WO2017070827A1 - Automatic zone melting crystal growth method and system - Google Patents

Automatic zone melting crystal growth method and system Download PDF

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Publication number
WO2017070827A1
WO2017070827A1 PCT/CN2015/092868 CN2015092868W WO2017070827A1 WO 2017070827 A1 WO2017070827 A1 WO 2017070827A1 CN 2015092868 W CN2015092868 W CN 2015092868W WO 2017070827 A1 WO2017070827 A1 WO 2017070827A1
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Prior art keywords
growth
single crystal
diameter
polycrystalline
crystal
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PCT/CN2015/092868
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French (fr)
Chinese (zh)
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刘和松
陈辉
张立杰
伍月爽
尚锐刚
周冰
杨凯
高辉
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北京京运通科技股份有限公司
北京天能运通晶体技术有限公司
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Priority to CN201580000631.6A priority Critical patent/CN107002276B/en
Priority to PCT/CN2015/092868 priority patent/WO2017070827A1/en
Publication of WO2017070827A1 publication Critical patent/WO2017070827A1/en

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B13/00Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/28Controlling or regulating
    • C30B13/30Stabilisation or shape controlling of the molten zone, e.g. by concentrators, by electromagnetic fields; Controlling the section of the crystal
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

Definitions

  • the invention relates to a method and a production device for growing a zone melting crystal, in particular to a method and a system for automatically growing a zone melting crystal.
  • the process of growing single crystal by zone melting method mainly consists of preheating, chemical compounding, seeding, expanding shoulder, equal diameter and closing.
  • the use of full manual method for pulling crystal has significant shortcomings, mainly reflected in the long drawing time of large-size single crystal, and the mass production is difficult; the human influence factor is large, and the growth process is difficult to control; Poor quality consistency.
  • the invention provides an automatic growth method and system for a zone melting crystal, which solves the technical problem that the shape of the grown single crystal is unpredictable compared with the prior art.
  • the present invention provides an automatic growth method for a zone melting crystal, comprising the steps of:
  • the growth interval of the single crystal is the circular truncated growth interval of the layer; a growing interval growth of the configured growth parameter; wherein the growth parameter includes at least a polycrystalline falling speed and a heating power, respectively adjusted according to a configured functional relationship, so that the single crystal grows according to a growth angle in which the growth interval is configured;
  • the growth angle refers to the angle between the round busbar and the lower bottom surface;
  • the diameter of the single crystal reaches the target value, it is switched to the automatic equal diameter growth stage.
  • the growth interval in which the single crystal is located is the growth interval of the uppermost layer, and the single crystal grows in the axial direction in the growth interval.
  • the growth parameter further includes a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein the lower melting zone equivalent height is equal to the liquid volume of the lower melting zone.
  • the height of the cylindrical melting zone is equal to the liquid volume of the lower melting zone.
  • the functional relationship that the polycrystalline falling speed has been configured is specifically:
  • V poly is the polycrystalline falling speed
  • V mono is the single crystal falling speed
  • D is the measured diameter of the polycrystal
  • d is the diameter of the single crystal
  • ⁇ l is the liquid density of the crystal
  • ⁇ s is the solid density of the crystal
  • h Lqd is the equivalent height of the lower melting zone
  • is the configured growth angle of the growth zone in which the single crystal is located.
  • the polycrystalline falling speed is adjusted according to the configured function relationship, and the functional relationship is specifically: Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystalline, and d is the diameter of the single crystal.
  • the functional relationship P f(d) of the heating power is obtained by a curve fitting technique, wherein P is the heating power and d is the diameter of the single crystal.
  • the curve fitting technique employs a polynomial as a fitting function.
  • the curve fitting technique employs a least squares fitting method.
  • the present invention also provides an automatic growth system for a zone melting crystal, comprising:
  • a diameter measuring device for measuring the diameter of a single crystal
  • Polycrystalline drop servo motor for controlling the falling speed of the polycrystalline material rod
  • a high frequency heating device for heating the crystal
  • a programmable logic controller for storing the configured multi-layer truncated cone growth interval and the configured growth angle of each growth interval, wherein the growth angle refers to an angle between the truncated bus bar and the lower bottom surface; and is also used for storage a function of the configured polycrystalline falling speed, and a heating power function relationship;
  • the programmable logic controller is further configured to switch to an automatic shoulder growth stage after the diameter of the single crystal is larger than the diameter of the bottom surface of the configured lowermost truncated growth section; and is also used in the automatic shoulder growth stage.
  • the growth interval of the single crystal is determined as the growth range of the truncated cone, and is controlled according to the growth parameters of the growth interval.
  • the polycrystalline falling servo motor causes the polycrystalline falling speed to be adjusted according to a configured function relationship, while controlling the high frequency heating device such that the heating power is adjusted according to a configured function relationship;
  • the diameter reaches the target value, it switches to the automatic equal diameter growth stage to control the growth of the single crystal in the axial direction.
  • the growth parameter further includes a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein the lower melting zone equivalent height is equal to the liquid volume of the lower melting zone.
  • the height of the cylindrical melting zone is equal to the liquid volume of the lower melting zone.
  • the diameter measuring device is further used to determine the diameter of the polycrystalline material rod
  • the programmable logic controller is further configured to control the polycrystalline falling servo motor, and in the automatic shoulder growth stage, the function relationship of the polycrystalline falling speed has been configured as follows: Wherein, V poly polycrystalline lowering speed, V mono monocrystalline lowering speed, D is the measured diameter polycrystalline, d is the diameter of a single crystal, ⁇ l is the density of the liquid crystal, ⁇ s is the solid state density crystals, h Lqd is the equivalent height of the lower melting zone, and ⁇ is the configured growth angle of the growth zone in which the single crystal is located.
  • the diameter measuring device is further used to determine the diameter of the polycrystalline material rod
  • the programmable logic controller is further configured to control the servo motor and, in an automatic equal diameter growth phase, the polycrystalline falling speed is adjusted according to a configured function relationship, and the function relationship of the polycrystalline falling speed configured is specifically Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystalline, and d is the diameter of the single crystal.
  • the functional relationship P f(d) of the heating power is obtained by a curve fitting technique, wherein P is the heating power and d is the diameter of the single crystal.
  • the curve fitting technique uses a polynomial as a fitting function.
  • the curve fitting technique employs a least squares fitting method.
  • the single crystal in the automatic shoulder growth stage, the single crystal grows in the growth interval of the configured growth parameters, and the polycrystal falling speed and heating power in the growth parameters are respectively configured according to the configuration.
  • the functional relationship adjustment causes the single crystal to grow in accordance with the growth angle at which the growth interval is disposed, so that the actual growth shape of the single crystal is predictable.
  • the automatic growth method of the zone melting crystal of the present invention and the actual shape of the single crystal grown by the system are predictable, and the shape of the single crystal can be conveniently formed to reduce the waste of raw materials.
  • the manual operation is reduced, and the stability of the single crystal quality is enhanced.
  • Figure 1 is a schematic view showing the preparation of crystals by a suspension zone melting method
  • FIG. 2 is a schematic view showing a configuration of a multi-layered truncated cone growth section and a growth angle of each truncated cone growth section in the automatic growth method of the zone melting crystal of the present invention
  • FIG. 3 is a schematic view of a single-crystal truncated cone growth section shown in FIG. 2 and a growth angle grown single crystal in each truncated cone growth section;
  • FIG. 4 is a schematic view showing the preparation of crystals by the automatic growth method of the zone melting crystal of the present invention.
  • Fig. 5 is a flow chart showing the method of automatically growing a zone melting crystal of the present invention.
  • the preparation of crystals by suspension zone melting is carried out in a sealed reaction chamber filled with argon.
  • the cylindrical polycrystalline material rod 10 is vertically placed in a high temperature reaction chamber, and the end of the polycrystalline material rod is melted by the high frequency heating device 20 to produce a melting zone, wherein the melting zone portion is located above the high frequency heating device.
  • the portion of the melting zone located below the high frequency heating device is the lower melting zone 32; then the seed crystal 40 is melted into the already melted region, and the melt will be suspended in the seed by the surface tension of the molten crystal.
  • the high frequency heating device is slowly raised upward to melt the polycrystalline raw material rod above the molten crystal. At this time, the molten crystal near one end of the seed crystal starts to solidify, forming the same crystal orientation as the seed crystal.
  • the high frequency heating device sweeps across the entire polycrystalline material rod, it is converted into a single crystal ingot.
  • the automatic growth method of the zone melting crystal of the present invention is an automatic growth method using a suspension zone melting method, and the object to be achieved is to ensure the crystallization (ie, no crystal transformation occurs, resulting in failure of single crystal growth to become polycrystalline).
  • the single crystal can grow in a set shape.
  • the set shape of the single crystal should first be set; then, the growth parameters in the single crystal growth process are controlled to achieve the actual growth shape of the single crystal in accordance with the set shape of the single crystal.
  • the actual growth shape of the single crystal is consistent with the shape of the single crystal
  • Crystal falling speed, polycrystalline rotating speed, heating power and equivalent melting zone equivalent height wherein the lower melting zone equivalent height refers to the height of the cylindrical melting zone equal to the volume of the lower melting zone liquid.
  • the growth parameters closely related to the actual growth shape of the crystal include the heating power, and the relationship between the polycrystalline falling speed and the single crystal falling speed. Therefore, it is necessary to precisely control the relationship between the heating power, the polycrystalline falling speed, and the single crystal falling speed.
