CN114164489B - Method for manufacturing silicon single crystal rod - Google Patents
Method for manufacturing silicon single crystal rod Download PDFInfo
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- CN114164489B CN114164489B CN202010949545.2A CN202010949545A CN114164489B CN 114164489 B CN114164489 B CN 114164489B CN 202010949545 A CN202010949545 A CN 202010949545A CN 114164489 B CN114164489 B CN 114164489B
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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
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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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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Abstract
The embodiment of the invention provides a method for manufacturing a silicon single crystal rod, which comprises the following steps: heating and melting the mixed silicon material in the crucible to obtain mixed silicon liquid, wherein the mixed silicon material comprises a doping agent and a polycrystalline silicon material, and the mixed silicon liquid is used for drawing N monocrystalline silicon rods; when the Nth single crystal silicon rod is pulled, calculating the difference between the weight of the mixed silicon liquid and the weight of the crucible bottom materials under the condition that the difference is larger than a preset value; performing first crystal pulling operation in the mixed silicon liquid according to the first crystal pulling parameters to obtain a first section of single crystal silicon rod with a preset length; and performing a second crystal pulling operation according to the second crystal pulling parameters, and continuously connecting a second section of the monocrystalline silicon rod on the first section of the monocrystalline silicon rod to obtain a first monocrystalline silicon rod with the target length. According to the segregation effect of the dopant, when the Nth monocrystalline silicon rod is pulled, the crystal pulling operation is divided into two sections, and reasonable crystal pulling parameters are correspondingly set in each crystal pulling operation, so that the first section of monocrystalline silicon rod and the second section of monocrystalline silicon rod obtained by crystal pulling can be utilized.
Description
Technical Field
The invention relates to the technical field of photovoltaics, in particular to a method for manufacturing a silicon single crystal rod.
Background
With the development of photovoltaic technology and the requirement of 'zero carbon' production, photovoltaic power generation is widely applied. Because the monocrystalline silicon is an important raw material for manufacturing the solar cell, the demand is more and more large, and correspondingly, higher and higher requirements are put forward on the quality and the manufacturing cost of the monocrystalline silicon.
Because the monocrystalline silicon added with the dopant has the advantages of high conversion efficiency, long service life, good severe environment resistance and the like, the preparation and the use of the monocrystalline silicon are widely concerned. However, since the segregation coefficient of some dopants in silicon is low, it is difficult to control the doping concentration during doping, resulting in a distribution of resistivity of the obtained single crystal silicon rod between 0.1 and 5 Ω · cm, which is too large, and an acceptable portion satisfying a resistivity between 0.8 and 3 Ω · cm is usually less than 50%. In a specific application, only the part with qualified resistivity can be utilized for a single silicon single crystal rod, and the part with unqualified resistivity is usually used as waste material, so that the availability of the whole silicon single crystal rod is low and the cost is high.
Disclosure of Invention
In view of this, in order to solve the problems of low availability and high cost of the whole single crystal silicon rod in the prior art, embodiments of the present invention provide a method for manufacturing a single crystal silicon rod.
In order to solve the above problem, an embodiment of the present invention discloses a method for manufacturing a silicon single crystal rod, including: heating and melting a mixed silicon material in a crucible to obtain a mixed silicon liquid, wherein the mixed silicon material comprises a gallium dopant and a primary polycrystalline silicon material which are prepared according to a preset proportion;
performing a first crystal pulling operation in the mixed silicon liquid according to a first crystal pulling parameter to obtain a first section of monocrystalline silicon rod with a preset length, wherein the first crystal pulling parameter comprises a first crucible rotation, a first furnace pressure, a first argon flow and a first pulling speed;
and executing second crystal pulling operation according to second crystal pulling parameters, and continuously connecting a second section of single crystal silicon rod on the first section of single crystal silicon rod to obtain a first single crystal silicon rod with the target length, wherein second preset parameters comprise a second crucible rotation, a second furnace pressure, a second argon flow and a second pulling speed, the second crucible rotation is 80% -90% of the first crucible rotation, the second furnace pressure is 80% -90% of the first furnace pressure, the second argon flow is 115% -130% of the first argon flow, and the second pulling speed is 80% -90% of the first pulling speed.
