US20210395097A1 - Polysilicon rod and method for manufacturing polysilicon rod - Google Patents

Polysilicon rod and method for manufacturing polysilicon rod Download PDF

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US20210395097A1
US20210395097A1 US17/353,509 US202117353509A US2021395097A1 US 20210395097 A1 US20210395097 A1 US 20210395097A1 US 202117353509 A US202117353509 A US 202117353509A US 2021395097 A1 US2021395097 A1 US 2021395097A1
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grain boundary
coincidence
polysilicon
polysilicon rod
length
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Atsushi Yoshida
Naruhiro Hoshino
Masahiko Ishida
Takeshi Aoyama
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Shin Etsu Chemical Co Ltd
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Shin Etsu Chemical Co Ltd
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Assigned to SHIN-ETSU CHEMICAL CO., LTD. reassignment SHIN-ETSU CHEMICAL CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AOYAMA, TAKESHI, HOSHINO, Naruhiro, ISHIDA, MASAHIKO, YOSHIDA, ATSUSHI
Priority to US18/479,801 priority Critical patent/US20240025754A1/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/60—Compounds characterised by their crystallite size
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
    • 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

Definitions

  • the present invention relates to raw polysilicon for improving the defect rate in the manufacture of single crystal and a method for manufacturing the same.
  • the manufacturing process of single crystal silicon is required to control impurities, lattice defects, etc., and maintain productivity.
  • Examples of the currently mainstream method for manufacturing single crystal include a floating zone (FZ) method and a Czochralski (CZ) method.
  • FZ floating zone
  • CZ Czochralski
  • the FZ method is a method of directly heating a polysilicon rod by high-frequency heating to obtain single crystal, which has more features favorable for controlling impurities than the CZ method using a quartz crucible.
  • a defect in the FZ method means that single crystal growth is inhibited and dislocation occurs, and a crystal defect is caused in a single crystal rod.
  • One of the factors that inhibit the single crystal growth is a phenomenon in which polysilicon is left unmelted to cause the defect.
  • the crystal characteristics of the raw polysilicon rod used are greatly associated with the defect in the FZ that occurs during the manufacture of single crystal.
  • Manufacture of polysilicon rods as a raw material in the FZ method is mainly performed by a Siemens method that is a CVD method in which silane gas as a raw material is precipitated on a heated silicon rod in the air.
  • JP 2008-285403 A, JP 2013-193902 A, JP 2014-28747 A, and JP 2017-197431 A discloses a polysilicon rod characterized by its acicular crystal, area ratio of coarse grains, and size of a crystal grain.
  • JP 2013-217653 A, JP 2015-3844 A, and JP 2016-150885 A discloses a method for selecting a single crystal raw material according to the peak intensities and the numbers of peaks of Miller indices ⁇ 111> and ⁇ 220> by an X-ray diffraction method.
  • JP 2019-19010 A discloses a polysilicon rod characterized by the size of a crystal grain and the diffraction intensity of a Miller index ⁇ 222> by an X-ray diffraction method.
  • the present invention provides a polysilicon rod in which the single crystallization defect in the FZ method is reduced by the ratio of the breadth of a grain boundary surface to coincidence grain boundary, which is a feature of a grain boundary that is a boundary surface between particles.
  • a silicon rod having the largest crystal grain is a single crystal silicon rod, and when a model in which this single crystal silicon rod is single-crystallized by the FZ method is considered, it can be said that the defect rate due to the raw material is zero.
  • this single crystal is divided, a grain boundary surface appears.
  • a coincidence grain boundary closest to a single crystal bond is ⁇ 3
  • a grain boundary surface having no coincidence lattice point or having no regularity is a random grain boundary. It can be said that a grain boundary containing a large amount of ⁇ 3 that is a bonding surface closest to single crystal is close to single crystal.
  • a reactor for performing a CVD reaction by the Siemens method is generally a bell jar type.
  • the inner wall of a reactor receives radiation from a heated rod.
