CN114438585A - Method for producing single crystal and silicon crystal - Google Patents

Method for producing single crystal and silicon crystal Download PDF

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Publication number
CN114438585A
CN114438585A CN202111619103.2A CN202111619103A CN114438585A CN 114438585 A CN114438585 A CN 114438585A CN 202111619103 A CN202111619103 A CN 202111619103A CN 114438585 A CN114438585 A CN 114438585A
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China
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stage
equal
width
temperature
temperature zone
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王双丽
陈俊宏
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Zhonghuan Leading Xuzhou Semiconductor Materials Co ltd
Zhonghuan Advanced Semiconductor Materials Co Ltd
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Xuzhou Xinjing Semiconductor Technology Co Ltd
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Priority to CN202111619103.2A priority Critical patent/CN114438585A/en
Publication of CN114438585A publication Critical patent/CN114438585A/en
Priority to PCT/CN2022/140778 priority patent/WO2023125206A1/en
Priority to TW111149973A priority patent/TWI829486B/en
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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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C30B15/203—Controlling or regulating the relationship of pull rate (v) to axial thermal gradient (G)
    • 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

Abstract

The invention discloses a preparation method of a single crystal and a silicon crystal, wherein the preparation method comprises the following steps: in the equal-diameter growth stage, according to the linear equation Gh＝k*h+G0To obtain GhWherein G is0The temperature gradient at the solid-liquid interface is 35-55K/cm, h is the height of the solid-liquid interface and is 0-10 mm, and G ishThe axial temperature gradient of the crystal bar at the height h from the solid-liquid interface is represented by the unit of K/cm; adjusting the temperature gradient to G in the region from the solid-liquid interface to the reference surfacehWherein the reference surface is an interface 10mm above a solid-liquid interface. According to the method, the axial temperature gradient of the crystal bar in the region from the solid-liquid interface to the reference surface is regulated, so that the point defects in the crystal are fully subjected to convection diffusion and recombination, and the concentrations of free V-type point defects and I-type point defects are reduced.

Description

Method for producing single crystal and silicon crystal
Technical Field
The invention belongs to the field of semiconductors, and particularly relates to a preparation method of a monocrystal and a silicon crystal.
Background
Voronkov provides a V/G theory, specifically, a critical value exists in a CZ crystal growth process of a temperature gradient G ratio of a pulling speed to a pulling direction near a long crystal boundary surface, when the V/G ratio is smaller than the critical value, the concentration of lattice gap type point defects (I type point defects) is higher than that of void type point defects (V type point defects), and excessive I type point defects remain in crystals, so that the crystals are called I-type silicon crystals; when the V/G ratio is larger than a critical value, the concentration of the lattice gap type point defects (I type point defects) is lower than that of the hole type point defects (V type point defects), and excessive V type point defects are remained in the crystal, so that the crystal is called V-type silicon crystal; when the V/G ratio is equal to the critical value, the concentrations of the type I point defects and the type V point defects remaining in the crystal are small, the difference is not large, and the crystal with few point defects grows, namely, the perfect crystal.
However, the V/G value is strictly controlled to be at a critical value, namely the concentrations of the I-type point defect and the V-type point defect at the solid-liquid interface of the long crystal are controlled to be equivalent, and the difficulty is higher.
Therefore, the existing techniques for preparing perfect crystals are yet to be explored.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, an object of the present invention is to provide a method for producing a single crystal and a silicon crystal, which can reduce the concentrations of free V-type point defects and I-type point defects by controlling the temperature gradient in the axial direction of the ingot in the region from the solid-liquid interface to the reference plane to allow sufficient convective diffusion and recombination of point defects in the crystal.
In one aspect of the invention, a method of preparing a crystal is provided. According to an embodiment of the invention, the method comprises:
in the equal-diameter growth stage, according to the linear equation Gh＝k*h+G0To obtain GhWherein G is0The temperature gradient at the solid-liquid interface is 35-55K/cm, h is the height of the solid-liquid interface and is 0-10 mm, and G ishThe axial temperature gradient of the crystal bar at the height h from the solid-liquid interface is represented by the unit of K/cm;
adjusting the temperature gradient to G in the region from the solid-liquid interface to the reference surfacehWherein the reference surface is an interface 10mm above a solid-liquid interface.
According to the preparation method of the crystal, disclosed by the embodiment of the invention, the axial temperature gradient of the crystal bar in the region from the solid-liquid interface to the reference surface is regulated and controlled, so that the I-type point defects and the V-type point defects formed in the crystal growing process are fully diffused and recombined in the region near the solid-liquid interface, and the formation concentration of free point defects is reduced.
In addition, the preparation method of the crystal according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the present invention, k is taken as k at the beginning of the isodiametric growth phase1Calculated to obtain Gh1Root of Chinese characterAccording to Gh1Adjusting the pulling speed of the crystal bar to be v1Liquid gap of d1Wherein, said k1Said v1And d is1Satisfies the following conditions: -0.12. ltoreq. k1≤-0.1，0.4≤v1≤0.8mm/min，50≤d1Less than or equal to 52 mm; in the middle stage of the equal-diameter growth stage, k is taken as k2Calculated to obtain Gh2According to Gh2Adjusting the pulling speed of the crystal bar to be v2Liquid gap of d2Wherein, said k2Said v2And d is2Satisfies the following conditions: -0.25. ltoreq. k2≤-0.23，0.4≤v2≤0.6mm/min，52≤d2Less than or equal to 53 mm; taking k as k at the later stage of the equal-diameter growth stage3Calculated to obtain Gh3According to Gh3Adjusting the pulling speed of the crystal bar to be v3Liquid gap of d3Wherein, said k3Said v3And d is3Satisfies the following conditions: -0.16. ltoreq. k3≤0.14，0.6≤v3≤0.8mm/min，54≤d3≤55mm。
In some embodiments of the invention, Δ G is controlled during the initial growth phase of the constant diameter growth phasec0.2 to 1K/cm,. DELTA.G e5 to 10K/cm, GrNot more than 6K/cm; controlling delta G in the middle stage of the equal-diameter growth stage c2 to 6K/cm,. DELTA.G e5 to 10K/cm, GrNot more than 10K/cm; controlling delta G at the later stage of the equal-diameter growth stagec0.2 to 1K/cm,. DELTA.G e5 to 10K/cm, GrNot more than 6K/cm, wherein the variation of the axial temperature gradient at the central position of the crystal bar is delta GcThe variation of the axial temperature gradient at the edge of the ingot is Delta GeThe radial temperature gradient of the ingot is Gr。
In some embodiments of the invention, the method further comprises adjusting a width of a temperature zone on the boule, the temperature zone comprising a first temperature zone ranging from 1685K to 1605K, a second temperature zone ranging from 1605K to 1355K, and a third temperature zone ranging from 1355K to 955K.
