WO2018163726A1 - 単結晶シリコン中の炭素濃度測定方法 - Google Patents

単結晶シリコン中の炭素濃度測定方法 Download PDF

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Publication number
WO2018163726A1
WO2018163726A1 PCT/JP2018/004987 JP2018004987W WO2018163726A1 WO 2018163726 A1 WO2018163726 A1 WO 2018163726A1 JP 2018004987 W JP2018004987 W JP 2018004987W WO 2018163726 A1 WO2018163726 A1 WO 2018163726A1
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Prior art keywords
silicon
carbon concentration
single crystal
concentration
carbon
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PCT/JP2018/004987
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English (en)
French (fr)
Japanese (ja)
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清隆 高野
雅紀 高沢
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信越半導体株式会社
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Priority to CN201880007837.5A priority Critical patent/CN110199057B/zh
Priority to KR1020197022361A priority patent/KR102447217B1/ko
Publication of WO2018163726A1 publication Critical patent/WO2018163726A1/ja

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    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light

Definitions

  • the present invention relates to a method for measuring carbon concentration in single crystal silicon, and more particularly, to a method for measuring a low carbon concentration that cannot be measured by FT-IR in a silicon single crystal manufactured by the Czochralski method.
  • a silicon single crystal substrate widely used as a substrate for semiconductor devices contains carbon as an impurity. Carbon is mixed in the manufacturing process of the silicon single crystal, and may be further mixed in the wafer processing process, the epitaxial growth process, and the device manufacturing process.
  • Carbon in a silicon single crystal normally exists at a lattice position of silicon (carbon existing at the lattice position is called substitutional carbon), and itself is electrically inactive. However, when it is ejected to the interstitial position by ion implantation or heat treatment in the device process (carbon existing at the interstitial position is called interstitial carbon), it reacts with other impurities to form a composite. Becomes active and adversely affects device characteristics.
  • infrared absorption spectroscopy As a method of measuring the concentration of carbon contained in a silicon substrate, infrared absorption spectroscopy (FT-IR) is widely used (for example, Patent Document 1).
  • FT-IR infrared absorption spectroscopy
  • infrared rays are transmitted through a silicon substrate, and the carbon concentration is measured from the intensity of the local vibration absorption peak due to substitutional carbon.
  • the difference absorption spectrum obtained by taking the difference between the infrared absorption spectrum of the sample to be measured and the infrared absorption spectrum of the reference sample that can be regarded as substantially carbon-free.
  • the carbon concentration is quantified from the intensity of the local vibrational absorption peak due to substitutional carbon appearing in the vicinity of 605 cm ⁇ 1 , and as shown in Non-Patent Document 3, the carbon concentration is generally measured by FT-IR.
  • the lower limit of detection is said to be 1 to 2 ⁇ 10 15 atoms / cm 3, and the silicon single crystals currently mass-produced are generally below the lower limit of detection.
  • a sample is irradiated with an electron beam, an ion beam of carbon ions or oxygen ions to generate a composite defect, and the photoluminescence intensity resulting from the composite defect is measured using a low-temperature PL apparatus.
  • strength is disclosed (for example, patent document 2, nonpatent literature 1).
  • the luminescence intensity derived from silicon and the luminescence intensity of defects derived from carbon are obtained by a photoluminescence method, and the intensity and a calibration curve prepared in advance are used.
  • a method for measuring the carbon concentration is disclosed (Patent Document 3, Non-Patent Document 2).
  • C s substitutional carbon
  • C i interstitial carbon
  • O i interstitial oxygen
  • Non-Patent Document 3 shows that the intensity of CiCs-related luminescence changes reflecting the carbon concentration even below the FT-IR detection limit, and carbon-related luminescence is sufficiently detected even in the single crystal head with the lowest carbon concentration. I knew it was possible.
  • the intensity change of the light emission related to C i O i is smaller than the light intensity change related to C i C s .
  • the reason for this is simply considered when C i C s 2 carbon, C i O i is due to hold from 1 carbon, better utilizing the change in intensity of G-line is large intensity variation relative to the carbon concentration, when the concentration quantitatively It turns out that it is easy to handle as a peak to be used.