  • the set shape of the single crystal includes: setting a plurality of coaxial and stacked circular truncated growth intervals and growth angles of each growth interval,
  • the diameter of the bottom surface of each growth interval is larger than the diameter of the lower bottom surface, and the bottom surface of each growth interval is used as the upper layer The lower bottom surface of the long section;
  • the growth angle refers to the angle between the round busbar and the lower bottom surface, and the diameter of the bottom surface of the uppermost growth section is larger than the target diameter; that is, by configuring the multi-layer truncated cone growth interval and configuring each growth interval
  • the growth angle defines a set shape of the single crystal;
  • the bottom surface of the truncated cone growth section is the lower bottom surface, and the upper bottom surface is the upper bottom surface;
  • the automatic growth method of the zone melting crystal is given below.
  • the number of growth intervals set is 18, which are 40-80mm, 80-85mm, 85-95mm, 95-110mm, 110-130mm, 130-140mm, 140-150mm, 150-160mm, 160-165mm, 165-175mm. , 175 ⁇ 183mm, 183 ⁇ 186mm, 186 ⁇ 190mm, 190 ⁇ 194mm, 194 ⁇ 198mm, 198 ⁇ 200mm, 200 ⁇ 202mm, 202 ⁇ 204.0mm, the growth angle of the growth interval is 72 °, 78 °, 81 °, 78°, 77°, 77°, 78°, 79°, 80°, 80.5°, 81°, 83°, 85°, 86°, 87°, 88°, 89°, 90°; 90° means single crystal Growing in the axial direction, the diameter of the single crystal no longer needs to be increased; as for the number of growth intervals, the more the number, the smoother the crystal surface grown according to the
  • the truncated cone growth interval is indicated by a broken line, and is set in the range of d 0 to d 1 , and the growth angle of the single crystal in the growth interval is ⁇ 1; in the interval d 1 ⁇ d 2, the growth angle of the single crystal growing section is ⁇ 2; in d 2 ⁇ d 3 range, the growth angle of the single crystal growing section is ⁇ 3, in d 3
  • the set shape of the single crystal according to the growth interval and the growth angle of each growth interval is as shown by the solid line in FIG. 3 , wherein The lowermost column is the seed crystal;
  • the process personnel set the set value of the single crystal falling speed, the single crystal rotating speed, the polycrystalline rotating speed, and the lower melting zone equivalent height in the growth parameters of each of the growth intervals by the craftsman based on experience or conventional crystal pulling data.
  • the lower melting zone equivalent height h lqd is the height of the cylindrical molten zone equal to the liquid volume of the lower melting zone; for example, the polycrystalline rotating speed is 0.18 in the growth interval of 160.0 to 165.0 mm.
  • the single crystal rotation speed is 13.5 rpm, the single crystal falling speed is 2.5 mm/min, and the lower melting zone equivalent height is 7 mm; that is, the growth rate of the single crystal in the growth parameter is set for each growth interval, and the single crystal rotation speed is Polycrystalline rotation speed and equivalent height of the lower melting zone;
  • the curve heating technique is used to obtain the heating power as a function of the single crystal diameter; wherein the pre-stored heating power and the corresponding single crystal diameter data are obtained.
  • the record is the historical data of the heating power recorded by the computer and the corresponding single crystal diameter during the artificial extension process; that is, the growth parameter also includes the heating power, which is a function relationship of the heating power configuration;
  • a functional relationship is configured for the polycrystalline falling speed; by configuring the heating power function relationship and the polycrystalline falling speed configuration function relationship, the single crystal is grown according to the growth angle that has been configured in the growth interval.
  • the growth interval of the single crystal is the circular truncated growth interval of the layer, that is, when the single crystal When the diameter is greater than 40 mm and less than 80 mm, the growth interval of the single crystal is the lowermost growth interval; when the diameter of the single crystal is greater than 80 mm and less than 85 mm, the growth interval of the single crystal is the sub-lower growth interval; and so on;
  • the single crystal grows in the growth interval of the configured growth parameter; wherein the growth parameter includes at least the polycrystal falling speed and the heating power, and the growth of the single crystal according to the configured growth interval is adjusted according to the configured function relationship, respectively.
  • Angle growth wherein the growth angle refers to the angle between the round busbar and the lower bottom surface;
  • the diameter of the single crystal reaches the target value of 8 inches, it is switched to the automatic equal diameter growth stage.
  • the growth interval of the single crystal is the uppermost growth interval, and the single crystal grows in the axial direction in the uppermost growth interval.
  • the single crystal grows in the growth interval of the configured growth parameters, and the polycrystal falling speed and heating power in the growth parameters are respectively configured according to the configuration.
  • the adjustment of the functional relationship causes the single crystal to grow according to the growth angle at which the growth interval is arranged, so that the actual growth shape of the single crystal is close to the set shape of the single crystal, and the actual growth shape of the single crystal is predictable.
  • the actual shape of the single crystal grown by the automatic growth method of the zone melting crystal of the present invention is predictable, and the shape of the single crystal can be conveniently formed to reduce the waste of the raw material.
  • the reduced manual operation enhances the stability of the single crystal quality.
  • the function relationship of the polycrystalline falling speed has been configured as follows: Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystal, d is the diameter of the single crystal, ⁇ l is the liquid density of the crystal, ⁇ s is the solid density of the crystal, h Lqd is the equivalent height of the lower melting zone, and ⁇ is the growth angle of the single crystal that has been configured in the current growth interval, that is, the polycrystalline falling speed is closely matched with the single crystal falling speed and the configured growth angle.
  • the polycrystalline falling speed is a control parameter closely related to the crystal growth shape. By controlling the polycrystalline falling speed, precise control of the crystal growth shape can be achieved.
  • the functional relationship P f(d) of the heating power is obtained by curve fitting technique, where P is the heating power and d is the diameter of the single crystal.
  • Heating power is closely related to the actual growth shape of the crystal
  • the growth parameters require fine control, and in the relationship between the heating power obtained by the curve fitting technique and the diameter of the single crystal, the heating power continuously changes with the diameter of the single crystal, which facilitates the fine control of the heating power.
  • the curve fitting technique may use a polynomial as a fitting function.
  • the curve fitting technique may adopt a least squares fitting method.
  • the polycrystalline falling speed is adjusted according to the configured function relationship, and the function relationship of the polycrystalline falling speed has been configured as follows:
  • the polycrystalline falling speed is a control parameter closely related to the crystal growth shape. By controlling the polycrystalline falling speed, precise control of the crystal growth shape can be achieved.
  • An automatic growth system for a zone melting crystal of the present invention comprises:
  • a diameter measuring device for measuring the diameter of a single crystal
  • Polycrystalline drop servo motor for controlling the falling speed of the polycrystalline material rod
  • a high frequency heating device for heating the crystal
  • a programmable logic controller for storing the configured multi-layer truncated cone growth interval and the configured growth angle of each growth interval, wherein the growth angle refers to an angle between the truncated bus bar and the lower bottom surface; and is also used for storage a function of the configured polycrystalline falling speed, and a heating power function relationship;
  • the programmable logic controller is further configured to switch to an automatic shoulder growth stage after the diameter of the single crystal is larger than the diameter of the bottom surface of the configured lowermost truncated growth section; and is also used in the automatic shoulder growth stage.
  • the growth interval of the single crystal is determined as the growth range of the truncated cone, and is controlled according to the growth parameters of the growth interval.
  • the polycrystalline falling servo motor causes the polycrystalline falling speed to be adjusted according to a configured function relationship, while controlling the high frequency heating device such that the heating power is adjusted according to a configured function relationship;
  • the diameter reaches the target value, it switches to the automatic equal diameter growth stage to control the growth of the single crystal in the axial direction.
  • the automatic growth system of the zone melting crystal of the present invention in the automatic shoulder growth stage, when the diameter of the single crystal is larger than the diameter of the lower bottom surface of a certain circular truncated growth section and smaller than the diameter of the upper bottom surface, the programmable logic controller judges the single The growth interval of the crystal is the circular growth zone of the layer, controlling the growth of the single crystal in the growth interval of the configured growth parameters, and controlling at least the polycrystalline falling servo motor so that the polycrystalline falling speed is adjusted according to the configured function relationship. Simultaneously controlling the heating device so that the heating power is adjusted according to the configured function relationship, so that the single crystal grows according to the growth interval in which it is placed. Growth; thus, the actual growth shape of the single crystal is predictable.
  • the growth parameter further includes a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein the lower melting zone equivalent height is equal to the liquid volume of the lower melting zone.
  • the diameter measuring device is further configured to determine a diameter of the polycrystalline material rod
  • the programmable logic controller is further configured to control the polycrystalline falling servo motor, and in the automatic shoulder growth stage, the function relationship of the polycrystalline falling speed has been configured as follows: Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystal, d is the diameter of the single crystal, ⁇ l is the liquid density of the crystal, ⁇ s is the solid density of the crystal, h Lqd is the equivalent height of the lower melting zone, and ⁇ is the growth angle of the growth interval in which the single crystal is placed, that is, the polycrystalline falling speed is closely matched with the single crystal falling speed and the configured growth angle.
  • the polycrystalline falling speed is a control parameter closely related to the crystal growth shape. By controlling the polycrystalline falling speed, precise control of the crystal growth shape can be achieved.
  • the system for preparing crystals by zone melting method includes other servo motors and motors involved in motion, such as single crystal falling servo motors and single crystal falling motors, single crystal rotating servo motors and single crystal rotating motors, polycrystalline rotating servo motors and
  • a moving servo motor controls the speed of the corresponding motion by controlling a motor corresponding to the motion, such as a single crystal rotating servo motor for controlling the single crystal rotating speed by controlling the single crystal rotating motor.