  • the reflectance is high and an effect of returning the radiant energy from the rod to the rod can be obtained, but when the inner wall is fogged, the reflectance is decreased, so that the absorption of the energy into the wall surface is increased and the energy is not returned to the rod.
  • the cause of the fogging is that chlorosilanes as a raw material cause hydrolysis with the moisture in the air when the reactor is opened between batches, so that the reflectance tends to be decreased with each batch.
  • Polysilicon having a desired grain boundary can be manufactured by feeding back the grain boundary characteristics of the previous batch to the reaction conditions of the next batch.
  • An inhibitor for single crystallization by the FZ method is included in the characteristics of a grain boundary surface, and by measuring and analyzing it, and feeding back to the manufacturing conditions, polysilicon rods suitable for single crystallization by the FZ method can be manufactured.
  • an area near the center of a polysilicon rod is easily affected by a grain boundary because it reaches a single crystal growth surface immediately after being melted, while an area near the outer periphery of the polysilicon rod is less affected than the area near the center because it passes through a heating zone by an induced current.
  • an area having a small random grain boundary length and a large grain boundary length is favorable, and as the distance from the center becomes larger, even an area having a smaller grain boundary length becomes acceptable.
  • the rod containing polysilicon is beneficial, in which in an area whose distance from the center of the cross section of the polysilicon rod is within 2 ⁇ 3 of the radius and that excludes the seed core, the average coincidence grain boundary ratio exceeds 20%, the average grain boundary length exceeds 550 mm/mm 2 , and the average random grain boundary length does not exceed 800 mm/mm 2 . Further, the polysilicon rod is favorable, in which the coincidence grain boundary ratio exceeds 25%, the grain boundary length exceeds 650 mm/mm 2 , and the random grain boundary length does not exceed 700 mm/mm 2 .
  • the rod containing polysilicon is beneficial, in which in an area including the entire polysilicon rod but the seed core, the average coincidence grain boundary ratio exceeds 20%, the average grain boundary length exceeds 550 mm/mm 2 , and the average random grain boundary length does not exceed 800 mm/mm 2 . Further, the polysilicon rod is favorable, in which the coincidence grain boundary ratio exceeds 25%, the grain boundary length exceeds 650 mm/mm 2 , and the random grain boundary length does not exceed 700 mm/mm 2 .
  • the grain boundary length is intended to be increased, it is also necessary to increase the coincidence grain boundary ratio in order to reduce the random grain boundary length to 700 mm/mm 2 or less, so that it is realistic from the above reason that the grain boundary length is 3000 mm/mm 2 or less.
  • the environment inside a reactor gradually changes as described above. Therefore, it is considered that polysilicon is analyzed at constant intervals and the results are fed back to the CVD conditions.
  • the coincidence grain boundary ratio that is a feature of a grain boundary, the grain boundary length that is an index of the breadth of a grain boundary, and the random grain boundary length obtained from them are quantitative values and characterized by being able to be associated with manufacturing conditions.
  • the grain boundary characteristics from the inner periphery to the outer periphery of a polysilicon rod can be controlled, so that polysilicon rods according to the requirements of customers can be provided.
  • the defect rate in single crystallization by the FZ method can be reduced, and the yield and productivity can be improved, and
  • polysilicon rods can be stably manufactured by feedback from the grain boundary characteristics to the manufacturing conditions.
  • FIG. 1 is a graph showing the relationship between a grain boundary length and a coincidence grain boundary ratio
  • FIG. 2 is a graph showing the relationship between a grain boundary length and a ⁇ 3 coincidence grain boundary ratio
  • FIG. 3A is a view showing images of ⁇ 3 coincidence grain boundaries
  • FIG. 3B is a view showing images of ⁇ 9 coincidence grain boundaries
  • FIG. 3C is a view showing images of random grain boundaries, and ⁇ 3 to 49 coincidence grain boundaries
  • FIG. 4 is a schematic view for explaining the outline of a measurement method 1 in an embodiment of the present invention.
  • FIG. 5 is a schematic view for explaining the outline of a measurement method 2 in the embodiment of the present invention.