  • the C-line becomes dominant when the oxygen concentration in the crystal is high (Non-patent Document 3), in order to quantify the carbon concentration with high sensitivity by the photoluminescence method, measurement is performed with a sample with a reduced oxygen concentration. There was a problem that had to be done.
  • the present invention has been made in view of the above problems, and can measure a low carbon concentration that cannot be measured by FT-IR even if the silicon concentration of the product portion exceeds 5 ppma-JEIDA.
  • An object of the present invention is to provide a method for measuring carbon concentration in single crystal silicon.
  • the present invention is a method for measuring the carbon concentration of a silicon single crystal pulled by a Czochralski method from a silicon melt to which a horizontal magnetic field is applied, wherein the oxygen concentration is 5 ppma-JEIDA or less.
  • the test sample is cut out from the rounded region of the silicon single crystal and the carbon concentration of the test sample is measured by low-temperature PL measurement, so that the measurement lower limit of the carbon concentration is 5 ⁇ 10 14 atoms / cm 3 or less.
  • There is provided a carbon concentration measurement method in single crystal silicon wherein the carbon concentration in a straight body of the silicon single crystal is calculated.
  • the test sample is cut out from the rounded region where the oxygen concentration is 5 ppma-JEIDA or less, and the carbon concentration of the test sample is measured to measure the carbon concentration with a measurement lower limit of 5 ⁇ 10 14 atoms / cm 3 or less.
  • the carbon concentration of the product part (straight barrel part) is calculated from the segregation coefficient, so that the oxygen concentration of the product part is adjusted to a high value according to customer requirements, while the low concentration of carbon. Concentration measurement is possible. For this reason, it is not necessary to separately manufacture a product part with a reduced oxygen concentration and measure the carbon concentration, thereby improving the production efficiency and increasing the reliability of the measured value.
  • the oxygen concentration in the straight body of the silicon single crystal can exceed 5 ppma-JEIDA.
  • the present invention can be suitably applied to such a silicon single crystal having a high oxygen concentration in the straight body.
  • the magnetic flux density at the magnetic field center of the horizontal magnetic field is 2000 Gauss or more, and the silicon melt is accommodated.
  • the crucible rotation speed is preferably 1 rpm or less.
  • the magnetic flux density at the center of the horizontal magnetic field to 2000 Gauss or more and the rotational speed of the crucible containing the silicon melt to 1 rpm or less
  • the convection of the silicon melt is sufficiently suppressed, and the melt surface Due to the acceleration of evaporation, the oxygen concentration at the surface of the silicon melt near the crystal is lowered.
  • the rotation of the crucible containing the silicon melt is 1 rpm or less
  • the concentration of oxygen eluted from the quartz crucible decreases, and particularly the oxygen concentration near the free surface of the melt (silicon melt) decreases.
  • the oxygen concentration inside can be reliably reduced.
  • the inspection sample is cut out from a region where the area ratio of the crystal cross section to the free surface of the silicon melt is 1% or less during crystal pulling.
  • the area ratio of the free surface of the melt (silicon melt) with respect to the cross-sectional area of the crystal increases, so that more SiO evaporates from the melt surface, and the melt surface near the crystal
  • the oxygen concentration contained further decreases.
  • the area ratio of the crystal cross section to the free surface of the silicon melt is 1% or less, the degree of influence on the melt convection due to the crystal rotation becomes small even if the crystal rotation speed is about the same as the product part.
  • the low oxygen melt on the free surface of the melt is easily taken into the crystal, the low oxygen concentration crystal can be obtained more reliably, so the lower limit of carbon concentration detection by low-temperature PL measurement can be further reduced. It becomes.
  • the oxygen concentration in single crystal silicon of the present invention even if the silicon concentration of the product part (straight body part) exceeds 5 ppma-JEIDA, the oxygen concentration is 5 ppma-
  • a carbon concentration measurement of 5 ⁇ 10 14 atoms / cm 3 or lower is possible.
  • the carbon concentration of the product part (straight body part) can be calculated from the measurement result using the segregation coefficient, and the carbon concentration of the product part of single crystal silicon can be accurately measured.
  • FT-IR is widely used as a method for measuring the concentration of carbon contained in a silicon substrate.