In some of the present inventionIn an embodiment, during the isometric growth phase, the first temperature band ranges according to linear equation Dx＝m*G0+ b adjusting the temperature zone width, where G0The temperature gradient at the solid-liquid interface is 35-55K/cm, DxIs the temperature zone width in mm.
In some embodiments of the present invention, at the beginning of the isodiametric growth phase, m is taken to be m1，b＝b1Calculating to obtain D1According to D1Adjusting the height of the guide shell from the solid-liquid interface, wherein m is more than or equal to-0.11≤-0.09，9≤b1Less than or equal to 9.1; taking m as m at the later stage of the equal-diameter growth stage2，b＝b2Calculating to obtain D2According to D2The height between the guide shell and the solid-liquid interface is adjusted, wherein m is more than or equal to-0.092≤-0.05，7≤b2Less than or equal to 8.5; in the middle stage of the equal-diameter growth stage, the temperature band width D of the middle stage3The width D of the temperature zone at the initial stage1And the width D of the temperature zone of the later stage2In the meantime.
In some embodiments of the invention, during the isometric growth phase, the second temperature band ranges according to linear equation Dy＝m*G0+ b adjusting the temperature zone width, where G0The temperature gradient at the solid-liquid interface is 35-55K/cm, DyIs the temperature zone width in mm.
In some embodiments of the present invention, at the beginning of the isodiametric growth phase, m is taken to be m3，b＝b3Calculating to obtain D4According to D4Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve, wherein m is more than or equal to-0.273≤-0.24，23.5≤b3Less than or equal to 25.5; taking m as m at the later stage of the equal-diameter growth stage4，b＝b4Calculating to obtain D5According to D5Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve, wherein m is more than or equal to-0.14≤-0.06，16.5≤b4Less than or equal to 17.5; in the middle stage of the equal-diameter growth stage, the temperature band width D of the middle stage6The width D of the temperature zone at the initial stage4And the temperature of the latter stageWidth D of the width band5In the meantime.
In some embodiments of the invention, during the isometric growth phase, the third temperature band ranges according to linear equation DzAdjusting the temperature band width (n x L + c) DzThe temperature zone width is expressed in mm, and L is the length of the ingot expressed in mm.
In some embodiments of the present invention, n is taken as n during the initial stage of the isodiametric growth phase1，c＝c1Calculating to obtain D7According to D7Adjusting the flow rate of cooling water in the water cooling jacket, wherein n is more than or equal to-0.0351≤-0.015，35≤c1Less than or equal to 45; in the middle and later stages of the equal-diameter growth stage, the width of the temperature band is controlled to be kept unchanged, and the width D of the temperature band in the middle stage is controlled8Equal to the initial temperature zone width D7。
In yet another aspect, the invention features a silicon crystal. According to the embodiment of the invention, the silicon crystal is prepared by the method.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 shows the axial temperature gradient G of an ingot at the initial stage of the isometric growth (ingot length 400mm)hAnd a graph with respect to the solid-liquid interface height h;
FIG. 2 shows the axial temperature gradient G of the ingot at the middle stage of the isodiametric growth (ingot length 700mm)hAnd a graph with respect to the solid-liquid interface height h;
FIG. 3 shows the axial temperature gradient G of the ingot at the later stage of the isometric growth stage (ingot length 1000mm)hAnd a graph with respect to the solid-liquid interface height h;
FIG. 4 shows the axial temperature gradient G of the ingot at the later stage of the isometric growth stage (the length of the ingot is 1300mm)hAnd a graph with respect to the solid-liquid interface height h;
FIG. 5 is a graph showing the width of the temperature zone in the first and second stages of the equal-diameter growth in the 1685K-1665K temperature zone of the first temperature zone;
FIG. 6 is a graph of the width of the temperature zone in the later stage of the equal-diameter growth stage in the 1685K-1665K temperature zone of the first temperature zone;
FIG. 7 is a graph showing the width of the temperature zone in the early and middle stages of the isometric growth stage in the 1665K-1645K temperature zone of the first temperature zone;
FIG. 8 is a graph of the width of the temperature band at the later stage of the isometric growth stage in the 1665K-1645K temperature band of the first temperature band;
FIG. 9 is a graph showing the width of the temperature zone in the initial and middle stages of the isometric growth stage in the 1645K to 1625K temperature zones of the first temperature zone;
FIG. 10 is a graph of the width of the temperature zone in the late stage of the isometric growth stage in the 1645K-1625K temperature zone of the first temperature zone;
FIG. 11 is a graph showing the width of the temperature zone in the initial and middle stages of the equal-diameter growth in the 1625K-1605K temperature zone of the first temperature zone;
FIG. 12 is a graph showing the width of the temperature zone in the late stage of the equal-diameter growth stage in the 1625K-1605K temperature zone of the first temperature zone;
FIG. 13 is a schematic diagram showing the operation of the copper decorating method.
Detailed Description
The following detailed description of the embodiments of the present invention is intended to be illustrative, and not to be construed as limiting the invention.
In the present invention, unless otherwise specified, the following meanings and symbols are defined as follows: the distance between the liquid ports is the distance between the lower end of the guide shell and the solid-liquid interface. The term "perfect crystal" as used herein does not mean an absolutely perfect crystal or a crystal without any defects, but rather allows the presence of a very small amount of one or more defects, which are insufficient to produce a large change in some electrical or mechanical property of the crystal or resulting wafer, which degrades the performance of its finished electronic device.