  • a horizontal plane orthogonal to the growth direction of a polysilicon rod is cut out, and the crystal orientations of the crystal grains exposed on a measurement surface are entirely measured at an electron backscatter diffraction (EBSD) step of 1 ⁇ m, whereby the state of a grain boundary is calculated from differences between the orientations/angles of adjacent crystals of the obtained data matrix.
  • EBSD electron backscatter diffraction
  • a ⁇ 3 coincidence grain boundary means a grain boundary surface where one coincidence lattice point appears with respect to three atoms, which can be said to be a grain boundary surface closest to single crystal among coincidence grain boundaries. It can be said that when a grain boundary has more coincidence lattice points, the thermal and physical properties of the grain boundary are closer to those of single crystal.
  • the ⁇ 3 to 49 detected using an EBSD analysis software are defined as coincidence grain boundaries. About 80% of all the coincidence grain boundaries of ⁇ 3 to 49 are occupied by ⁇ 3 and ⁇ 9, in which ⁇ 3 is slightly more than ⁇ 9. As the ⁇ value becomes larger, the interval between coincidence lattice points becomes larger, which becomes closer to a random grain boundary. Therefore, in the present embodiment, a coincidence grain boundary ratio is calculated by using the sum of ⁇ 3 to ⁇ 9 coincidence grain boundaries, which is adopted as an index.
  • ⁇ 1 means single crystal.
  • the grain boundary is a boundary between grains, it is obtained as a surface when surface observation is performed, so that the grain boundary is indicated as an area.
  • the information obtained by a measurement using an actual apparatus becomes a line (becomes the length of a boundary line around when surface observation is performed).
  • the coincidence grain boundary ratio is defined as follows (see FIGS. 3A to 3C ):
  • coincidence grain boundary ratio (%) boundary lines of observed coincidence grain boundaries/boundary lines of observed grain boundaries.
  • the boundary lines include boundary lines exceeding ⁇ 49.
  • the “boundary lines of observed grain boundaries” in the above expression are all the grain boundaries observed by the above EBSD analysis software. In the present embodiment, the “ ⁇ 3 to 49” are referred to as coincidence grain boundaries as described above. The boundary lines in the coincidence grain boundaries are about 50 to 60% of the “boundary lines of observed grain boundaries.”
  • the orientations (angles) of crystals on an observation surface are measured at intervals of, for example, 1 ⁇ m in the case of ⁇ 150.
  • a grain boundary When there is a difference of a certain angle or more in the changes in the obtained continuous data, it is regarded as a grain boundary.
  • the coincidence grain boundaries of “ ⁇ 3 to 49” can be obtained from the orientations and directions of the crystals with the grain boundary interposed therebetween.
  • boundary lines of observed grain boundaries >boundary lines of “ ⁇ 3 to 49 coincidence grain boundaries”>boundary lines of “ ⁇ 3 to ⁇ 9 coincidence grain boundaries”.
  • the boundary lines of observed grain boundaries include the coincidence grain boundaries and grain boundaries that are not the coincidence grain boundaries. Therefore, the coincidence grain boundary ratio is obtained by dividing the sum of the boundary lines of “ ⁇ 3 to ⁇ 9 coincidence grain boundaries” by the sum of the boundary lines of “ ⁇ 3 to 49 grain boundaries” and the boundary lines exceeding ⁇ 49.
  • a grain boundary having a low coincidence lattice point density (a grain boundary close to a random grain boundary) has high energy and is unstable. Therefore, when there are many grain boundaries each having a low coincidence lattice point density, it triggers falling off of unmelted particles on an FZ melt surface, causing an FZ defect.
  • a polysilicon rod having physical properties close to those of single crystal is used as a raw material in the FZ method, stable melting can be obtained.
  • a grain boundary surface cannot currently be determined by images of SEM or the like.
  • the length of a grain boundary on the measurement surface can be obtained, so that the average size of particles can be indirectly expressed.
  • a grain boundary length per unit area can be obtained. In the present embodiment, this is defined as a grain boundary length (unit: length/area) that is an index of the breadth of a grain boundary surface.