  • the lower limit of detection of carbon concentration measurement by FT-IR is a silicon single crystal that is currently mass-produced. Then, it was almost below the lower limit of detection.
  • the luminescence intensity derived from silicon and the luminescence intensity of defects derived from carbon are obtained by a photoluminescence method, and these intensities are prepared in advance.
  • a method for measuring a carbon concentration using a calibration curve is disclosed.
  • the present inventors have found that in a single crystal silicon that can measure a low concentration of carbon that cannot be measured by FT-IR even if the oxygen concentration of the product part (straight barrel part) exceeds 5 ppma-JEIDA.
  • the carbon concentration measurement method was studied earnestly.
  • the present inventors cut out a test sample from the rounded region of the silicon single crystal having an oxygen concentration of 5 ppma-JEIDA or less, measured the carbon concentration of the test sample by the low-temperature PL method, and directly calculated this measurement result.
  • the carbon concentration in the barrel we found that even if it is a silicon single crystal in which the oxygen concentration in the straight barrel exceeds 5 ppma-JEIDA, a low concentration of carbon that cannot be measured by FT-IR can be measured. Completed the invention.
  • FIG. 1 is a flowchart showing an example of an embodiment of a method for measuring carbon concentration in single crystal silicon according to the present invention.
  • a silicon single crystal pulled up by a Czochralski method from a silicon melt to which a horizontal magnetic field is applied is prepared (see S11 in FIG. 1).
  • the silicon single crystal pulled up by the Czochralski method includes a straight body portion having a substantially constant diameter for products and a reduced diameter portion called a rounded portion.
  • a test sample is cut out from the region of the rounded portion of the silicon single crystal having an oxygen concentration of 5 ppma-JEIDA or less (see S12 in FIG. 1).
  • the rounded part which is a reduced diameter part, is smaller in diameter than the straight body part, and the area ratio of the free surface of the silicon melt that is the raw material contained in the crucible to the cross-sectional area of the crystal is compared with the straight body part. Therefore, the amount of SiO evaporated from the silicon melt surface increases, and the oxygen concentration contained in the silicon melt surface portion in the vicinity of the crystal is lower than that of the straight body portion.
  • a test sample is cut out from a region having a small diameter where the oxygen concentration is 5 ppma-JEIDA or less in the rounded portion of the silicon single crystal where the oxygen concentration is lower than that of the straight body portion.
  • the carbon concentration of the test sample is measured by low-temperature PL measurement, and the measurement lower limit value of the carbon concentration is set to 5 ⁇ 10 14 atoms / cm 3 or less (see S13 in FIG. 1).
  • this is an emission line derived from C i O i
  • the intensity change with respect to the carbon concentration Is a light emission line derived from C i C s and can be treated as a peak used for concentration determination, because it is a light emission line derived from C i C s.
  • the lower limit value can be 5 ⁇ 10 14 atoms / cm 3 or less.
  • the test sample is cut out from the rounded region where the oxygen concentration is 5 ppma-JEIDA or less, and the carbon concentration of the test sample is measured to measure the carbon concentration with a measurement lower limit of 5 ⁇ 10 14 atoms / cm 3 or less.
  • the oxygen concentration in the straight body of the silicon single crystal can exceed 5 ppma-JEIDA.
  • the present invention can be suitably applied to such a silicon single crystal having a high oxygen concentration in the straight body.
  • the magnetic flux density at the center of the horizontal magnetic field is 2000 Gauss or more at least during the step of forming the round portion of the silicon single crystal when pulling up the silicon single crystal.
  • the rotational speed of the crucible which accommodates a silicon melt shall be 1 rpm or less.
  • the rotation of the crucible containing the silicon melt is 1 rpm or less, the concentration of oxygen eluted from the quartz crucible decreases, and particularly the oxygen concentration near the free surface of the melt (silicon melt) decreases.
  • the oxygen concentration inside can be reliably reduced.
  • the test sample is preferably cut out from a region where the area ratio of the crystal cross section to the free surface of the silicon melt is 1% or less during crystal pulling.
  • the area ratio of the free surface of the melt (silicon melt) with respect to the cross-sectional area of the crystal increases, so that more SiO evaporates from the melt surface, and the melt surface near the crystal The oxygen concentration contained further decreases.