The crystal preparation by the Czochralski method is a process of putting a raw material polycrystalline silicon block into a quartz crucible, heating the quartz crucible, melting polycrystalline silicon filled in the quartz crucible, inserting seed crystals into the surface of a melt for fusion welding, simultaneously rotating the seed crystals, then reversing the crucible, slowly lifting the seed crystals upwards, and preparing a crystal rod through the processes of seeding, amplifying, shoulder rotating, isometric growth, ending and the like. And in the process of preparing the crystal by the Czochralski method, the heat history in the crystal bar is directly related to the distribution, the type and the size of the crystal defects, and the method is used for fully convectively diffusing and reuniting the point defects in the crystal and reducing the concentration of free V-type point defects and I-type point defects.
To this end, in one aspect of the invention, a method for producing a single crystal is proposed. According to an embodiment of the invention, the method comprises: according to the linear equation G in the equal-diameter growth stageh＝k*h+G0To obtain GhWherein G is0The temperature gradient at the solid-liquid interface is 35-55K/cm, h is the height of the solid-liquid interface and is 0-10 mm, and G ishThe axial temperature gradient of the crystal bar at the height h from the solid-liquid interface is adjusted to G in the region from the solid-liquid interface to the reference surface with the unit of K/cmhWherein the reference surface is an interface 10mm above the solid-liquid interface. Therefore, the axial temperature gradient of the crystal bar in the region from the solid-liquid interface to the reference surface is controlled, so that the I-type point defect and the V-type point defect formed in the crystal growing process are fully diffused and recombined in the region near the solid-liquid interface, and the forming concentration of the point defect is reduced.
According to the embodiment of the invention, in order to accurately control the temperature gradient of the crystal bar in the region from the solid-liquid interface to the reference surface, the temperature gradients corresponding to the initial stage of the constant diameter growth stage, the middle stage of the constant diameter growth stage and the later stage of the constant diameter growth stage are respectively optimized. It should be noted that "the initial stage of the isometric growth stage" is defined as a stage in which the length of the grown crystal is not more than 400 mm; the 'middle stage of the equal-diameter growth stage' is defined as the stage before the length of the grown crystal is more than 400mm and the liquid level of the silicon melt in the crucible enters the R angle of the crucible; the later stage of the isodiametric growth stage is defined as the stage after the liquid level of the silicon melt in the crucible enters the R angle of the crucible.
In particular, the method comprises the following steps of,at the beginning of the isometric growth phase, according to the linear equation Gh＝k*h+G0Where k is k1Calculated to obtain Gh1According to the calculated Gh1Adjusting the pulling speed of the crystal bar to be v1Liquid gap of d1Wherein, the above k1、v1And d1Satisfies the following conditions: -0.12. ltoreq. k1≤-0.1，0.4≤v1≤0.8mm/min，50≤d1Less than or equal to 52mm, i.e. according to linear equation Gh＝k*h+G0Where k is k1Calculated to obtain Gh1Then at v above1And d1Within the corresponding range by adjusting the pull-up speed v1Distance d between liquid inlet and liquid outlet1So that G ish1Is equal to Gh1The theoretical value of (1). It can be understood that when G ish1When the actual value of (d) is smaller than the theoretical value, the liquid gap d is reduced1So that G is0Increase, then Gh1Near the theoretical value and at the same time at the above-mentioned pulling speed v1The pulling speed can be reduced within the range, so that the point defects formed in the crystal can be fully diffused and recombined for a certain time, and the forming concentration of the point defects is reduced; in the middle stage of the isodiametric growth stage, according to the above-mentioned linear equation Gh＝k*h+G0Where k is k2Calculated to obtain Gh2According to the calculated Gh2Adjusting the pulling speed of the crystal bar to be v2Liquid gap of d2Wherein, the above k2、v2And d2Satisfies the following conditions: -0.25. ltoreq. k2≤-0.23，0.4≤v2≤0.6mm/min，52≤d2Less than or equal to 53mm, i.e. according to linear equation Gh＝k*h+G0Where k is k2Calculated to obtain Gh2Then at v above2And d2Within the corresponding range by adjusting the pull-up speed v2Distance d between liquid inlet and liquid outlet2So that G ish2Is equal to Gh2The theoretical value of (1). It can be understood that when G ish2When the actual value of (d) is larger than the theoretical value, the liquid gap d is increased2So that G is0Decrease, then Gh2Close to the theoretical value, and the pull rate v can be reduced within the above-mentioned range2So that the point defect formed in the crystal has oneThe formation concentration of point defects is reduced by sufficiently diffusing and recombining in a fixed time; at the later stage of the isodiametric growth stage, according to the above-mentioned linear equation Gh＝k*h+G0Where k is k3Calculated to obtain Gh3According to the calculated Gh3Adjusting the pulling speed of the crystal bar to be v3Liquid gap of d3Wherein, the above k3、v3And d3Satisfies the following conditions: -0.16. ltoreq. k3≤0.14，0.6≤v3≤0.8mm/min，54≤d3Less than or equal to 55mm, i.e. according to linear equation Gh＝k*h+G0Where k is k3Calculated to obtain Gh3Then at v above3And d3By adjusting the pull speed v within the corresponding range3Distance d between liquid inlet and liquid outlet3So that G ish3Is equal to Gh3The theoretical value of (1). It can be understood that when G ish3Is less than Gh3Theoretical value of (d), reducing the liquid gap distance d3So that G is0Increase, then Gh3Close to the theoretical value, and the pull rate v can be reduced within the above-mentioned range3So that the point defects formed in the crystal can be sufficiently diffused and recombined for a certain time, and the formation concentration of the point defects can be reduced. Thus, according to the above-mentioned production method, the temperature gradient G for each period is realized by controlling the pull rate and the liquid gap distance in the initial stage, the middle stage and the later stage of the isometric growth stage, respectivelyhThe adjustment of (3) enables the I-type point defect and the V-type point defect formed in the growth process to be fully diffused and recombined in the area near the solid-liquid interface, and reduces the concentration of the free V-type point defect and the I-type point defect. The variation range of the pulling speed in the crystal growth stage can be increased by 10%, and the variation range of the liquid gap can be increased by 5%, so that the adjustable window of the process parameters is enlarged, and the crystal quality and the perfect crystal yield are improved. Wherein, the yield is the ratio of the amount of the melting material for growing perfect crystals to the amount of the fed material.