  • the programmable logic controller is further configured to control the servo motor and, in an automatic equal diameter growth phase, the polycrystalline falling speed is adjusted according to a configured function relationship, and the polycrystalline falling speed has a configured function relationship.
  • V poly is the polycrystalline falling speed
  • V mono is the single crystal falling speed
  • D is the measured diameter of the polycrystalline
  • d is the diameter of the single crystal.
  • the heating power configured function relationship P f(d) is obtained by a curve fitting technique, where P is the heating power and d is the diameter of the single crystal.
  • the heating power is a growth parameter closely related to the actual growth shape of the crystal, which requires fine control.
  • the heating power continuously changes with the diameter of the single crystal. It is convenient to achieve fine control of heating power.
  • the curve fitting technique adopts a least squares fitting method.
  • the curve fitting technique uses a polynomial as a fitting function.

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Abstract

The present invention discloses an automatic zone melting crystal growth method and system. The method comprises the following steps: during an automatic diameter increasing stage, if a diameter of a single crystal is greater than a lower base surface diameter of a certain layer of truncated cone-shaped growth region and less than an upper base surface diameter thereof, then determining a growth region of the single crystal to be said layer of truncated cone-shaped growth region, and growing the single crystal in the growth region having a pre-configured growth parameter, wherein the growth parameter at least comprises a polycrystal dropping rate and a heating power; performing, according to a pre-configured function relationship, adjustment to grow the single crystal according to a pre-configured growth angle for the growth region of the single crystal, wherein the growth angle is defined as an included angle between a cone generatrix and a lower base bottom surface; and if the diameter of the single crystal reaches a target value, then switching to an automatic constant diameter growth stage, wherein the current growth region of the single crystal is in a topmost layer of growth region, and the single crystal grows along an axial direction in said growth region. A single crystal grown using the present invention has a predictable shape.

Description

区熔晶体的自动生长方法及系统Automatic growth method and system for zone melting crystal 技术领域Technical field
本发明涉及区熔晶体的生长方法及生产设备,尤其涉及一种区熔晶体的自动生长方法及系统。The invention relates to a method and a production device for growing a zone melting crystal, in particular to a method and a system for automatically growing a zone melting crystal.
背景技术Background technique
近年来,区熔单晶硅晶体生长的工艺水平有了大幅提高,已经具备人工拉制8英寸单晶的水平。区熔法生长单晶的工艺过程主要由预热、化料、引晶、扩肩、等径、收尾组成。对于大尺寸单晶来讲,采用全人工方式进行拉晶有着显著的缺点,主要体现在大尺寸单晶拉制时间过长,量产难度大;人为影响因素大,生长过程难以控制;单晶质量一致性差等。In recent years, the process level of zone melting single crystal silicon crystal growth has been greatly improved, and the level of artificially drawn 8-inch single crystal has been obtained. The process of growing single crystal by zone melting method mainly consists of preheating, chemical compounding, seeding, expanding shoulder, equal diameter and closing. For large-size single crystals, the use of full manual method for pulling crystal has significant shortcomings, mainly reflected in the long drawing time of large-size single crystal, and the mass production is difficult; the human influence factor is large, and the growth process is difficult to control; Poor quality consistency.
为解决上述问题,现有技术中出现了自动生产单晶的方法,可以实现扩肩和等径生长阶段的自动生长,但是存在单晶实际生长形状只能在生长完成后才能知道,单晶生长形状无法预先设定的技术问题。In order to solve the above problems, a method for automatically producing a single crystal has appeared in the prior art, and automatic growth of the shoulder and equal diameter growth stages can be realized, but the actual growth shape of the single crystal can only be known after the growth is completed, and the single crystal growth is known. A technical problem that the shape cannot be preset.
发明内容Summary of the invention
本发明提供了一种区熔晶体的自动生长方法及系统,与现有技术相比,解决了生长的单晶的形状无法预知的技术问题。The invention provides an automatic growth method and system for a zone melting crystal, which solves the technical problem that the shape of the grown single crystal is unpredictable compared with the prior art.
一方面,本发明提供区熔晶体的自动生长方法,包括如下步骤:In one aspect, the present invention provides an automatic growth method for a zone melting crystal, comprising the steps of:
人工引晶及扩肩,形成单晶;当单晶的直径大于已配置的多层圆台形生长区间的最下层圆台形生长区间下底面的直径后,切换至自动扩肩生长阶段;Manually seeding and expanding the shoulder to form a single crystal; when the diameter of the single crystal is larger than the diameter of the bottom surface of the lowermost truncated growth section of the configured multi-layer truncated cone growth section, switching to the automatic shoulder growth stage;
在自动扩肩生长阶段,当单晶的直径大于某层圆台形生长区间的下底面直径且小于上底面直径时,单晶所处的生长区间即为该层圆台形生长区间;单晶在所处的已配置生长参数的生长区间生长;其中,生长参数至少包括多晶下降速度和加热功率,分别按照已配置的函数关系调整使单晶按照所处的生长区间已配置的生长角度生长;其中,生长角度指的是圆台母线与下底面之间的夹角;In the automatic shoulder growth stage, when the diameter of the single crystal is larger than the diameter of the lower bottom surface of a certain circular truncated growth section and smaller than the diameter of the upper bottom surface, the growth interval of the single crystal is the circular truncated growth interval of the layer; a growing interval growth of the configured growth parameter; wherein the growth parameter includes at least a polycrystalline falling speed and a heating power, respectively adjusted according to a configured functional relationship, so that the single crystal grows according to a growth angle in which the growth interval is configured; The growth angle refers to the angle between the round busbar and the lower bottom surface;
当单晶的直径达到目标值时,切换至自动等径生长阶段,此时,单晶所处的生长区间是最上层的生长区间,单晶在该生长区间沿轴向生长。When the diameter of the single crystal reaches the target value, it is switched to the automatic equal diameter growth stage. At this time, the growth interval in which the single crystal is located is the growth interval of the uppermost layer, and the single crystal grows in the axial direction in the growth interval.
优选的,所述生长参数还包括单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度,其中,下熔区等效高度指的是与下熔区液体体积相等的圆柱形熔区的高度。 Preferably, the growth parameter further includes a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein the lower melting zone equivalent height is equal to the liquid volume of the lower melting zone. The height of the cylindrical melting zone.
优选的,在自动扩肩生长阶段,多晶下降速度已配置的函数关系具体为:
Figure PCTCN2015092868-appb-000001
其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径,ρl为晶体的液态密度,ρs为晶体的固态密度,hlqd为下熔区等效高度,θ为单晶所处的生长区间已配置的生长角度。
Preferably, in the automatic shoulder growth stage, the functional relationship that the polycrystalline falling speed has been configured is specifically:
Figure PCTCN2015092868-appb-000001
Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystal, d is the diameter of the single crystal, ρ l is the liquid density of the crystal, ρ s is the solid density of the crystal, h Lqd is the equivalent height of the lower melting zone, and θ is the configured growth angle of the growth zone in which the single crystal is located.
优选的,在自动等径生长阶段,多晶下降速度按照已配置的函数关系调整,函数关系具体为:
Figure PCTCN2015092868-appb-000002
其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径。
Preferably, in the automatic equal diameter growth stage, the polycrystalline falling speed is adjusted according to the configured function relationship, and the functional relationship is specifically:
Figure PCTCN2015092868-appb-000002
Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystalline, and d is the diameter of the single crystal.
优选的,在自动扩肩生长阶段,加热功率已配置的函数关系P=f(d)是采用曲线拟合技术得到的,其中,P为加热功率,d为单晶的直径。Preferably, in the automatic shoulder growth phase, the functional relationship P = f(d) of the heating power is obtained by a curve fitting technique, wherein P is the heating power and d is the diameter of the single crystal.
优选的,所述曲线拟合技术采用多项式作为拟合函数。Preferably, the curve fitting technique employs a polynomial as a fitting function.
优选的,所述曲线拟合技术采用最小二乘拟合方法。Preferably, the curve fitting technique employs a least squares fitting method.
另一方面,本发明还提供一种区熔晶体的自动生长系统,包括:In another aspect, the present invention also provides an automatic growth system for a zone melting crystal, comprising:
直径测量设备,用于测定单晶的直径;a diameter measuring device for measuring the diameter of a single crystal;
多晶下降伺服电机,用于控制多晶原料棒的下降速度;Polycrystalline drop servo motor for controlling the falling speed of the polycrystalline material rod;
高频加热设备,用于对晶体进行加热;a high frequency heating device for heating the crystal;
可编程逻辑控制器,用于存储已配置的多层圆台形生长区间和各生长区间已配置的生长角度,其中,生长角度指的是圆台母线与下底面之间的夹角;还用于存储已配置的多晶下降速度的函数关系,以及加热功率函数关系;a programmable logic controller for storing the configured multi-layer truncated cone growth interval and the configured growth angle of each growth interval, wherein the growth angle refers to an angle between the truncated bus bar and the lower bottom surface; and is also used for storage a function of the configured polycrystalline falling speed, and a heating power function relationship;
所述可编程逻辑控制器还用于在单晶的直径大于已配置的最下层圆台形生长区间下底面的直径后,切换至自动扩肩生长阶段;还用于在自动扩肩生长阶段,当单晶的直径大于某层圆台形生长区间的下底面直径且小于上底面直径时,判断单晶所处的生长区间即为该层圆台形生长区间,并按该生长区间已配置的生长参数控制单晶生长,其中,至少控制多晶下降伺服电机使得多晶下降速度按照已配置的函数关系调整,同时控制高频加热设备使得加热功率按照已配置的函数关系调整;还用于在单晶的直径达到目标值时,切换至自动等径生长阶段,控制单晶沿轴向生长。The programmable logic controller is further configured to switch to an automatic shoulder growth stage after the diameter of the single crystal is larger than the diameter of the bottom surface of the configured lowermost truncated growth section; and is also used in the automatic shoulder growth stage. When the diameter of the single crystal is larger than the diameter of the lower surface of the growth section of a certain circular trough and smaller than the diameter of the upper surface, the growth interval of the single crystal is determined as the growth range of the truncated cone, and is controlled according to the growth parameters of the growth interval. Single crystal growth, wherein at least controlling the polycrystalline falling servo motor causes the polycrystalline falling speed to be adjusted according to a configured function relationship, while controlling the high frequency heating device such that the heating power is adjusted according to a configured function relationship; When the diameter reaches the target value, it switches to the automatic equal diameter growth stage to control the growth of the single crystal in the axial direction.