  • the area ratio of the crystal cross section to the free surface of the silicon melt is 1% or less, the degree of influence on the melt convection due to the crystal rotation becomes small even if the crystal rotation speed is about the same as the product part.
  • the low oxygen melt on the free surface of the melt is easily taken into the crystal, a crystal with a lower oxygen concentration can be obtained, so that the lower limit of carbon concentration detection by low-temperature PL measurement can be further reduced. .
  • Each of the silicon single crystals obtained as described above was appropriately cut, and a sample was cut out from the straight body portion, and the oxygen concentration was measured. Furthermore, after the sample was polished, it was irradiated with an electron beam, and the carbon concentration was measured with a low-temperature PL apparatus. Table 1 shows to what level the carbon concentration can be detected at each oxygen concentration.
  • Example 1 Among the silicon single crystals of the experimental example, the vertical sample was taken from the rounded portion of the silicon single crystal in which the oxygen concentration in the straight body portion was 10 ppma-JEIDA (sample 1) and 14 ppma-JEIDA (sample 2). Cutting out and measuring the oxygen concentration along the central axis. The measurement results are shown in FIG. As a result, it was found that the oxygen concentration gradually decreased as the crystal diameter decreased from the straight body portion, and then all of them rapidly decreased when the rounding length was around 170 mm (see FIG. 2). In FIG. 2, the horizontal axis is the crystal cross-sectional area ratio with respect to the melt free surface, and FIG.
  • the effect of the crystal diameter is considered to be that the concentration of oxygen taken into the crystal decreases because the SiO cross-sectional area with respect to the free surface of the melt decreases and the SiO evaporated from the free surface of the melt increases.
  • a product part (straight body part) with a diameter of 306 mm is pulled up from an 800 mm crucible and then a rounded part is formed, if the rounded part has a crystal diameter of about 80 mm or more, silicon convection in the melt is transported due to the effect of crystal rotation. Therefore, since the oxygen concentration taken into the crystal is also affected, it is difficult to reliably obtain a sample having an oxygen concentration of 5 ppma-JEIDA or lower.
  • the present invention it is possible to eliminate the influence of oxygen concentration due to crystal rotation by cutting the inspection sample from a region where the ratio of the crystal cross section to the melt free surface is 1% or less, and the crystal rotation speed is changed.
  • a sample with an oxygen concentration of 5 ppma-JEIDA or less can be collected stably, a sample with a low oxygen concentration of 5 ppma-JEIDA or less can be reliably collected, and measurement with a low-temperature PL apparatus is possible. (See FIG. 3).
  • Example 2 400 kg of silicon polycrystalline material was charged, and the pulling was started in the same manner as in the experimental example. A rounded portion was created from a portion of the straight body of 150 cm, and a measurement sample A was cut out from a portion of 190 mm from the start of rounding (FIG. 2, 3).
  • the pulling conditions were such that the oxygen concentration in the straight body portion was 10 ppma-JEIDA.
  • the oxygen concentration of the measurement sample A was measured, the oxygen concentration of the measurement sample A was 1 ppma-JEIDA.
  • carbon concentration of the measurement sample A was implemented by low-temperature PL measurement, the carbon concentration of the measurement sample A was 2 ⁇ 10 13 atoms / cm 3 .
  • Example 2 since the measurement sample was cut out from the rounded part of 1 ppma-JEIDA where the oxygen concentration was 5 ppma-JEIDA or less, the carbon concentration could be measured by low-temperature PL measurement. On the other hand, in the comparative example, since the measurement sample was cut out from the rounded part of 6 ppma-JEIDA where the oxygen concentration exceeded 5 ppma-JEIDA, the carbon concentration could not be detected even in the low temperature PL measurement.
  • the carbon concentration in the straight body could be calculated as shown in FIG.
  • the carbon concentration of the measurement sample B of the comparative example could not be detected, the carbon concentration was assumed to be 5 ⁇ 10 13 atoms / cm 3 (see Table 1), which is the lower limit of detection in the oxygen concentration of 6 ppma-JEIDA.
  • the concentration in the straight body is assured with a value including a value nearly twice that of the measurement sample A of Example 2.
  • the present invention is not limited to the above embodiment.
  • the above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.