Further, in order to verify the fitting of the above linear equation, the temperature gradient in the axial direction of the ingot at different growth stages in the region from the growth solid-liquid interface to the reference surface and the height with respect to the solid-liquid interface were plotted, as shown in FIG. 1, at the initial stage of the constant diameter growth stage (ingot)Length 400mm) of the ingot, with the height h of the long grain boundary surface as the abscissa, and with the temperature gradient G in the axial direction of the ingothPlotting a curve for the ordinate, the linear equation being Gh-0.10h +41.361, degree of fit R of this equation20.9994; as shown in FIG. 2, in the middle stage of the equal diameter growth stage (ingot length 700mm), the height h of the grain boundary surface is plotted on the abscissa and the temperature gradient G in the axial direction of the ingot is plottedhPlotting a curve for the ordinate, the linear equation being GhH +47.031, degree of fit R of this equation20.9988; as shown in FIGS. 3 and 4, in the later stage of the isodiametric growth stage (the lengths of the ingot are 1000mm and 1300mm, respectively), the height h of the crystal grain boundary surface is taken as the abscissa, and the temperature gradient G in the axial direction of the ingot is taken as the temperature gradienthDrawing a curve for the ordinate, wherein the linear equation corresponding to the length of the crystal bar of 1000mm is Gh-0.2463h +49.155, degree of fit R of this equation20.999, the linear equation corresponding to the crystal bar length of 1300mm is Gh-0.1507 h +45.003, and the fitting degree R of the equation20.999. In a word, the fitting degree of each linear equation is more than 0.998, which shows that the fitted linear equation is very consistent with the actual condition, so that the pulling speed and the liquid gap distance are correspondingly adjusted according to the linear equation, the axial temperature gradient in the region from the solid-liquid interface to the reference plane can be accurately controlled, and the forming concentration of point defects is effectively reduced.
According to the embodiment of the invention, in order to further improve the crystal quality and the yield of perfect crystals, the temperature gradient variation quantity delta G in the axial direction of the central position of the crystal bar is controlled in the initial stage of the equal-diameter growth stagec0.2 to 1K/cm, and controlling the temperature gradient variation delta G in the axial direction of the edge position of the crystal bare5 to 10K/cm, and controlling the radial temperature gradient G of the crystal barrNot more than 6K/cm; controlling the temperature gradient variation delta G in the axial direction of the central position of the crystal bar in the middle stage of the equal diameter growth stagec2-6K/cm, and controlling the temperature gradient variation delta G of the edge position of the crystal bar in the axial directione5 to 10K/cm, and controlling the radial temperature gradient G of the crystal barrNot more than 10K/cm; controlling the temperature gradient variation delta G in the axial direction of the central position of the crystal bar at the later stage of the equal-diameter growth stagecIs 0.2 &1K/cm, and controlling the temperature gradient variation delta G of the edge position of the crystal bar in the axial directione5-10K/cm, and controlling the radial temperature gradient G of the crystal barrNot more than 6K/cm. In each different period of the equal-diameter growth stage, the shape of the solid-liquid interface is ensured to be approximate to a plane by controlling the axial temperature gradient variation and the radial temperature gradient of the central position and the edge position of the crystal bar, so that the axial temperature gradient in the same section is approximate to uniform, the window for growing perfect crystals can be enlarged according to a V/G theory, and the yield of perfect crystals is improved.
According to an embodiment of the present invention, the method further comprises adjusting a width of a temperature zone of 1685K to 955K on the ingot, wherein the temperature zone comprises a first temperature zone, a second temperature zone and a third temperature zone, the first temperature zone is in a range of 1685K to 1605K, the second temperature zone is in a range of 1605K to 1355K, and the third temperature zone is in a range of 1355K to 955K.
According to one embodiment of the invention, the first temperature zone comprises 1685K-1665K, 1665K-1645K, 1645K-1625K and 1625K-1605K temperature zones, the first temperature zone comprises a plurality of small temperature zones, the width difference of each small temperature zone is less than 1.0mm, and the width of the same temperature zone changes less than 0.5mm during the growth process. During the growth process and in the first temperature zone range of the equal diameter growth stage, according to the linear equation Dx＝m*G0+ b adjusting the temperature zone width, where G0The temperature gradient at the solid-liquid interface is 35-55K/cm, DxIs the temperature zone width in mm. It can be understood that the first temperature zone widths are adjusted according to the above linear equation, so that in the same period of the equal-diameter growth stage, the difference between the width of each small temperature zone in the first temperature zone is less than 1.0mm, that is, the width of each small temperature zone is relatively close, and in each period of the equal-diameter growth stage, the difference between the width of each small temperature zone is less than 0.5mm, that is, the variation of the width of each small temperature zone is relatively small, so that the position of the first temperature zone width on the ingot can be accurately controlled.
