the silicon melt can be controlled by paying attention to the relationship between the liquid level fluctuation of the silicon melt and the silica glass crucible.
  • the silica glass crucible can be evaluated based on the detection result of the AE wave, and a crucible in which there is no microcrack that affects cracking or deformation during pulling can be selected.
  • a crucible in which there is no microcrack that affects cracking or deformation during pulling can be selected.
  • microcracks exist in the silica glass crucible, the crucible is likely to be deformed at a high temperature for a long time during the pulling of the silicon single crystal. If the silica glass crucible is deformed during the pulling of the silicon single crystal, the surface of the silicon melt is disturbed, and various pulling conditions such as the pulling speed cannot be controlled.
  • a high quality epitaxial wafer can be provided by forming an epitaxial layer on the substrate portion of the wafer using the ingot.
  • the epitaxial layer 720 may be formed on the entire surface of the substrate portion 710 or may be partially formed. As a result, it is possible to provide a high-quality epitaxial wafer 700 that can be used when crystal integrity is required or when a multilayer structure with different resistivity is required.
  • FIG. 17 is a flowchart illustrating the steps from crucible manufacturing to wafer manufacturing. Steps S201 to S206 shown in FIG. 17 are crucible manufacturing processes, steps S207 to S214 are ingot manufacturing processes, steps S215 to S221 are silicon wafer manufacturing processes, and steps S222 to S227 are the same. It is a manufacturing process of an epitaxial wafer.
  • a series of processes from crucible production to ingot production shown in steps S201 to S214 is referred to as a crucible-ingot production process.
  • a series of processes from crucible manufacturing to silicon wafer manufacturing shown in steps S201 to S221 is referred to as a crucible-silicon wafer manufacturing process.
  • a series of processes from crucible manufacturing to epitaxial wafer manufacturing shown in steps S201 to S227 is referred to as a crucible-epiwafer manufacturing process.
  • an integrated control system is used for production management that assumes the quality of silicon single crystal products (ingots, silicon wafers, epitaxial wafers) due to crucible manufacturing.
  • the diameter of the straight body portion is controlled to be constant by ADC (automatic diameter control).
  • ADC automatic diameter control
  • the time required for pulling up the straight body having a diameter of about 300 mm to a total length of 2000 mm is about 4000 minutes as 0.5 mm / min.
  • the control during this period is mainly based on the relationship between the lifting speed and the weight, and the aim is to raise the COP free over the entire length of the straight body with a constant diameter.
  • the height H between the surface of the silicon melt important for pulling and the cone portion 571 is high when the pulling speed is high, and is low when the pulling speed is slow. Conventionally, the height H is controlled based on the individual difference for each lifting device and the experience of the operator.
  • the height H at the time of pulling up can be controlled more uniformly by predicting the amount of inner surface deformation of the crucible. That is, in the pulling device, the crucible is housed in the carbon susceptor 520, and becomes a weight of, for example, 500 kg due to the filling of polycrystalline silicon. In addition, the crucible being pulled becomes a high temperature of about 1600 ° C. and is pushed outward by the silicon melt, and the gap with the carbon susceptor 520 disappears. Since the carbon susceptor 520 is not deformed, as a result, the crucible is easily deformed inward by a reaction force from the carbon susceptor 520.
  • the integrated control system of the present embodiment accumulates information such as the manufacturing history of the crucible used so far, the measurement result of the internal residual stress before use, the shape change after use, etc. Calculate the behavior and deformation of the crucible when it is pulled up before use.
  • transformation of the crucible internal volume can be known from the deformation
  • Example A silica glass crucible was manufactured based on the rotational molding method. Specifically, silica powder having an average thickness of 15 mm was deposited on the inner surface of a 32-inch rotating mold to form a silica powder layer, and arc discharge was performed with three electrodes of three-phase alternating current. In the arc melting step, the energization time was 90 minutes, the output was 2500 kVA, and the silica powder layer was evacuated for 10 minutes from the start of energization. Eight silica glass crucibles were produced by the method as described above.
  • Test conditions and measurement conditions are shown below.
  • A Measurement conditions (a-1) Test machine crosshead speed: 3 mm / sec (a-2) Target load: 500 Newton (N)
  • B Measurement conditions (b-1) Preamplifier gain: 40 dB (dB) (B-2) Filter: 20 to 400 kHz bandpass filter (b-3)
  • Load analog signal 500 N / V
  • FIG. 18 is a diagram showing the relationship between the number of AE wave generations and the maximum energy value.
  • FIG. 18 shows the result of detecting AE waves for the eight manufactured silica glass crucibles according to the test conditions and measurement conditions.
  • the horizontal axis represents the number of AE waves generated (pieces / cm 2 ), and the vertical axis represents the maximum energy value (dBs) of the AE waves.
  • the silicon single crystal was pulled up using the silica glass crucible, and the presence or absence of cracking of the silica glass crucible was inspected.
  • the silica glass crucible shown by the circled plots in FIG. 18 is not cracked.
  • cracks occurred in the silica glass crucible indicated by the triangular plot in FIG. For this reason, the threshold for the number of AE waves generated was set to 6 / cm 2, and the threshold for the maximum energy value of the AE waves was set to 10 dBs.
  • silica glass crucibles were manufactured by the same manufacturing method as the above eight silica glass crucibles.
  • AE waves at the side wall, corner and bottom are measured, and the silica glass crucible after pulling up the above-mentioned threshold of the number of AE waves generated, the threshold of the maximum energy value, and the silicon single crystal.
  • the relationship between the presence or absence of cracks was investigated.
  • the relationship between the measurement results and the cracking of the silica glass crucible was as follows.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