  • Various coincidence grain boundaries are included in the grain boundaries other than the ⁇ 3 to ⁇ 9 coincidence grain boundaries.
  • the interval between the coincidence lattice points becomes larger, so that the features of a grain boundary having a low ⁇ value (having low grain boundary energy and being stable) are lost. Therefore, the sum of ⁇ s larger than ⁇ 9 is defined as a random grain boundary, for convenience, and a random grain boundary length is determined from the grain boundary length per unit area. That is, when the sum of the length of grain boundaries which have ⁇ s larger than ⁇ 9 on the measurement surface is divided by the measured area, a random grain boundary length per unit area can be obtained.
  • the coincidence grain boundary ratio and the grain boundary length are in a contradictory relationship for the most part.
  • the polysilicon manufactured under the condition of increasing the coincidence grain boundary ratio its grain boundary length is small. Therefore, it is important to find the best point for both the grain boundary characteristics.
  • the cause of the falling off of crystal particles, which inhibits single crystal growth, is that the bonding at a grain boundary surface is weak and unstable. As the number of random grain boundaries with less bonding of coincidence lattice points becomes larger, peeling off and falling off from the melt surface are more likely to occur. It can be said that when of the grain boundary characteristics, the ⁇ value is small and the coincidence grain boundary ratio is large, the bonding at a grain boundary surface is strong and stable, so that the falling off of crystal particles is less likely to occur.
  • the falling off of crystal particles due to a random grain boundary occurs at a temperature lower than the melting temperature of the single crystal because the energy at the grain boundary surface is high.
  • the single crystal particles that have fallen off are not sufficiently heated and melted, and reach the single crystal growth surface while the unmelted and semi-melted particles are in a cluster form, causing a crystal defect.
  • the unmelted and semi-melted particles depend on the sizes of the crystal particles that have fallen off. The larger the size is, the longer the existence time is, so that they are more likely to reach the single crystal growth surface.
  • an aspect (hereinafter, also referred to as a “measurement method 1”) as shown in FIG. 4 may be used.
  • the prepared silicon rod is cut at arbitrary positions (three positions in the aspect shown in FIG. 4 ) and sliced, whereby samples are cut out. The samples thus obtained are measured. Since the characteristics of both the feet of a U-rod are basically the same, the measurement may be performed only on one foot.
  • the measurement results show that in all the cut-out samples, the yield in the FZ becomes good according to the following conditions in which: in an area whose distance from the center of the cross section of the polysilicon rod is within 2 ⁇ 3 of the radius and that excludes the seed core, the average coincidence grain boundary ratio exceeds 20%, the average grain boundary length exceeds 550 mm/mm 2 , and the average random grain boundary length does not exceed 800 mm/mm 2 ; or in an area including the entire polysilicon rod but the seed core, the average coincidence grain boundary ratio exceeds 20%, the average grain boundary length exceeds 550 mm/mm 2 , and the average random grain boundary length does not exceed 800 mm/mm 2 .
  • products with a good yield can be manufactured when the FZ is performed by using the foot that has not been cut out into slices in FIG. 4 .
  • the foot, from which the sliced samples are obtained in FIG. 4 may be used as a chunk for the CZ.
  • Measurement is performed using the measurement method 1, and the foot, which is opposite to the foot that has passed by meeting the above conditions, is subjected to single crystal growth by the FZ (if the manufacturing apparatus is of the same type, one is regarded as a representative.).
  • the measurement method 1 may be performed on every silicon rod in the same chamber that has grown into a silicon core wire, and if they pass by meeting the above conditions, the foot, which is opposite to the foot that has passed, may be subjected to single crystal growth by the FZ;
  • the measurement method 1 may be performed on a representative of those outside the chamber, like the representative of those inside the chamber, and if it passes by meeting the above conditions, the rest of those may be subjected to single crystal growth by the FZ; or
  • one representative may be measured by the measurement method 1, and if it passes by meeting the above conditions, the rest may be subjected to single crystal growth by the FZ.