Specifically, in the initial stage of the isodiametric growth stage, the linear equation D is usedx＝m*G0+ b where m is m1，b＝b1Calculating to obtain D1According to D1Adjusting the height of the guide shell from the solid-liquid interface, wherein m is more than or equal to-0.11≤-0.09，9≤b1Less than or equal to 9.1, i.e. according to linear equation Dx＝m*G0+ b where m is m1，b＝b1Calculating to obtain D1Then adjusting the height of the guide shell from the solid-liquid interface to ensure that D1Is equal to D1The theoretical value of (1). It can be understood that the temperature gradient G at the solid-liquid interface is realized by adjusting the height between the guide shell and the solid-liquid interface0To thereby realize the adjustment of D1And (4) adjusting. According to the actual production situation, the height H of the guide shell from the solid-liquid interface is increased by descending the quartz crucible through the rotation of the crucible shaft, and the quartz crucible is closer to the heater, so that G0Decrease and thus the temperature zone width D1Increasing; in the same way, the height H of the guide cylinder from the solid-liquid interface is reduced by rotating the crucible shaft to enable the quartz crucible to rise, and then the quartz crucible is far away from the heater, so that G0Increase and thus the temperature zone width D1And decreases. At the later stage of the isodiametric growth stage, according to the above-mentioned linear equation Dx＝m*G0+ b where m is m2，b＝b2Calculating to obtain D2According to D2The height between the guide shell and the solid-liquid interface is adjusted, wherein m is more than or equal to-0.092≤-0.05，7≤b2Less than or equal to 8.5, i.e. according to linear equation Dx＝m*G0+ b where m is m2，b＝b2Calculating to obtain D2Then adjusting the height of the guide shell from the solid-liquid interface to ensure that D2Is equal to D2The theoretical value of (1). It can be understood that the temperature gradient G at the solid-liquid interface is realized by adjusting the height H between the guide shell and the solid-liquid interface0To thereby realize the adjustment of D2And (4) adjusting. According to the actual production situation, the height H of the guide shell from the solid-liquid interface is increased by rotating the crucible shaft to enable the quartz crucible to descend, and the quartz crucible is closer to the heater, so that G0Decrease and thus the temperature zone width D2Increasing; the height H from the guide cylinder to the solid-liquid interface is reduced by rotating the crucible shaftWhen the quartz crucible rises, the quartz crucible is farther from the heater, so that G0Increase and thus the temperature zone width D2And decreases. Meanwhile, in the middle stage of the equal-diameter growth stage, the temperature band width D in the middle stage3Width D of temperature zone at initial stage1And the width D of the temperature zone at the later stage2In the meantime. At the time of transition from the initial stage to the middle stage in the process from the initial stage to the middle stage, the temperature zone width D of the middle stage at that time3Width D of temperature zone from initial stage1Equal to each other, at the time of transition from the middle stage to the later stage, the temperature zone width D of the middle stage3Width D of temperature zone in later period2Equal to each other, and the temperature zone width D during the middle period3At D1And D2To change between. In a word, according to the linear equation of each period, the width of the first temperature zone is timely adjusted by adjusting the height between the guide cylinder and the solid-liquid interface, so that the first temperature zone is finally close to a theoretical value, and the temperature distribution of the crystal bar is effectively controlled.
Specifically, in the 1685K-1665K temperature zone of the first temperature zone, as shown in fig. 5, the temperature zone width curves of the initial stage and the middle stage of the isodiametric growth stage are shown, and the linear equation of the temperature zone width is Dx＝-0.0998G0+9.0432, degree of fit R of this equation20.9923; FIG. 6 is a graph of the temperature band width at the later stage of the isodiametric growth stage, and the linear equation of the temperature band width is Dx＝-0.0879G0+8.5236, degree of fit R of this equation20.9963, the temperature gradient G at the solid-liquid interface is shown0As abscissa, with temperature band width DxThe graph is plotted as ordinate.
Specifically, in the 1665K-1645K temperature band of the first temperature band, as shown in fig. 7, the temperature band width curves in the initial and middle stages of the isodiametric growth stage are shown, and the linear equation of the temperature band width is Dx＝-0.0971G0+9.0516, degree of fit R of this equation20.989; FIG. 8 is a graph showing the temperature band width at the later stage of the isodiametric growth stage, where the linear equation of the temperature band width is Dx＝-0.0688G0+7.7369, degree of fit R of this equation20.9977, wherein the temperature gradient G at the solid-liquid interface is shown0As abscissa, with temperature band width DxIs the ordinate.
Specifically, in the 1645K to 1625K temperature band of the first temperature band, as shown in fig. 9, the temperature band width curves in the initial stage and the middle stage of the isodiametric growth stage are shown, and the linear equation of the temperature band width is Dx＝-0.0909G0+8.872, degree of fit R of this equation20.9763; FIG. 10 is a graph showing the temperature band width at the later stage of the isodiametric growth stage, where the linear equation of the temperature band width is Dx＝-0.0705G0+7.8889, degree of fit R of this equation20.9906, the temperature gradient G at the solid-liquid interface is shown0As abscissa, with temperature band width DxIs the ordinate.
Specifically, in the 1625K to 1605K temperature zone of the first temperature zone, as shown in fig. 11, the temperature zone width curves in the initial stage and the middle stage of the equal diameter growth stage are shown, and the linear equation of the temperature zone width is Dx＝-0.093G0+9.0792, degree of fit R of this equation20.9562; FIG. 12 is a graph showing the temperature band width at the later stage of the isodiametric growth stage, where the linear equation of the temperature band width is Dx＝-0.0582G0+7.3744, degree of fit R of equation20.9979, the temperature gradient G at the solid-liquid interface is shown0As abscissa, with temperature band width DxIs the ordinate.
In a word, the fitting degree of linear equations of the widths of the small temperature bands in the first temperature band is more than 0.95, which shows that the fitted linear equations are very consistent with the actual conditions. Therefore, the height of the guide cylinder from the solid-liquid interface can be adjusted in an instructive way according to the linear equation of the first temperature zone, the width of the first temperature zone can be accurately adjusted, the thermal history of the crystal bar is controlled, the growth of point defects is inhibited, the size of the defects is controlled, and the yield of perfect crystal growth is improved.
According to still another embodiment of the present invention, the second temperature zone includes 1605K-1555K, 1555K-1505K, 1505K-1455K, 1455K-1405K, 1405K-1355K temperature zones, the second temperature zone includes a plurality of small temperature zones, and widths of the respective small temperature zones are different by less than 1.5mm, and widths of the same temperature zone are varied during the growth processThe chemical conversion is less than 1.0 mm. And in the second temperature zone range of the equal-diameter growth stage according to a linear equation Dy＝m*G0+ b adjusting the temperature zone width, where G0The temperature gradient at the solid-liquid interface is 35-55K/cm, DyIs the temperature zone width in mm. It can be understood that the second temperature zone widths are adjusted according to the above linear equation, so that the difference between the respective small temperature zone widths in the second temperature zone is smaller than 1.5mm in the same period of the equal-diameter growth stage, that is, the respective small temperature zones are almost the same, and meanwhile, in the respective periods of the equal-diameter growth stage, the difference between each small temperature zone width is smaller than 1.0mm, that is, the variation of each small temperature zone width is small, so that the position of the first temperature zone width on the ingot can be accurately controlled.