优选的,所述生长参数还包括单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度,其中,下熔区等效高度指的是与下熔区液体体积相等的圆柱形熔区的高度。Preferably, the growth parameter further includes a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein the lower melting zone equivalent height is equal to the liquid volume of the lower melting zone. The height of the cylindrical melting zone.
优选的,所述直径测量设备还用于测定多晶原料棒的直径;Preferably, the diameter measuring device is further used to determine the diameter of the polycrystalline material rod;
所述可编程逻辑控制器,还用于控制所述多晶下降伺服电机,且在自动扩肩生长阶段, 所述多晶下降速度已配置的函数关系具体为:
Figure PCTCN2015092868-appb-000003
其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径,ρl为晶体的液态密度,ρs为晶体的固态密度,hlqd为下熔区等效高度,θ为单晶所处的生长区间已配置的生长角度。
The programmable logic controller is further configured to control the polycrystalline falling servo motor, and in the automatic shoulder growth stage, the function relationship of the polycrystalline falling speed has been configured as follows:
Figure PCTCN2015092868-appb-000003
Wherein, V poly polycrystalline lowering speed, V mono monocrystalline lowering speed, D is the measured diameter polycrystalline, d is the diameter of a single crystal, ρ l is the density of the liquid crystal, ρ s is the solid state density crystals, h Lqd is the equivalent height of the lower melting zone, and θ is the configured growth angle of the growth zone in which the single crystal is located.
优选的,所述直径测量设备还用于测定多晶原料棒的直径;Preferably, the diameter measuring device is further used to determine the diameter of the polycrystalline material rod;
所述可编程逻辑控制器,还用于控制所述伺服电机且在自动等径生长阶段,多晶下降速度按照已配置的函数关系调整,所述多晶下降速度已配置的函数关系具体为
Figure PCTCN2015092868-appb-000004
其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径。
The programmable logic controller is further configured to control the servo motor and, in an automatic equal diameter growth phase, the polycrystalline falling speed is adjusted according to a configured function relationship, and the function relationship of the polycrystalline falling speed configured is specifically
Figure PCTCN2015092868-appb-000004
Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystalline, and d is the diameter of the single crystal.
优选的,在自动扩肩生长阶段,加热功率已配置的函数关系P=f(d)是采用曲线拟合技术得到的,其中,P为加热功率,d为单晶的直径。Preferably, in the automatic shoulder growth phase, the functional relationship P = f(d) of the heating power is obtained by a curve fitting technique, wherein P is the heating power and d is the diameter of the single crystal.
优选的,所述曲线拟合技术,采用多项式作为拟合函数。Preferably, the curve fitting technique uses a polynomial as a fitting function.
优选的,所述曲线拟合技术,采用最小二乘拟合方法。Preferably, the curve fitting technique employs a least squares fitting method.
本发明的区熔晶体的自动生长方法及系统,在自动扩肩生长阶段,单晶在所处的已配置生长参数的生长区间生长,生长参数中的多晶下降速度和加热功率分别按照已配置的函数关系调整使单晶按照所处的生长区间已配置的生长角度生长,这样,使单晶实际生长形状是可以预知的。与现有技术相比,本发明的区熔晶体的自动生长方法及系统生长的单晶的实际形状是可以预知的,进而可以方便的形成符合所需的单晶的形状,减少了原料的浪费,同时减少了的人工操作,增强了单晶质量的稳定性。In the automatic growth method and system for the zone melting crystal of the present invention, in the automatic shoulder growth stage, the single crystal grows in the growth interval of the configured growth parameters, and the polycrystal falling speed and heating power in the growth parameters are respectively configured according to the configuration. The functional relationship adjustment causes the single crystal to grow in accordance with the growth angle at which the growth interval is disposed, so that the actual growth shape of the single crystal is predictable. Compared with the prior art, the automatic growth method of the zone melting crystal of the present invention and the actual shape of the single crystal grown by the system are predictable, and the shape of the single crystal can be conveniently formed to reduce the waste of raw materials. At the same time, the manual operation is reduced, and the stability of the single crystal quality is enhanced.
附图说明DRAWINGS
为了更清楚地说明本发明实施例中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings to be used in the embodiments will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the present invention. Those skilled in the art can also obtain other drawings based on these drawings without paying any creative work.
图1为利用悬浮区熔法制备晶体的示意图;Figure 1 is a schematic view showing the preparation of crystals by a suspension zone melting method;
图2为本发明的区熔晶体的自动生长方法中已配置的多层圆台形生长区间及每个圆台形生长区间已配置的生长角度的示意图;2 is a schematic view showing a configuration of a multi-layered truncated cone growth section and a growth angle of each truncated cone growth section in the automatic growth method of the zone melting crystal of the present invention;
图3为按照图2所示的已配置的多层圆台形生长区间及每个圆台形生长区间已配置的生长角度生长的单晶的示意图; 3 is a schematic view of a single-crystal truncated cone growth section shown in FIG. 2 and a growth angle grown single crystal in each truncated cone growth section;
图4为本发明的区熔晶体的自动生长方法制备晶体的示意图;4 is a schematic view showing the preparation of crystals by the automatic growth method of the zone melting crystal of the present invention;
图5为本发明的区熔晶体的自动生长方法的流程图。Fig. 5 is a flow chart showing the method of automatically growing a zone melting crystal of the present invention.
附图标记说明:Description of the reference signs:
10多晶原料棒,20加热设备,31上熔区,32下熔区,40籽晶。10 polycrystalline raw material rods, 20 heating equipment, 31 upper melting zone, 32 lower melting zone, 40 seed crystals.
具体实施方式detailed description
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention are clearly and completely described in the following with reference to the accompanying drawings in the embodiments of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, but not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative efforts are within the scope of the present invention.
如图1所示,利用悬浮区熔法制备晶体是在充满氩气的密封反应室中进行的。首先将圆柱形多晶原料棒10垂直放置在高温反应室里,用高频加热设备20将多晶原料棒的末端融化,产生一熔区,其中,位于高频加热设备之上的熔区部分为上熔区31,位于高频加热设备之下的熔区部分为下熔区32;然后把籽晶40熔入已经熔化的区域,熔体将会藉着熔融晶体的表面张力而悬浮在籽晶与多晶原料棒之间;之后,高频加热设备缓慢向上升高而把熔融晶体上方部分的多晶原料棒熔化。此时靠近籽晶的一端熔融晶体开始凝固,形成与籽晶相同的晶向。当高频加热设备扫过整个多晶原料棒后,使其转变成单晶的晶棒。As shown in Figure 1, the preparation of crystals by suspension zone melting is carried out in a sealed reaction chamber filled with argon. First, the cylindrical polycrystalline material rod 10 is vertically placed in a high temperature reaction chamber, and the end of the polycrystalline material rod is melted by the high frequency heating device 20 to produce a melting zone, wherein the melting zone portion is located above the high frequency heating device. For the upper melting zone 31, the portion of the melting zone located below the high frequency heating device is the lower melting zone 32; then the seed crystal 40 is melted into the already melted region, and the melt will be suspended in the seed by the surface tension of the molten crystal. Between the crystal and the polycrystalline raw material rod; thereafter, the high frequency heating device is slowly raised upward to melt the polycrystalline raw material rod above the molten crystal. At this time, the molten crystal near one end of the seed crystal starts to solidify, forming the same crystal orientation as the seed crystal. When the high frequency heating device sweeps across the entire polycrystalline material rod, it is converted into a single crystal ingot.