Further, the first crystal pulling parameters comprise a first crucible rotation, a first furnace pressure, a first argon flow and a first pulling speed;
the second preset parameter comprises a second crucible rotation, a second furnace pressure, a second argon flow and a second pulling speed, the second crucible rotation is 80% -90% of the first crucible rotation, the second furnace pressure is 80% -90% of the first furnace pressure, the second argon flow is 115% -130% of the first argon flow, and the second pulling speed is 80% -90% of the first pulling speed.
Further, the step of performing a first crystal pulling operation in the mixed silicon liquid according to the first crystal pulling parameter to obtain a first section of monocrystalline silicon rod with a preset length comprises the following steps:
in the mixed silicon liquid, sequentially performing temperature adjustment, seeding, shouldering and diameter equalization operations according to a first preset parameter to obtain a monocrystalline silicon rod with a transition length;
and adjusting the first crystal pulling parameter to a second crystal pulling parameter while performing the isodiametric operation on the monocrystalline silicon rod with the transition length to obtain a first section of monocrystalline silicon rod with a preset length.
Further, the step of performing a second crystal pulling operation according to the second crystal pulling parameters to continue a second segment of the single crystal silicon rod on the first segment of the single crystal silicon rod to obtain a target length of the first single crystal silicon rod comprises:
and sequentially performing temperature adjustment, seeding, shouldering and diameter equalization according to a second crystal pulling parameter, and continuously connecting a second section of single crystal silicon rod on the first single crystal silicon rod to obtain the first single crystal silicon rod with the target length.
Further, the resistivity of the first section of the single crystal silicon rod is a first resistivity, the resistivity of the second section of the single crystal silicon rod is a second resistivity, and the second resistivity is smaller than the first resistivity.
Further, the first resistivity is between 0.8 and 3 Ω -cm, and the second resistivity is between 0.1 and 2 Ω -cm.
Further, in the case that the difference value is smaller than or equal to the preset value, crystal pulling operation is carried out in the mixed silicon liquid according to a third crystal pulling parameter so as to obtain a second monocrystalline silicon rod.
Further, the resistivity of the second single crystal silicon rod is between 0.1 and 2 Ω · cm.
Further, the ratio of the preset length to the target length is (0.35-0.45): 1.
Further, the preset length is the sum of the switching length and the length of a transition section, and the length of the transition section is between 100 and 200 mm;
the switching length is equal to (m) 1 -m 2 -(l 2 +l 3 )/a 2 )*a 1 -l 1 Wherein m is 1 Represents the weight of the mixed silicon liquid, m 2 Denotes the weight of the crucible bottom material,/ 1 Denotes the transition region length, l 2 Representing a desired length of a second segment of the single crystal silicon rod, the secondThe required length of the section of the single crystal silicon rod is the usable effective length l of the second section of the single crystal silicon rod 3 Representing a safety length, the safety length being a preset percentage of the target length, the preset percentage being between 8% and 10%, a 1 Representing the conversion coefficient of a first section of single crystal silicon rod, wherein the conversion coefficient of a second section of single crystal silicon rod is the length of the second section of single crystal silicon rod with the diameter corresponding to the required diameter of 1kg of mixed silicon material, a 2 And the conversion coefficient of the second section of the single crystal silicon rod is expressed, and the conversion coefficient of the first section of the single crystal silicon rod is the length of the first section of the single crystal silicon rod with the diameter required by the 1kg of mixed silicon material.
Further, the dopant is gallium dopant, and the gallium dopant and the polysilicon material are configured according to a preset ratio.