  • a rod for the FZ can also be acquired in the foot from which the samples have been made.
  • a sample for quality evaluation is taken from a portion outside the effective length of the ingot for the FZ, mainly from the vicinity of the electrode. The sample is analyzed to determine a resistance value, metal components, etc.
  • the following procedure can be taken.
  • a foot is measured by the measurement method 2, and the foot, which has passed by meeting the above conditions, and its opposite foot are both subjected to single crystal growth by the FZ (if the manufacturing apparatus is of the same type, one is regarded as a representative.).
  • the measurement method 2 may be performed on a representative of those outside the chamber, like the representative of those inside the chamber, and if it passes by meeting the above conditions, all of the those may be subjected to single crystal growth by the FZ method; or
  • one presentative may be measured by the measurement method 2, and if it passes by meeting the above conditions, all may be subjected to single crystal growth by FZ.
  • either of the measurement methods 1 and 2 may be performed in each apparatus.
  • the manufacturing conditions may be continuously reviewed, or the inside of the bell jar may be cleaned to return to the initial state.
  • electropolishing is performed to clean the inside of the bell jar, the cost is highly expensive. Therefore, it is a realistic choice to continue to review the manufacturing conditions.
  • a crystal sample was prepared by the Siemens method using trichlorosilane and hydrogen as raw materials, the grain boundary characteristics were measured by EBSD, and the results of actual pull-out experiments by the FZ method are shown below.
  • Wafers each having a thickness of 10 mm were cut out from both ends of an effective length (the electrode side and the bridge side were removed) of a U rod taken out from a Siemens method CVD apparatus (see FIG. 5 ).
  • a line segment a was drawn from the outer periphery to the seed core of the wafer, the line segment a bisecting, on the acute angle side, the angle formed between lines that are drawn to extend from the outer periphery to the seed core of the wafer in a portion where the line is the largest and a portion where the line is shortest.
  • reaction conditions Facts that affect a grain boundary, such as the temperature of a rod, reaction pressure, raw material concentration, raw material supply speed, CVD apparatus, and radiant heat that a rod receives from outside
  • reaction conditions factors that affect a grain boundary, such as the temperature of a rod, reaction pressure, raw material concentration, raw material supply speed, CVD apparatus, and radiant heat that a rod receives from outside
  • An example is taken, in which: in an apparatus for manufacturing polysilicon by the Siemens method, the apparatus having a function of keeping a constant temperature by generating heat by making a current flow through the seed core of the polysilicon that is connected to the electrode, and the gas phase portion of the apparatus being filled with hydrogen and chlorosilane, a deposited layer of polysilicon is formed on the surface of the seed core of heated silicon, thereby forming a polysilicon rod.
  • the temperature of the surface of the rod is relatively raised in order to increase a region where the coincidence grain boundary ratio is increased when the diameter is small, while the temperature of the surface of the silicon rod is made lower and the chlorosilane concentration is made higher (to prevent the heat inside the silicon rod from rising) in order to increase the grain boundary length as the diameter becomes larger.
  • a polysilicon rod having a “proper region” can be manufactured.

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
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US17/353,509 2020-06-23 2021-06-21 Polysilicon rod and method for manufacturing polysilicon rod Abandoned US20210395097A1 (en)

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US20140004377A1 (en) * 2012-06-29 2014-01-02 Mitsubishi Materials Corporation Polycrystalline silicon rod

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JP4887504B2 (ja) * 2005-07-04 2012-02-29 国立大学法人東北大学 粒界性格制御多結晶の作製方法
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JP5969230B2 (ja) * 2012-03-16 2016-08-17 株式会社トクヤマ 多結晶シリコンロッド
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
JP5947248B2 (ja) 2013-06-21 2016-07-06 信越化学工業株式会社 多結晶シリコン棒の選択方法
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JP6969917B2 (ja) 2017-07-12 2021-11-24 信越化学工業株式会社 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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US20140004377A1 (en) * 2012-06-29 2014-01-02 Mitsubishi Materials Corporation Polycrystalline silicon rod

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