本发明的区熔晶体的自动生长方法,是利用悬浮区熔法的自动生长方法,要实现的目标是在保证成晶(即不发生晶变,导致单晶生长失败变为多晶)的前提条件下,在自动扩肩生长阶段和自动等径生长阶段中,单晶能够按照设定的形状生长。为了实现这个目标,首先应该设置单晶的设定形状;然后,通过对单晶生长过程中的生长参数加以控制以实现单晶实际生长形状与单晶的设定形状一致。为了实现单晶实际生长形状与单晶设定形状一致,需要对利用悬浮区熔法制备晶体的单晶生长过程中的多个生长参数进行控制,包括单晶下降速度,单晶旋转速度,多晶下降速度,多晶旋转速度,加热功率和下熔区等效高度,其中,下熔区等效高度指的是与下熔区液体体积相等的圆柱形熔区的高度。与晶体实际生长形状密切相关的生长参数包括加热功率,以及多晶下降速度和单晶下降速度之间的配合关系。因此,需要对加热功率,多晶下降速度和单晶下降速度之间的配合关系进行精确控制。The automatic growth method of the zone melting crystal of the present invention is an automatic growth method using a suspension zone melting method, and the object to be achieved is to ensure the crystallization (ie, no crystal transformation occurs, resulting in failure of single crystal growth to become polycrystalline). Under the conditions, in the automatic shoulder growth stage and the automatic equal diameter growth stage, the single crystal can grow in a set shape. In order to achieve this goal, the set shape of the single crystal should first be set; then, the growth parameters in the single crystal growth process are controlled to achieve the actual growth shape of the single crystal in accordance with the set shape of the single crystal. In order to realize that the actual growth shape of the single crystal is consistent with the shape of the single crystal, it is necessary to control a plurality of growth parameters in the single crystal growth process of the crystal prepared by the suspension zone melting method, including the single crystal falling speed, the single crystal rotation speed, and the like. Crystal falling speed, polycrystalline rotating speed, heating power and equivalent melting zone equivalent height, wherein the lower melting zone equivalent height refers to the height of the cylindrical melting zone equal to the volume of the lower melting zone liquid. The growth parameters closely related to the actual growth shape of the crystal include the heating power, and the relationship between the polycrystalline falling speed and the single crystal falling speed. Therefore, it is necessary to precisely control the relationship between the heating power, the polycrystalline falling speed, and the single crystal falling speed.
在利用区熔晶体的自动生长方法生长单晶之前,首先,需要设置单晶的设定形状,具体包括:设置多个同轴且层叠排列的圆台形生长区间和每个生长区间的生长角度,每一层生长区间上底面的直径大于下底面的直径且每一层生长区间上底面作为上一层圆台形生 长区间的下底面;其中,生长角度指的是圆台母线与下底面之间的夹角,最上层生长区间上底面的直径大于目标直径;即通过配置多层圆台形生长区间和配置各生长区间的生长角度,限定了单晶的设定形状;圆台形生长区间位于下方的底面为下底面,位于上方的底面为上底面;Before the single crystal is grown by the automatic growth method of the zone melting crystal, firstly, it is necessary to set the set shape of the single crystal, and specifically includes: setting a plurality of coaxial and stacked circular truncated growth intervals and growth angles of each growth interval, The diameter of the bottom surface of each growth interval is larger than the diameter of the lower bottom surface, and the bottom surface of each growth interval is used as the upper layer The lower bottom surface of the long section; wherein, the growth angle refers to the angle between the round busbar and the lower bottom surface, and the diameter of the bottom surface of the uppermost growth section is larger than the target diameter; that is, by configuring the multi-layer truncated cone growth interval and configuring each growth interval The growth angle defines a set shape of the single crystal; the bottom surface of the truncated cone growth section is the lower bottom surface, and the upper bottom surface is the upper bottom surface;
下面给出区熔晶体的自动生长方法生长直径为8英寸(1英寸=25.4mm,其中,mm为毫米)的单晶硅时,配置18层圆台形生长区间和各生长区间的生长角度以限定了单晶的设定形状的实例,需要说明的是,在本实施例中,区熔晶体的自动生长方法生长单晶硅仅用于举例,区熔晶体的自动生长方法不限于生长单晶硅,还可以是其他单晶晶体。设置的生长区间数量为18个,依次为40~80mm,80~85mm,85~95mm,95~110mm,110~130mm,130~140mm,140~150mm,150~160mm,160~165mm,165~175mm,175~183mm,183~186mm,186~190mm,190~194mm,194~198mm,198~200mm,200~202mm,202~204.0mm,生长区间的生长角度依次为72°,78°,81°,78°,77°,77°,78°,79°,80°,80.5°,81°,83°,85°,86°,87°,88°,89°,90°;90°表示单晶沿轴向生长,单晶的直径不再需要增大;关于生长区间的数量,数量越多则按照生长区间的生长角度生长出的晶体表面越光滑;The automatic growth method of the zone melting crystal is given below. When a single crystal silicon having a diameter of 8 inches (1 inch = 25.4 mm, wherein mm is a millimeter) is grown, an 18-layer truncated cone growth interval and growth angles of the respective growth intervals are arranged to define An example of the set shape of the single crystal, it should be noted that in the present embodiment, the method of automatically growing the region-melting crystal grows single crystal silicon for example only, and the method for automatically growing the crystal-melting crystal is not limited to growing single crystal silicon. It can also be other single crystal crystals. The number of growth intervals set is 18, which are 40-80mm, 80-85mm, 85-95mm, 95-110mm, 110-130mm, 130-140mm, 140-150mm, 150-160mm, 160-165mm, 165-175mm. , 175 ~ 183mm, 183 ~ 186mm, 186 ~ 190mm, 190 ~ 194mm, 194 ~ 198mm, 198 ~ 200mm, 200 ~ 202mm, 202 ~ 204.0mm, the growth angle of the growth interval is 72 °, 78 °, 81 °, 78°, 77°, 77°, 78°, 79°, 80°, 80.5°, 81°, 83°, 85°, 86°, 87°, 88°, 89°, 90°; 90° means single crystal Growing in the axial direction, the diameter of the single crystal no longer needs to be increased; as for the number of growth intervals, the more the number, the smoother the crystal surface grown according to the growth angle of the growth interval;
为了图示方便,在图2中,仅以四段圆台形生长区间为例,圆台形生长区间用虚线表示,设定在d0~d1区间内,该生长区间内单晶的生长角度为θ1;在d1~d2区间内,该生长区间内单晶的生长角度为θ2;在d2~d3区间内,该生长区间内单晶的生长角度为θ3,在d3~d4区间内,该生长区间内单晶的生长角度为θ4=90°,按照生长区间和每个生长区间的生长角度的单晶的设定形状如图3中实线所示,其中,最下端的细柱是籽晶;For convenience of illustration, in FIG. 2, only the four-stage truncated cone growth interval is taken as an example, and the truncated cone growth interval is indicated by a broken line, and is set in the range of d 0 to d 1 , and the growth angle of the single crystal in the growth interval is θ 1; in the interval d 1 ~ d 2, the growth angle of the single crystal growing section is θ 2; in d 2 ~ d 3 range, the growth angle of the single crystal growing section is θ 3, in d 3 In the interval of -d 4 , the growth angle of the single crystal in the growth interval is θ 4 = 90°, and the set shape of the single crystal according to the growth interval and the growth angle of each growth interval is as shown by the solid line in FIG. 3 , wherein The lowermost column is the seed crystal;
之后,由工艺人员依据经验或以往拉晶数据,为每个所述生长区间的生长参数中的单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度设置设定值,其中,如图4所示,下熔区等效高度hlqd是与下熔区液体体积相等的圆柱形熔区的高度;例如,在生长区间160.0~165.0mm内,多晶旋转速度为0.18rpm,单晶旋转速度为13.5rpm,单晶下降速度为2.5mm/min,下熔区等效高度7mm;即为每个生长区间配置了生长参数中的单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度;Thereafter, the process personnel set the set value of the single crystal falling speed, the single crystal rotating speed, the polycrystalline rotating speed, and the lower melting zone equivalent height in the growth parameters of each of the growth intervals by the craftsman based on experience or conventional crystal pulling data. , wherein, as shown in FIG. 4, the lower melting zone equivalent height h lqd is the height of the cylindrical molten zone equal to the liquid volume of the lower melting zone; for example, the polycrystalline rotating speed is 0.18 in the growth interval of 160.0 to 165.0 mm. Rpm, the single crystal rotation speed is 13.5 rpm, the single crystal falling speed is 2.5 mm/min, and the lower melting zone equivalent height is 7 mm; that is, the growth rate of the single crystal in the growth parameter is set for each growth interval, and the single crystal rotation speed is Polycrystalline rotation speed and equivalent height of the lower melting zone;
之后,根据预先存储的加热功率及对应的单晶直径的数据记录,采用曲线拟合技术,得到加热功率与单晶直径的函数关系;其中,预先存储的加热功率及对应的单晶直径的数据记录是以往人工扩肩过程中,计算机记录的加热功率及对应的单晶直径的历史数据;即生长参数还包括加热功率,为加热功率配置的函数关系; Then, according to the pre-stored heating power and the corresponding single crystal diameter data record, the curve heating technique is used to obtain the heating power as a function of the single crystal diameter; wherein the pre-stored heating power and the corresponding single crystal diameter data are obtained. The record is the historical data of the heating power recorded by the computer and the corresponding single crystal diameter during the artificial extension process; that is, the growth parameter also includes the heating power, which is a function relationship of the heating power configuration;
最后,为多晶下降速度配置函数关系;通过对加热功率函数关系和多晶下降速度配置函数关系配置,实现单晶按照所处的生长区间已配置的生长角度生长。Finally, a functional relationship is configured for the polycrystalline falling speed; by configuring the heating power function relationship and the polycrystalline falling speed configuration function relationship, the single crystal is grown according to the growth angle that has been configured in the growth interval.
下面给出利用区熔法制备晶体的方法生长等径处的直径为8英寸(1英寸=25.4mm,其中,mm为毫米)的单晶的步骤:如图5所示,The following is a method for preparing a crystal by a zone melting method: a step of growing a single crystal having a diameter of 8 inches (1 inch = 25.4 mm, wherein mm is a millimeter) at an equal diameter: as shown in FIG.