La présente invention vise à résoudre le problème de l'incapacité à tester la présence de fissures qui peuvent initier une rupture. Ce dispositif de test de creuset, qui teste la fragilité d'un creuset en verre de silice, comprend un moyen de détection d'une onde d'émission acoustique (EA) qui est disposé sur une surface du creuset en verre de silice et détecte des ondes d'EA générées lorsqu'une force externe prédéterminée est appliquée au creuset en verre de silice. Le dispositif de test de creuset évalue également la fragilité du creuset en verre de silice sur base du résultat de détection provenant du moyen de détection d'onde d'AE.
PCT/JP2016/088285 2015-12-25 2016-12-22 Dispositif de test de creuset, procédé de test de creuset, creuset en verre de silice, procédé de fabrication d'un creuset en verre de silice, procédé de fabrication d'un lingot de silicium et procédé de fabrication d'une tranche homoépitaxiale Ceased WO2017110967A1 (fr)

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JP2019129174A (ja) * 2018-01-22 2019-08-01 株式会社ディスコ ウエーハの生成方法およびウエーハの生成装置
CN114720318A (zh) * 2022-04-24 2022-07-08 华中科技大学 热失重自动化检测装置及系统
CN115236198A (zh) * 2022-07-22 2022-10-25 中交七鲤古镇(赣州)文化旅游有限公司 陶瓷制品微裂纹检测方法
US20220373514A1 (en) * 2021-05-13 2022-11-24 Idkorea Co., Ltd. Method for locating fault using acoustic emission signal
CN117233028A (zh) * 2023-11-13 2023-12-15 陕西三义高科石墨新材料有限公司 一种石墨坩埚检测装置
TWI839915B (zh) * 2022-09-27 2024-04-21 大陸商西安奕斯偉材料科技股份有限公司 用於晶圓表面微損傷的檢測方法和檢測系統
JP2024530248A (ja) * 2021-08-18 2024-08-16 ジルトロニック アクチエンゲゼルシャフト 単結晶シリコンからエピタキシャルコーティングされた半導体ウェハを製造する方法
KR20250045676A (ko) 2023-09-26 2025-04-02 에스디티 주식회사 도가니의 박리 및 크랙 검출 방법

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JP2019129174A (ja) * 2018-01-22 2019-08-01 株式会社ディスコ ウエーハの生成方法およびウエーハの生成装置
JP7046617B2 (ja) 2018-01-22 2022-04-04 株式会社ディスコ ウエーハの生成方法およびウエーハの生成装置
US20220373514A1 (en) * 2021-05-13 2022-11-24 Idkorea Co., Ltd. Method for locating fault using acoustic emission signal
JP2024530248A (ja) * 2021-08-18 2024-08-16 ジルトロニック アクチエンゲゼルシャフト 単結晶シリコンからエピタキシャルコーティングされた半導体ウェハを製造する方法
CN114720318A (zh) * 2022-04-24 2022-07-08 华中科技大学 热失重自动化检测装置及系统
CN114720318B (zh) * 2022-04-24 2024-04-12 华中科技大学 热失重自动化检测装置及系统
CN115236198A (zh) * 2022-07-22 2022-10-25 中交七鲤古镇(赣州)文化旅游有限公司 陶瓷制品微裂纹检测方法
TWI839915B (zh) * 2022-09-27 2024-04-21 大陸商西安奕斯偉材料科技股份有限公司 用於晶圓表面微損傷的檢測方法和檢測系統
KR20250045676A (ko) 2023-09-26 2025-04-02 에스디티 주식회사 도가니의 박리 및 크랙 검출 방법
CN117233028A (zh) * 2023-11-13 2023-12-15 陕西三义高科石墨新材料有限公司 一种石墨坩埚检测装置
CN117233028B (zh) * 2023-11-13 2024-01-16 陕西三义高科石墨新材料有限公司 一种石墨坩埚检测装置

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