Specifically, in the initial stage of the isodiametric growth stage, according to the linear equation Dy＝m*G0+ b where m is m3，b＝b3Calculating to obtain D4According to D4Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve, wherein m is more than or equal to-0.273≤-0.24，23.5≤b325.5 or less, i.e. according to the linear equation D-m G0+ b where m is m3，b＝b3Calculating to obtain D4Then adjusting the distance of the water cooling sleeve from the outer wall of the crystal bar to enable D4Is equal to D4The theoretical value of (1). It is to be understood that if D4The actual value of (D) is less than the theoretical value, the flow of cooling water in the water cooling jacket is reduced or the distance between the water cooling jacket and the outer wall of the crystal bar is increased, and then the width D of the temperature zone is obtained4Increasing, closer to the theoretical value; in the later stage of the isodiametric growth phase, according to the linear equation D-m G0+ b where m is m4，b＝b4Calculating to obtain D5According to D5Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve, wherein m is more than or equal to-0.14≤-0.06，16.5≤b4Less than or equal to 17.5, i.e. according to the linear equation D-m G0+ b where m is m4，b＝b4Calculating to obtain D5Then adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve to ensure that D5Is equal to D5The theoretical value of (1). It is to be understood that if D5The actual value of the temperature zone is larger than the theoretical value, the flow rate of cooling water in the water cooling jacket is increased or the distance between the water cooling jacket and the outer wall of the crystal bar is reduced, and the width D of the temperature zone5Becomes smaller and closer to the theoretical value; middle stage of the equal-diameter growth stage, middle temperature band width D6Width D of temperature zone at initial stage4And the width D of the temperature zone at the later stage5In the meantime. It can be understood that the time point of transition from the initial stage to the intermediate stage in the process from the initial stage to the intermediate stage, the temperature zone width D in the intermediate stage6Width D of temperature zone from initial stage4Equal to each other, at the time of transition from the middle stage to the later stage, the temperature zone width D of the middle stage6Width D of temperature zone in later period5Equal to each other, and the temperature zone width D during the middle period6At D4And D5To change between.
Similarly, by using the simulation method of the second temperature width, the fitting degree of the linear equations of the widths of the small temperature bands in the second temperature band is greater than 0.95, which is not described herein again. Therefore, the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve can be adjusted in an instructive way according to the linear equation of the second temperature zone, the width of the second temperature zone can be accurately adjusted, the thermal history of the crystal bar and the size of the defect can be controlled, and the yield of the perfect crystal can be improved.
According to yet another embodiment of the present invention, in the third temperature band range of the isometric growth phase, according to linear equation DzAdjusting the temperature band width (n x L + c) DzThe temperature zone width is expressed in mm, and L is the length of the ingot expressed in mm. Specifically, in the initial stage of the isodiametric growth phase, n-n in D-L + c is expressed according to the linear equation1，c＝c1Calculating to obtain D7According to D7Adjusting the flow rate of cooling water in the water cooling jacket, wherein n is more than or equal to-0.0351≤-0.015，35≤c1N ≦ 45, i.e. n ≦ n in the linear equation D ═ n L + c1，c＝c1Calculating to obtain D7Then adjusting the cooling water flow in the water cooling jacket to enable D7Is equal to D7The theoretical value of (1). Can be used forIn the sense that if D7If the actual value of (D) is greater than the theoretical value, the cooling water flow in the water cooling jacket is increased, and the width D of the temperature zone is increased7Increasing, closer to the theoretical value; in the middle and later stages of the equal-diameter growth stage, the width of the temperature band is controlled to be kept unchanged, and the width D of the temperature band in the middle stage is controlled8Equal to the initial temperature zone width D7. It can be understood that the temperature zone width D is the time from the initial stage to the middle stage in the equal diameter growth stage8Equal to the width D of the temperature belt in the initial stage at the moment7At the middle and later stages, the temperature zone width D8Remain unchanged at all times.
Similarly, by using the simulation method of the third temperature width, the fitting degree of the linear equation of the third temperature zone is also greater than 0.95, which is not described herein again. Therefore, the flow of cooling water in the water cooling jacket can be adjusted in an instructive way according to the linear equation of the third temperature zone, the width of the third temperature zone can be accurately adjusted, the thermal history of the crystal bar and the size of the defect can be controlled, and the yield of the grown perfect crystal can be improved.
In a word, by accurately controlling the temperature bandwidth of the crystal bar, the nucleation and the size of the microdefect are effectively inhibited, and the yield of the grown perfect crystal is improved by 10 to 20 percent.