人工引晶及扩肩,形成单晶;当单晶的直径大于已配置的多层圆台形生长区间的最下层圆台形生长区间下底面的直径40mm后,切换至自动扩肩生长阶段;Manually seeding and expanding the shoulder to form a single crystal; when the diameter of the single crystal is larger than the diameter of the bottom surface of the lowermost truncated cone growth section of the configured multi-layer truncated cone growth section, the surface is switched to the automatic shoulder growth stage;
在自动扩肩生长阶段,当单晶的直径大于某层圆台形生长区间的下底面直径且小于上底面直径时,单晶所处的生长区间即为该层圆台形生长区间,即当单晶的直径大于40mm且小于80mm时,单晶所处的生长区间为最下层生长区间;当单晶的直径大于80mm且小于85mm时,单晶所处的生长区间为次下层生长区间;依次类推;单晶在所处的已配置生长参数的生长区间生长;其中,生长参数至少包括多晶下降速度和加热功率,分别按照已配置的函数关系调整使单晶按照所处的生长区间已配置的生长角度生长;其中,生长角度指的是圆台母线与下底面之间的夹角;In the automatic shoulder growth stage, when the diameter of the single crystal is larger than the diameter of the lower bottom surface of a certain circular truncated growth section and smaller than the diameter of the upper bottom surface, the growth interval of the single crystal is the circular truncated growth interval of the layer, that is, when the single crystal When the diameter is greater than 40 mm and less than 80 mm, the growth interval of the single crystal is the lowermost growth interval; when the diameter of the single crystal is greater than 80 mm and less than 85 mm, the growth interval of the single crystal is the sub-lower growth interval; and so on; The single crystal grows in the growth interval of the configured growth parameter; wherein the growth parameter includes at least the polycrystal falling speed and the heating power, and the growth of the single crystal according to the configured growth interval is adjusted according to the configured function relationship, respectively. Angle growth; wherein the growth angle refers to the angle between the round busbar and the lower bottom surface;
当单晶的直径达到目标值8英寸时,切换至自动等径生长阶段,此时,单晶所处的生长区间是最上层生长区间,单晶在最上层生长区间沿轴向生长。When the diameter of the single crystal reaches the target value of 8 inches, it is switched to the automatic equal diameter growth stage. At this time, the growth interval of the single crystal is the uppermost growth interval, and the single crystal grows in the axial direction in the uppermost growth interval.
本发明的利用区熔法制备晶体的方法,在自动扩肩生长阶段,单晶在所处的已配置生长参数的生长区间生长,生长参数中的多晶下降速度和加热功率分别按照已配置的函数关系调整使单晶按照所处的生长区间已配置的生长角度生长,这样,即单晶实际生长形状与单晶的设定形状比较接近,单晶实际生长形状是可以预知的。现有技术中,在单晶的生长过程中,无法预知得到的是什么形状的单晶。与现有技术相比,本发明的区熔晶体的自动生长方法生长的单晶的实际形状是可以预知的,进而可以方便的形成符合所需的单晶的形状,减少了原料的浪费,同时减少了的人工操作,增强了单晶质量的稳定性。In the method for preparing crystals by the zone melting method of the present invention, in the automatic shoulder growth stage, the single crystal grows in the growth interval of the configured growth parameters, and the polycrystal falling speed and heating power in the growth parameters are respectively configured according to the configuration. The adjustment of the functional relationship causes the single crystal to grow according to the growth angle at which the growth interval is arranged, so that the actual growth shape of the single crystal is close to the set shape of the single crystal, and the actual growth shape of the single crystal is predictable. In the prior art, it is impossible to predict what shape a single crystal is obtained during the growth of a single crystal. Compared with the prior art, the actual shape of the single crystal grown by the automatic growth method of the zone melting crystal of the present invention is predictable, and the shape of the single crystal can be conveniently formed to reduce the waste of the raw material. The reduced manual operation enhances the stability of the single crystal quality.
具体的,在自动扩肩生长阶段,多晶下降速度已配置的函数关系具体为:
Figure PCTCN2015092868-appb-000005
其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径,ρl为晶体的液态密度,ρs为晶体的固态密度,hlqd为下熔区等效高度,θ为当前生长区间已配置的单晶的生长角度,即多晶下降速度与单晶下降速度及已配置的生长角度之间是紧密配合的。多晶下降速度是与晶体生长形状密切相关的控制参数,通过控制多晶下降速度,可以实现晶体生长形状的精确控制。
Specifically, in the automatic shoulder growth stage, the function relationship of the polycrystalline falling speed has been configured as follows:
Figure PCTCN2015092868-appb-000005
Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystal, d is the diameter of the single crystal, ρ l is the liquid density of the crystal, ρ s is the solid density of the crystal, h Lqd is the equivalent height of the lower melting zone, and θ is the growth angle of the single crystal that has been configured in the current growth interval, that is, the polycrystalline falling speed is closely matched with the single crystal falling speed and the configured growth angle. The polycrystalline falling speed is a control parameter closely related to the crystal growth shape. By controlling the polycrystalline falling speed, precise control of the crystal growth shape can be achieved.
在自动扩肩生长阶段,加热功率已配置的函数关系P=f(d)是采用曲线拟合技术得到的,其中,P为加热功率,d为单晶的直径。加热功率,是与晶体实际生长形状密切相关 的生长参数,需要精细化控制,而在采用曲线拟合技术得到的加热功率与单晶的直径的函数关系中,加热功率随单晶的直径连续变化,便于实现加热功率的精细化控制。In the automatic shoulder growth phase, the functional relationship P = f(d) of the heating power is obtained by curve fitting technique, where P is the heating power and d is the diameter of the single crystal. Heating power is closely related to the actual growth shape of the crystal The growth parameters require fine control, and in the relationship between the heating power obtained by the curve fitting technique and the diameter of the single crystal, the heating power continuously changes with the diameter of the single crystal, which facilitates the fine control of the heating power.
具体的,所述曲线拟合技术可以采用多项式作为拟合函数。Specifically, the curve fitting technique may use a polynomial as a fitting function.
具体的,所述曲线拟合技术可以采用最小二乘拟合方法。Specifically, the curve fitting technique may adopt a least squares fitting method.
进一步的,在本实施例中,通过曲线拟合得到的单晶的加热功率与单晶直径的函数关系为:P=f(d)=-2.871×10-8d4+1.273×10-5d3-2.089×10-3d2+0.4116d+29.76;其中,P为加热功率,d为单晶的直径。Further, in the present embodiment, the heating power of the single crystal obtained by curve fitting is a function of the diameter of the single crystal: P = f (d) = - 2.871 × 10 -8 d 4 + 1.273 × 10 -5 d 3 -2.089×10 -3 d 2 +0.4116d+29.76; wherein P is the heating power and d is the diameter of the single crystal.
具体的,在自动等径生长阶段,多晶下降速度按照已配置的函数关系调整,多晶下降速度已配置的函数关系具体为:
Figure PCTCN2015092868-appb-000006
多晶下降速度是与晶体生长形状密切相关的控制参数,通过控制多晶下降速度,可以实现晶体生长形状的精确控制。
Specifically, in the automatic equal diameter growth stage, the polycrystalline falling speed is adjusted according to the configured function relationship, and the function relationship of the polycrystalline falling speed has been configured as follows:
Figure PCTCN2015092868-appb-000006
The polycrystalline falling speed is a control parameter closely related to the crystal growth shape. By controlling the polycrystalline falling speed, precise control of the crystal growth shape can be achieved.
最后,当单晶的长度达到目标值后,结束自动等径生长阶段,人工进行收尾。Finally, when the length of the single crystal reaches the target value, the automatic equal diameter growth stage is ended, and the finishing is performed manually.
本发明的一种区熔晶体的自动生长系统,包括:An automatic growth system for a zone melting crystal of the present invention comprises:
直径测量设备,用于测定单晶的直径;a diameter measuring device for measuring the diameter of a single crystal;
多晶下降伺服电机,用于控制多晶原料棒的下降速度;Polycrystalline drop servo motor for controlling the falling speed of the polycrystalline material rod;
高频加热设备,用于对晶体进行加热;a high frequency heating device for heating the crystal;
可编程逻辑控制器,用于存储已配置的多层圆台形生长区间和各生长区间已配置的生长角度,其中,生长角度指的是圆台母线与下底面之间的夹角;还用于存储已配置的多晶下降速度的函数关系,以及加热功率函数关系;a programmable logic controller for storing the configured multi-layer truncated cone growth interval and the configured growth angle of each growth interval, wherein the growth angle refers to an angle between the truncated bus bar and the lower bottom surface; and is also used for storage a function of the configured polycrystalline falling speed, and a heating power function relationship;
所述可编程逻辑控制器还用于在单晶的直径大于已配置的最下层圆台形生长区间下底面的直径后,切换至自动扩肩生长阶段;还用于在自动扩肩生长阶段,当单晶的直径大于某层圆台形生长区间的下底面直径且小于上底面直径时,判断单晶所处的生长区间即为该层圆台形生长区间,并按该生长区间已配置的生长参数控制单晶生长,其中,至少控制多晶下降伺服电机使得多晶下降速度按照已配置的函数关系调整,同时控制高频加热设备使得加热功率按照已配置的函数关系调整;还用于在单晶的直径达到目标值时,切换至自动等径生长阶段,控制单晶沿轴向生长。The programmable logic controller is further configured to switch to an automatic shoulder growth stage after the diameter of the single crystal is larger than the diameter of the bottom surface of the configured lowermost truncated growth section; and is also used in the automatic shoulder growth stage. When the diameter of the single crystal is larger than the diameter of the lower surface of the growth section of a certain circular trough and smaller than the diameter of the upper surface, the growth interval of the single crystal is determined as the growth range of the truncated cone, and is controlled according to the growth parameters of the growth interval. Single crystal growth, wherein at least controlling the polycrystalline falling servo motor causes the polycrystalline falling speed to be adjusted according to a configured function relationship, while controlling the high frequency heating device such that the heating power is adjusted according to a configured function relationship; When the diameter reaches the target value, it switches to the automatic equal diameter growth stage to control the growth of the single crystal in the axial direction.