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PCT/JP2018/004987 2017-03-06 2018-02-14 単結晶シリコン中の炭素濃度測定方法 WO2018163726A1 (ja)

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JP2013152977A (ja) * 2012-01-24 2013-08-08 Mitsubishi Electric Corp 不純物濃度測定方法および不純物濃度測定装置
JP2014199253A (ja) * 2013-03-12 2014-10-23 グローバルウェーハズ・ジャパン株式会社 飽和電圧推定方法及びシリコンエピタキシャルウエハの製造方法
JP2015101529A (ja) * 2013-11-28 2015-06-04 信越半導体株式会社 シリコン単結晶の炭素濃度測定方法
JP2015111615A (ja) * 2013-12-06 2015-06-18 信越半導体株式会社 シリコン単結晶中の炭素濃度評価方法、及び、半導体デバイスの製造方法
JP2015156420A (ja) * 2014-02-20 2015-08-27 信越半導体株式会社 シリコン単結晶中の炭素濃度評価方法及び半導体デバイスの製造方法

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JP2790020B2 (ja) 1992-09-30 1998-08-27 信越半導体株式会社 シリコン単結晶中の置換型炭素濃度の測定方法および自動測定装置
JP5524894B2 (ja) * 2011-04-04 2014-06-18 信越化学工業株式会社 多結晶シリコン中の炭素濃度測定方法
JP5921498B2 (ja) * 2013-07-12 2016-05-24 グローバルウェーハズ・ジャパン株式会社 シリコン単結晶の製造方法
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Publication number Priority date Publication date Assignee Title
JP2013152977A (ja) * 2012-01-24 2013-08-08 Mitsubishi Electric Corp 不純物濃度測定方法および不純物濃度測定装置
JP2014199253A (ja) * 2013-03-12 2014-10-23 グローバルウェーハズ・ジャパン株式会社 飽和電圧推定方法及びシリコンエピタキシャルウエハの製造方法
JP2015101529A (ja) * 2013-11-28 2015-06-04 信越半導体株式会社 シリコン単結晶の炭素濃度測定方法
JP2015111615A (ja) * 2013-12-06 2015-06-18 信越半導体株式会社 シリコン単結晶中の炭素濃度評価方法、及び、半導体デバイスの製造方法
JP2015156420A (ja) * 2014-02-20 2015-08-27 信越半導体株式会社 シリコン単結晶中の炭素濃度評価方法及び半導体デバイスの製造方法

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JP2018145052A (ja) 2018-09-20
KR102447217B1 (ko) 2022-09-26
CN110199057A (zh) 2019-09-03
CN110199057B (zh) 2021-03-16
KR20190119035A (ko) 2019-10-21

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