In yet another aspect, the invention features a silicon crystal. According to the embodiment of the invention, the silicon crystal is prepared by the method. Therefore, the silicon crystal has higher quality. It is understood that the proportion of the window in the silicon crystal that is perfect is large.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Examples
In the equal-diameter growth stage, the temperature gradient in the region from the solid-liquid interface to the reference surface is adjusted to GhAnd a temperature bandwidth of the ingot, wherein G0The value is 35-55K/cm:
at the beginning of the isometric growth phase, according to the linear equation Gh＝k*h+G0Where k is k1Is calculated to obtainGh1According to Gh1Adjusting the pulling speed of the crystal bar to be v1Liquid gap of d1Wherein-0.12. ltoreq. k1≤-0.1，0.4≤v1≤0.8mm/min，50≤d1Not more than 52mm, and simultaneously controlling the temperature gradient Delta G of the central position of the crystal bar in the axial directionc0.2 to 1K/cm, and controlling the temperature gradient delta G of the edge position of the crystal bar in the axial directione5 to 10K/cm, and controlling the radial temperature gradient G of the crystal barrNot more than 6K/cm, and in addition, in the first temperature zone 1685K-1605K range of the constant diameter growth stage according to linear equation Dx＝m*G0+ b where m is m1，b＝b1Calculating to obtain D1According to D1Adjusting the height of the guide shell from the solid-liquid interface, wherein m is more than or equal to-0.11≤-0.09，9≤b1Less than or equal to 9.1; in the second temperature zone 1605K to 1355K in the constant diameter growth stage according to the linear equation Dy＝m*G0+ b adjustment where m ═ m3，b＝b3Calculating to obtain D4According to D4Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve, wherein m is more than or equal to-0.273≤-0.24，23.5≤b3Less than or equal to 25.5, in the third temperature zone 1355K to 955K in the isometric growth stage according to the linear equation DzAdjusting the width of the temperature band, wherein n is equal to n1，c＝c1Calculating to obtain D7According to D7Adjusting the flow rate of cooling water in the water cooling jacket, wherein n is more than or equal to-0.0351≤-0.015，35≤c1≤45；
In the middle stage of the isodiametric growth stage, according to the linear equation Gh＝k*h+G0Where k is k2Calculated to obtain Gh2According to Gh2Adjusting the pulling speed of the crystal bar to be v2Liquid gap of d2Wherein-0.25. ltoreq. k2≤-0.23，0.4≤v2≤0.6mm/min，52≤d2Not more than 53mm, and simultaneously controlling the temperature gradient Delta G of the central position of the crystal bar in the axial directionc2-6K/cm, and controlling the temperature gradient delta G of the edge position of the crystal bar in the axial direction e5 to 10K/cm, and controlling the radial temperature gradient G of the crystal barrNot more than 10K/cm; at the same time, the middle stageControlling the width D of the first temperature zone 1685K to 1605K3Width D of temperature zone at initial stage1And the width D of the temperature zone at the later stage2In the middle of; controlling a temperature zone width D of the second temperature zones 1605K to 1355K6Temperature zone width D at initial stage4And the width D of the temperature zone at the later stage5To (c) to (d); controlling a width D of the third temperature zone 1355K to 955KzThe width D of the temperature zone in the third temperature zone range at the early stage of the equal-diameter growth stage7Remain unchanged.
At the later stage of the isodiametric growth stage, according to the linear equation Gh＝k*h+G0Where k is k3Calculated to obtain Gh3According to Gh3Adjusting the pulling speed of the crystal bar to be v3Liquid gap of d3Wherein, the above k3、v3And d3Satisfies the following conditions: -0.16. ltoreq. k3≤0.14，0.6≤v3≤0.8mm/min，54≤d3Not more than 55mm, and simultaneously controlling the temperature gradient Delta G of the central position of the crystal bar in the axial directionc0.2 to 1K/cm, and controlling the temperature gradient delta G of the edge position of the crystal bar in the axial directione5-10K/cm, and controlling the radial temperature gradient G of the crystal barrNot more than 6K/cm. In the range of 1685K to 1605K of the first temperature zone, taking m ═ m2，b＝b2Calculating to obtain D2According to D2The height between the guide shell and the solid-liquid interface is adjusted, wherein m is more than or equal to-0.092≤-0.05，7≤b2Less than or equal to 8.5; and in the range of the second temperature zone 1605K to 1355K, taking m as m4，b＝b4Calculating to obtain D5According to D5Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve, wherein m is more than or equal to-0.14≤-0.06，16.5≤b4Less than or equal to 17.5; controlling a width D of the temperature zone within a range of 1355K to 955K8The width D of the temperature zone in the third temperature zone range at the early stage of the equal-diameter growth stage7Remain unchanged.
For the parts related to the adjustment of the process parameters in the above embodiments, please refer to the manner described in detail above for adjustment, and further description is omitted here.
Comparative example
The existing growth device and preparation method are adopted to pull out the crystal bar, namely, compared with the process of the embodiment, the temperature gradient and the temperature zone are not controlled.
For the examples and the comparative examples, wafers with the lengths of the crystal bars of 180mm, 340 mm, 650 mm, 950 mm, 1200 mm and 1350mm were taken out, and defects thereof were characterized by using a copper decorating method, respectively, and the defect characterization results are shown in table 1, where the crystal bars in the examples and the comparative examples are silicon crystal bars. Referring to fig. 13, the specific operations of copper decorating include: firstly, washing a test piece by tap water, then washing the surface of the test piece by a surfactant to remove surface particles on the surface of the test piece, then polishing and cleaning the surface of the test piece by chemical polishing, then coating copper nitrate on the surface of the cleaned test piece, forming copper precipitates on the surface of the test piece after heat treatment, then polishing and cleaning the surface of the test piece, and finally carrying out etching development. Wherein the test piece is a silicon wafer. The microdefects of the wafer can be observed under a microscope because many copper precipitates and dislocations are formed around the microdefects to form a large area. In the micro defect map, a black part is a perfect area, and a white part is a defect area.
TABLE 1 results of wafer defect inspection of the respective positions of the crystal bars obtained in examples and comparative examples by the above copper decorating method
Wafer position (mm) Examples Comparative example
180 Type I defect Defect of V type
340 Perfect crystal Type I defect
650 Perfect crystal Type I defect
950 Perfect crystal Type I defect
1200 Perfect crystal Type I defect
1350 Type I defect Defect of V type
As can be seen from the above detection results in Table 1, the defects of the ingot grown by the comparative example were V-type defects in the beginning, I-type defects in the middle, and V-type defects in the end, and no perfect crystal appeared in the entire ingot. In the embodiment, by adopting the preparation method of the present application, perfect crystals exist in the grown crystal bar at the lengths of 340 mm, 650 mm, 950 mm and 1200 mm, the window is large (as can be directly seen from a copper decoration defect diagram), and according to the V/G theory, perfect crystals exist in a certain range of the pulling rate (V is more than or equal to 0.4 and less than or equal to 0.8mm/min), and the length of the crystal bar is within a range from 340 mm to 1200 mm. The preparation method of the application can be used for improving the yield of perfect crystals.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (11)

1. A method for producing a single crystal, comprising:
in the equal-diameter growth stage, according to the linear equation Gh＝k*h+G0To obtain GhWherein G is0The temperature gradient at the solid-liquid interface is 35-55K/cm, h is the height of the solid-liquid interface and is 0-10 mm, and G ishThe axial temperature gradient of the crystal bar at the height h from the solid-liquid interface is represented by the unit of K/cm;
adjusting the temperature gradient to G in the region from the solid-liquid interface to the reference surfacehWherein the reference surface is an interface 10mm above a solid-liquid interface.