本发明的区熔晶体的自动生长系统,在自动扩肩生长阶段,当单晶的直径大于某层圆台形生长区间的下底面直径且小于上底面直径时,所述可编程逻辑控制器判断单晶所处的生长区间为该层圆台形生长区间,控制单晶在所处的已配置生长参数的生长区间生长,至少控制多晶下降伺服电机使得多晶下降速度按照已配置的函数关系调整,同时控制加热设备使得加热功率按照已配置的函数关系调整,使单晶按照所处的生长区间已配置的生长角 度生长;这样,单晶实际生长形状是可以预知的。现有技术中,在单晶的生长过程中,无法预知得到的是什么形状的单晶。与现有技术相比,本发明的区熔晶体的自动生长系统生长的单晶的实际形状是可以预知的,进而可以方便的形成符合所需的单晶的形状,减少了原料的浪费,同时减少了的人工操作,增强了单晶质量的稳定性。The automatic growth system of the zone melting crystal of the present invention, in the automatic shoulder growth stage, when the diameter of the single crystal is larger than the diameter of the lower bottom surface of a certain circular truncated growth section and smaller than the diameter of the upper bottom surface, the programmable logic controller judges the single The growth interval of the crystal is the circular growth zone of the layer, controlling the growth of the single crystal in the growth interval of the configured growth parameters, and controlling at least the polycrystalline falling servo motor so that the polycrystalline falling speed is adjusted according to the configured function relationship. Simultaneously controlling the heating device so that the heating power is adjusted according to the configured function relationship, so that the single crystal grows according to the growth interval in which it is placed. Growth; thus, the actual growth shape of the single crystal is predictable. In the prior art, it is impossible to predict what shape a single crystal is obtained during the growth of a single crystal. Compared with the prior art, the actual shape of the single crystal grown by the automatic growth system of the zone melting crystal of the present invention is predictable, and the shape of the single crystal can be conveniently formed to reduce the waste of the raw material. The reduced manual operation enhances the stability of the single crystal quality.
具体的,所述生长参数还包括单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度,其中,下熔区等效高度指的是与下熔区液体体积相等的圆柱形熔区的高度;由工艺人员依据经验或以往拉晶数据,为每个所述生长区间的生长参数中的单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度设置设定值。Specifically, the growth parameter further includes a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein the lower melting zone equivalent height is equal to the liquid volume of the lower melting zone. The height of the cylindrical melting zone; the growth rate of the single crystal in the growth parameters of each of the growth intervals, the rotation speed of the single crystal, the rotation speed of the polycrystal, and the equivalent of the lower melting zone, based on experience or previous crystal pulling data by the craftsman Height setting value.
具体的,所述直径测量设备还用于测定多晶原料棒的直径;Specifically, the diameter measuring device is further configured to determine a diameter of the polycrystalline material rod;
所述可编程逻辑控制器,还用于控制所述多晶下降伺服电机,且在自动扩肩生长阶段,所述多晶下降速度已配置的函数关系具体为:
Figure PCTCN2015092868-appb-000007
其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径,ρl为晶体的液态密度,ρs为晶体的固态密度,hlqd为下熔区等效高度,θ为单晶所处的生长区间已配置的生长角度,即多晶下降速度与单晶下降速度及已配置的生长角度之间是紧密配合的。多晶下降速度是与晶体生长形状密切相关的控制参数,通过控制多晶下降速度,可以实现晶体生长形状的精确控制。
The programmable logic controller is further configured to control the polycrystalline falling servo motor, and in the automatic shoulder growth stage, the function relationship of the polycrystalline falling speed has been configured as follows:
Figure PCTCN2015092868-appb-000007
Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystal, d is the diameter of the single crystal, ρ l is the liquid density of the crystal, ρ s is the solid density of the crystal, h Lqd is the equivalent height of the lower melting zone, and θ is the growth angle of the growth interval in which the single crystal is placed, that is, the polycrystalline falling speed is closely matched with the single crystal falling speed and the configured growth angle. The polycrystalline falling speed is a control parameter closely related to the crystal growth shape. By controlling the polycrystalline falling speed, precise control of the crystal growth shape can be achieved.
进一步的,区熔法制备晶体的系统还包括其他涉及运动的伺服电机及电机,如单晶下降伺服电机及单晶下降电机,单晶旋转伺服电机及单晶旋转电机,多晶旋转伺服电机及多晶旋转电机等,某一运动的伺服电机通过控制对应运动的电机从而控制对应运动的速度,如单晶旋转伺服电机用于通过控制单晶旋转电机从而控制单晶旋转速度。Further, the system for preparing crystals by zone melting method includes other servo motors and motors involved in motion, such as single crystal falling servo motors and single crystal falling motors, single crystal rotating servo motors and single crystal rotating motors, polycrystalline rotating servo motors and In a polycrystalline rotating machine or the like, a moving servo motor controls the speed of the corresponding motion by controlling a motor corresponding to the motion, such as a single crystal rotating servo motor for controlling the single crystal rotating speed by controlling the single crystal rotating motor.
具体的,所述可编程逻辑控制器,还用于控制所述伺服电机且在自动等径生长阶段,多晶下降速度按照已配置的函数关系调整,所述多晶下降速度已配置的函数关系具体为
Figure PCTCN2015092868-appb-000008
其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径。
Specifically, the programmable logic controller is further configured to control the servo motor and, in an automatic equal diameter growth phase, the polycrystalline falling speed is adjusted according to a configured function relationship, and the polycrystalline falling speed has a configured function relationship. Specifically
Figure PCTCN2015092868-appb-000008
Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystalline, and d is the diameter of the single crystal.
在自动扩肩生长阶段,所述加热功率已配置的函数关系P=f(d)是采用曲线拟合技术得到的,其中,P为加热功率,d为单晶的直径。加热功率,是与晶体实际生长形状密切相关的生长参数,需要精细化控制,而在采用曲线拟合技术得到的加热功率与单晶的直径的函数关系中,加热功率随单晶的直径连续变化,便于实现加热功率的精细化控制。In the automatic shoulder growth phase, the heating power configured function relationship P = f(d) is obtained by a curve fitting technique, where P is the heating power and d is the diameter of the single crystal. The heating power is a growth parameter closely related to the actual growth shape of the crystal, which requires fine control. In the relationship between the heating power obtained by the curve fitting technique and the diameter of the single crystal, the heating power continuously changes with the diameter of the single crystal. It is convenient to achieve fine control of heating power.
具体的,所述曲线拟合技术采用最小二乘拟合方法。 Specifically, the curve fitting technique adopts a least squares fitting method.
具体的,所述曲线拟合技术采用多项式作为拟合函数。Specifically, the curve fitting technique uses a polynomial as a fitting function.
进一步的,在本实施例中,通过曲线拟合得到的单晶的加热功率与单晶直径的函数关系为:P=f(d)=-2.871×10-8d4+1.273×10-5d3-2.089×10-3d2+0.4116d+29.76;其中,P为加热功率,d为单晶的直径。Further, in the present embodiment, the heating power of the single crystal obtained by curve fitting is a function of the diameter of the single crystal: P = f (d) = - 2.871 × 10 -8 d 4 + 1.273 × 10 -5 d 3 -2.089×10 -3 d 2 +0.4116d+29.76; wherein P is the heating power and d is the diameter of the single crystal.
显然,本领域的技术人员可以对本发明实施例进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。 It is apparent that those skilled in the art can make various modifications and variations to the embodiments of the invention without departing from the spirit and scope of the invention. Thus, it is intended that the present invention cover the modifications and modifications of the invention

Claims (14)

  1. 一种区熔晶体的自动生长方法,其特征在于,包括如下步骤:An automatic growth method for a zone melting crystal, comprising the steps of:
    人工引晶及扩肩,形成单晶;当单晶的直径大于已配置的多层圆台形生长区间的最下层圆台形生长区间下底面的直径后,切换至自动扩肩生长阶段;Manually seeding and expanding the shoulder to form a single crystal; when the diameter of the single crystal is larger than the diameter of the bottom surface of the lowermost truncated growth section of the configured multi-layer truncated cone growth section, switching to the automatic shoulder growth stage;
    在自动扩肩生长阶段,当单晶的直径大于某层圆台形生长区间的下底面直径且小于上底面直径时,单晶所处的生长区间即为该层圆台形生长区间;单晶在所处的已配置生长参数的生长区间生长;其中,生长参数至少包括多晶下降速度和加热功率,分别按照已配置的函数关系调整使单晶按照所处的生长区间已配置的生长角度生长;其中,生长角度指的是圆台母线与下底面之间的夹角;In the automatic shoulder growth stage, when the diameter of the single crystal is larger than the diameter of the lower bottom surface of a certain circular truncated growth section and smaller than the diameter of the upper bottom surface, the growth interval of the single crystal is the circular truncated growth interval of the layer; a growing interval growth of the configured growth parameter; wherein the growth parameter includes at least a polycrystalline falling speed and a heating power, respectively adjusted according to a configured functional relationship, so that the single crystal grows according to a growth angle in which the growth interval is configured; The growth angle refers to the angle between the round busbar and the lower bottom surface;
    当单晶的直径达到目标值时,切换至自动等径生长阶段,此时,单晶所处的生长区间是最上层的生长区间,单晶在该生长区间沿轴向生长。When the diameter of the single crystal reaches the target value, it is switched to the automatic equal diameter growth stage. At this time, the growth interval in which the single crystal is located is the growth interval of the uppermost layer, and the single crystal grows in the axial direction in the growth interval.