The embodiment of the invention has the following advantages:
the embodiment of the invention provides a method for manufacturing silicon single crystal rods, wherein mixed silicon liquid is used for drawing N silicon single crystal rods, and according to the segregation effect of a doping agent, the quality of the N-1 silicon single crystal rods obtained by drawing is better, so that the silicon single crystal rods can be used for manufacturing solar cells. Since the product drawn by the nth single crystal silicon rod depends on the difference between the weight of the mixed silicon solution in the crucible and the weight of the crucible bed charge, in this embodiment, when the nth single crystal silicon rod is drawn, a first pulling operation is performed in the mixed silicon solution according to a first pulling parameter to obtain a first section of single crystal silicon rod with a preset length, and the first section of single crystal silicon rod can be used for manufacturing solar cell slices. And performing a second crystal pulling operation according to the second crystal pulling parameters, and continuously connecting a second section of the monocrystalline silicon rod on the first section of the monocrystalline silicon rod to obtain a first monocrystalline silicon rod with a target length, wherein the second section of the monocrystalline silicon rod can be used for manufacturing monocrystalline silicon cores or polycrystalline silicon. That is to say, according to the segregation effect of the dopant, the N single crystal silicon rods obtained by pulling can be utilized by switching the crystal pulling parameters, so that the waste of materials is avoided, the production cost is reduced, and the availability ratio of the whole single crystal silicon rod is improved.
Drawings
FIG. 1 is a flow chart illustrating the steps of an embodiment of a method for producing a single crystal silicon rod in accordance with the present invention;
FIG. 2 is a flow chart illustrating the steps of another embodiment of a method of forming a single crystal silicon rod in accordance with the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description thereof.
Example one
Referring to fig. 1, a flow chart of steps of an embodiment of a method for manufacturing a single crystal silicon rod according to the present invention is shown, and specifically, the method may include the following steps:
step 101: heating and melting a mixed silicon material in a crucible to obtain a mixed silicon liquid, wherein the mixed silicon material comprises a doping agent and a polycrystalline silicon material, the mixed silicon liquid is used for drawing N monocrystalline silicon rods, and N is an integer greater than or equal to 1.
Specifically, the mixed silicon liquid includes a dopant and a polysilicon material, and according to the requirements of the solar cell on the conversion efficiency, the service life, the harsh environment resistance and other performances, the dopant commonly used in the polysilicon material is a boron dopant or a gallium dopant, and the dopant is not limited thereto and can be selected according to the actual requirements.
Specifically, the native polysilicon material may be pure dense native polysilicon without adding any dopant, or may be redrawn polysilicon, and the specific type of the polysilicon material in the embodiment of the present invention may not be limited. Of course, in order to reduce the impurity content in the mixed silicon liquid obtained by melting silicon and the dopant, the embodiment is preferably applied to the raw polysilicon material, for example, when the crucible is charged, only the dense raw polysilicon material, the poor material such as other loose material and the dopant are allowed to be charged, but the dopant is not allowed to be charged.
Specifically, the crucible may be a quartz crucible, a graphite crucible, or the like, and the specific type of the crucible in the embodiment of the present invention may not be limited. In actual production, N single crystal silicon rods can be drawn from mixed silicon liquid obtained by heating and melting mixed silicon materials put in a crucible once, N is an integer greater than or equal to 1, the specific numerical value of N in the embodiment of the invention is not limited, and N can be set according to the size of the crucible.
In the embodiment of the present invention, the step of heating and melting the mixed silicon material in the crucible to obtain the mixed silicon liquid further includes:
adding the mixed silicon material into a crucible in a single crystal furnace; and vacuumizing a furnace chamber of the single crystal furnace, and filling argon into a hearth of the single crystal furnace. The two-step process operation is a conventional process operation in the field, and the description of the embodiment is omitted.