2. The method of claim 1, wherein k-k is taken at the beginning of the isodiametric growth phase1Calculated to obtain Gh1According to Gh1Adjusting the pulling speed of the crystal bar to be v1Liquid gap of d1Wherein, said k1Said v1And d is1Satisfies the following conditions: -0.12. ltoreq. k1≤-0.1，0.4≤v1≤0.8mm/min，50≤d1≤52mm；
In the middle stage of the equal-diameter growth stage, k is taken as k2Calculated to obtain Gh2According to Gh2Adjusting the pulling speed of the crystal bar to be v2Liquid gap of d2Wherein, said k2Said v2And d is2Satisfies the following conditions: -0.25. ltoreq. k2≤-0.23，0.4≤v2≤0.6mm/min，52≤d2≤53mm；
Taking k as k at the later stage of the equal-diameter growth stage3Calculated to obtain Gh3According to Gh3Adjusting the pulling speed of the crystal bar to be v3Liquid gap of d3Wherein, said k3Said v3And d is3Satisfies the following conditions: -0.16. ltoreq. k3≤0.14，0.6≤v3≤0.8mm/min，54≤d3≤55mm。
3. The method of claim 2, wherein Δ G is controlled during the initial stage of the constant diameter growth phasec0.2 to 1K/cm,. DELTA.Ge5 to 10K/cm, GrNot more than 6K/cm;
controlling delta G in the middle stage of the equal-diameter growth stagec2-6K/cm,. DELTA.Ge5 to 10K/cm, GrNot more than 10K/cm;
controlling delta G at the later stage of the equal-diameter growth stagec0.2 to 1K/cm,. DELTA.Ge5 to 10K/cm, GrNot more than 6K/cm;
wherein the axial temperature gradient variation at the central position of the crystal bar is delta GcThe variation of the axial temperature gradient at the edge of the ingot is Delta GeThe radial temperature gradient of the ingot is Gr。
4. The method of claim 1, further comprising adjusting a width of a temperature zone on the boule, the temperature zone comprising a first temperature zone in a range of 1685K to 1605K, a second temperature zone in a range of 1605K to 1355K, and a third temperature zone in a range of 1355K to 955K.
5. The method of claim 4, wherein during the isodiametric growth phase, the first temperature band ranges according to linear equation Dx＝m*G0+ b adjusting the temperature zone width, where G0The temperature gradient at the solid-liquid interface is 35-55K/cm, DxIs the temperature zone width in mm.
6. The method of claim 5, wherein m-m is taken at the beginning of the isodiametric growth phase1，b＝b1Calculating to obtain D1According to D1Adjusting the height of the guide shell from the solid-liquid interface, wherein m is more than or equal to-0.11≤-0.09，9≤b1≤9.1；
Taking m as m at the later stage of the equal-diameter growth stage2，b＝b2Calculating to obtain D2According to D2The height between the guide shell and the solid-liquid interface is adjusted, wherein m is more than or equal to-0.092≤-0.05，7≤b2≤8.5；
In the middle stage of the equal-diameter growth stage, the temperature band width D of the middle stage3The width D of the temperature zone at the initial stage1And the width D of the temperature zone of the later stage2In the meantime.
7. The method of claim 4, wherein during the isodiametric growth phase, the second temperature band ranges according to linear equation Dy＝m*G0+ b adjusting the temperature zone width, where G0The temperature gradient at the solid-liquid interface is 35-55K/cm, DyIs the temperature zone width in mm.
8. The method of claim 7, wherein m-m is taken at the beginning of the isodiametric growth phase3，b＝b3CalculatingTo obtain D4According to D4Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the cooling water flow in the water cooling sleeve, wherein m is more than or equal to-0.273≤-0.24，23.5≤b3≤25.5；
Taking m as m at the later stage of the equal-diameter growth stage4，b＝b4Calculating to obtain D5According to D5Adjusting the distance between the water cooling sleeve and the outer wall of the crystal bar or the flow of cooling water in the water cooling sleeve, wherein m is more than or equal to-0.14≤-0.06，16.5≤b4≤17.5；
In the middle stage of the equal-diameter growth stage, the temperature band width D of the middle stage6The width D of the temperature zone at the initial stage4And the width D of the temperature zone of the later stage5In between.
9. The method of claim 4, wherein during the isometric growth phase, the third temperature zone is within the range according to linear equation DzAdjusting the temperature band width (n x L + c) DzThe temperature zone width is expressed in mm, and L is the length of the ingot expressed in mm.
10. The method of claim 9, wherein n-n is taken at the beginning of the isodiametric growth phase1，c＝c1Calculating to obtain D7According to D7Adjusting the flow rate of cooling water in the water cooling jacket, wherein n is more than or equal to-0.0351≤-0.015，35≤c1≤45；
Controlling the width of the temperature band to be kept unchanged in the middle stage and the later stage of the equal-diameter growth stage, wherein the width D of the temperature band in the middle stage8Equal to the initial temperature zone width D7。
11. A silicon crystal, characterized in that it is prepared by the method of any one of claims 1-10.
CN202111619103.2A 2021-12-27 2021-12-27 Method for producing single crystal and silicon crystal Pending CN114438585A (en)

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WO2023125206A1 (en) * 2021-12-27 2023-07-06 中环领先半导体材料有限公司 Method for preparing single crystal, and silicon crystal

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CN110284186A (en) * 2019-07-30 2019-09-27 刘冬雯 A kind of measurement control method of czochralski crystal growing furnace and its longitudinal temperature gradient
TW202014565A (en) * 2018-08-23 2020-04-16 日商Ｓｕｍｃｏ股份有限公司 Method for growing silicon single crystal
CN113549997A (en) * 2021-06-25 2021-10-26 徐州鑫晶半导体科技有限公司 Method and apparatus for growing single crystal, and single crystal

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CN113549997A (en) * 2021-06-25 2021-10-26 徐州鑫晶半导体科技有限公司 Method and apparatus for growing single crystal, and single crystal

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