  2. 根据权利要求1所述的区熔晶体的自动生长方法,其特征在于,所述生长参数还包括单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度,其中,下熔区等效高度指的是与下熔区液体体积相等的圆柱形熔区的高度。The method according to claim 1, wherein the growth parameter further comprises a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein The equivalent height of the melt zone refers to the height of the cylindrical melt zone equal to the volume of the liquid in the lower melt zone.
  3. 根据权利要求2所述的区熔晶体的自动生长方法,其特征在于,在自动扩肩生长阶段,多晶下降速度已配置的函数关系具体为:
    Figure PCTCN2015092868-appb-100001
    其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径,ρl为晶体的液态密度,ρs为晶体的固态密度,hlqd为下熔区等效高度,θ为单晶所处的生长区间已配置的生长角度。
    The method for automatically growing a zone melting crystal according to claim 2, wherein in the automatic shoulder growth stage, the functional relationship of the polycrystalline falling speed has been configured as follows:
    Figure PCTCN2015092868-appb-100001
    Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystal, d is the diameter of the single crystal, ρ l is the liquid density of the crystal, ρ s is the solid density of the crystal, h Lqd is the equivalent height of the lower melting zone, and θ is the configured growth angle of the growth zone in which the single crystal is located.
  4. 根据权利要求1所述的区熔晶体的自动生长方法,其特征在于,在自动等径生长阶段,多晶下降速度按照已配置的函数关系调整,函数关系具体为:
    Figure PCTCN2015092868-appb-100002
    其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径。
    The method for automatically growing a zone melting crystal according to claim 1, wherein in the automatic equal diameter growth stage, the polycrystalline falling speed is adjusted according to a configured function relationship, and the functional relationship is specifically:
    Figure PCTCN2015092868-appb-100002
    Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystalline, and d is the diameter of the single crystal.
  5. 根据权利要求1所述的区熔晶体的自动生长方法,其特征在于,在自动扩肩生长阶段,加热功率已配置的函数关系P=f(d)是采用曲线拟合技术得到的,其中,P为加热功率,d为单晶的直径。The method for automatically growing a zone melting crystal according to claim 1, wherein in the automatic shoulder growth phase, the function relationship P*f(d) of the heating power is obtained by using a curve fitting technique, wherein P is the heating power and d is the diameter of the single crystal.
  6. 根据权利要求5所述的区熔晶体的自动生长方法,其特征在于,所述曲线拟合技术采用多项式作为拟合函数。The method of automatically growing a zone-melting crystal according to claim 5, wherein the curve fitting technique employs a polynomial as a fitting function.
  7. 根据权利要求5所述的区熔晶体的自动生长方法,其特征在于,所述曲线拟合技术采用最小二乘拟合方法。 The method of automatically growing a zone melting crystal according to claim 5, wherein the curve fitting technique employs a least squares fitting method.
  8. 一种区熔晶体的自动生长系统,其特征在于,包括:An automatic growth system for a zone melting crystal, comprising:
    直径测量设备,用于测定单晶的直径;a diameter measuring device for measuring the diameter of a single crystal;
    多晶下降伺服电机,用于控制多晶原料棒的下降速度;Polycrystalline drop servo motor for controlling the falling speed of the polycrystalline material rod;
    高频加热设备,用于对晶体进行加热;a high frequency heating device for heating the crystal;
    可编程逻辑控制器,用于存储已配置的多层圆台形生长区间和各生长区间已配置的生长角度,其中,生长角度指的是圆台母线与下底面之间的夹角;还用于存储已配置的多晶下降速度的函数关系,以及加热功率函数关系;a programmable logic controller for storing the configured multi-layer truncated cone growth interval and the configured growth angle of each growth interval, wherein the growth angle refers to an angle between the truncated bus bar and the lower bottom surface; and is also used for storage a function of the configured polycrystalline falling speed, and a heating power function relationship;
    所述可编程逻辑控制器还用于在单晶的直径大于已配置的最下层圆台形生长区间下底面的直径后,切换至自动扩肩生长阶段;还用于在自动扩肩生长阶段,当单晶的直径大于某层圆台形生长区间的下底面直径且小于上底面直径时,判断单晶所处的生长区间即为该层圆台形生长区间,并按该生长区间已配置的生长参数控制单晶生长,其中,至少控制多晶下降伺服电机使得多晶下降速度按照已配置的函数关系调整,同时控制高频加热设备使得加热功率按照已配置的函数关系调整;还用于在单晶的直径达到目标值时,切换至自动等径生长阶段,控制单晶沿轴向生长。The programmable logic controller is further configured to switch to an automatic shoulder growth stage after the diameter of the single crystal is larger than the diameter of the bottom surface of the configured lowermost truncated growth section; and is also used in the automatic shoulder growth stage. When the diameter of the single crystal is larger than the diameter of the lower surface of the growth section of a certain circular trough and smaller than the diameter of the upper surface, the growth interval of the single crystal is determined as the growth range of the truncated cone, and is controlled according to the growth parameters of the growth interval. Single crystal growth, wherein at least controlling the polycrystalline falling servo motor causes the polycrystalline falling speed to be adjusted according to a configured function relationship, while controlling the high frequency heating device such that the heating power is adjusted according to a configured function relationship; When the diameter reaches the target value, it switches to the automatic equal diameter growth stage to control the growth of the single crystal in the axial direction.
  9. 根据权利要求8所述的区熔晶体的自动生长系统,其特征在于,所述生长参数还包括单晶下降速度,单晶旋转速度,多晶旋转速度和下熔区等效高度,其中,下熔区等效高度指的是与下熔区液体体积相等的圆柱形熔区的高度。The automatic growth system for a zone melting crystal according to claim 8, wherein the growth parameter further comprises a single crystal falling speed, a single crystal rotating speed, a polycrystalline rotating speed, and a lower melting zone equivalent height, wherein The equivalent height of the melt zone refers to the height of the cylindrical melt zone equal to the volume of the liquid in the lower melt zone.
  10. 根据权利要求9所述的区熔晶体的自动生长系统,其特征在于,所述直径测量设备还用于测定多晶原料棒的直径;The automatic growth system for a zone melting crystal according to claim 9, wherein said diameter measuring device is further for measuring a diameter of a polycrystalline raw material rod;
    所述可编程逻辑控制器,还用于控制所述多晶下降伺服电机,且在自动扩肩生长阶段,所述多晶下降速度已配置的函数关系具体为:
    Figure PCTCN2015092868-appb-100003
    其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径,d为单晶的直径,ρl为晶体的液态密度,ρs为晶体的固态密度,hlqd为下熔区等效高度,θ为单晶所处的生长区间已配置的生长角度。
    The programmable logic controller is further configured to control the polycrystalline falling servo motor, and in the automatic shoulder growth stage, the function relationship of the polycrystalline falling speed has been configured as follows:
    Figure PCTCN2015092868-appb-100003
    Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystal, d is the diameter of the single crystal, ρ l is the liquid density of the crystal, ρ s is the solid density of the crystal, h Lqd is the equivalent height of the lower melting zone, and θ is the configured growth angle of the growth zone in which the single crystal is located.
  11. 根据权利要求8所述的区熔晶体的自动生长系统,其特征在于,所述直径测量设备还用于测定多晶原料棒的直径;The automatic growth system for a zone melting crystal according to claim 8, wherein said diameter measuring device is further for measuring a diameter of a polycrystalline material rod;
    所述可编程逻辑控制器,还用于控制所述伺服电机且在自动等径生长阶段,多晶下降速度按照已配置的函数关系调整,所述多晶下降速度已配置的函数关系具体为
    Figure PCTCN2015092868-appb-100004
    其中,Vpoly为多晶下降速度,Vmono为单晶下降速度,D为多晶的实测直径, d为单晶的直径。
    The programmable logic controller is further configured to control the servo motor and, in an automatic equal diameter growth phase, the polycrystalline falling speed is adjusted according to a configured function relationship, and the function relationship of the polycrystalline falling speed configured is specifically
    Figure PCTCN2015092868-appb-100004
    Where V poly is the polycrystalline falling speed, V mono is the single crystal falling speed, D is the measured diameter of the polycrystalline, and d is the diameter of the single crystal.
  12. 根据权利要求8所述的区熔晶体的自动生长系统,其特征在于,在自动扩肩生长阶段,加热功率已配置的函数关系P=f(d)是采用曲线拟合技术得到的,其中,P为加热功率,d为单晶的直径。The automatic growth system for a zone melting crystal according to claim 8, wherein in the automatic shoulder growth phase, the functional relationship P=f(d) of the heating power is obtained by a curve fitting technique, wherein P is the heating power and d is the diameter of the single crystal.
  13. 根据权利要求12所述的区熔晶体的自动生长系统,其特征在于,所述曲线拟合技术,采用多项式作为拟合函数。The automatic growth system for a zone melting crystal according to claim 12, wherein said curve fitting technique employs a polynomial as a fitting function.
  14. 根据权利要求12所述的区熔晶体的自动生长系统,其特征在于,所述曲线拟合技术,采用最小二乘拟合方法。 The automatic growth system for a zone melting crystal according to claim 12, wherein said curve fitting technique employs a least squares fitting method.
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