Step 102: and when the Nth single crystal silicon rod is pulled, calculating the difference value between the weight of the mixed silicon liquid and the weight of the crucible bed charge, wherein the crucible bed charge is the reserved silicon liquid in the crucible.
In actual production, in order to improve production efficiency, ending treatment is carried out after N single crystal silicon rods are cyclically pulled in one single crystal furnace, so that some silicon liquid can be left in a crucible after the N single crystal silicon rods are pulled, and the crucible can be prevented from being damaged by high temperature. In this embodiment, the reserved silicon liquid is a mixed silicon liquid.
In practical production, since the segregation coefficient of some dopants is very low, for example, the segregation coefficient of gallium dopant is 0.008, it is difficult to control the doping concentration during the whole drawing process during doping, and it is also difficult to accurately control the resistivity of the crystal, especially the nth (last) silicon single crystal rod after the end drawing, so that it is difficult to ensure the consistency of the head and tail resistivity of the nth silicon single crystal rod, thereby affecting the availability of the nth whole silicon single crystal rod. In actual production, the product drawn by the nth single crystal silicon rod depends on the weight of the mixed silicon liquid in the crucible when the nth single crystal silicon rod is drawn, the weight of the mixed silicon liquid in the crucible is the difference between the weight of the mixed silicon liquid and the weight of the crucible bottom material, and it should be noted that the mixed silicon liquid in this embodiment refers to the current mixed silicon liquid in the crucible.
In the mixed silicon liquid, a first single crystal silicon rod may be pulled according to preset pulling parameters, and the first single crystal silicon rod may be pulled cyclically according to the pulling method of the first single crystal silicon rod until reaching the nth-1 single crystal silicon rod, where the pulling parameters may include a crucible rotation, a furnace pressure, an argon gas flow, a pulling speed, and the like, and preferably, according to a segregation effect of a dopant (e.g., a gallium dopant) in silicon, in order to ensure that the first N-1 single crystal silicon rods have good quality and qualified resistivity, in this embodiment, the crucible rotation may be set to 10r/min, the furnace pressure may be set to 15torr, the argon gas flow may be set to 100slpm, and the pulling speed may be set to 100mm/h, and specific values of the pulling parameters may not be limited in the embodiments of the present invention. The qualified resistivity means the resistivity which can meet the requirement of manufacturing the solar cell, and the qualified resistivity is between 0.8 and 3 omega cm.
Step 103: and under the condition that the difference is larger than a preset value, performing first crystal pulling operation in the mixed silicon liquid according to a first crystal pulling parameter to obtain a first section of monocrystalline silicon rod with a preset length.
In the embodiment of the present invention, the required weight of the last single crystal silicon rod obtained by pulling may be M for manufacturing a single crystal silicon core product, and as the nth single crystal silicon rod is pulled, the single crystal silicon rod at the ending portion generally cannot be used, in this embodiment, in order to enable the nth single crystal silicon rod obtained by pulling to at least meet the required weight M for manufacturing a single crystal silicon core product, a wide value is added on the basis of M in this embodiment, that is, the preset value in the embodiment of the present invention may be M (1 + 10%), and the specific value of the preset value in this embodiment may not be limited.
In actual production, in order to make the nth single crystal silicon rod available due to segregation effect of the dopant in silicon, the embodiment sets a specific drawing step of the nth single crystal silicon rod according to the comparison between the difference value and the preset value. For example, in the case that the difference is larger than the preset value, a part of the nth monocrystalline silicon rod can be used for manufacturing a solar cell, another part of the nth monocrystalline silicon rod can be used for manufacturing a monocrystalline silicon core or used as a conductor for manufacturing polycrystalline silicon in the deposition center of the reduction furnace, and in the case that the difference is smaller than the preset value, the whole nth monocrystalline silicon rod can be used for manufacturing a monocrystalline silicon core or used as a conductor for manufacturing polycrystalline silicon in the deposition center of the reduction furnace.
In the embodiment of the invention, for the pulling of the Nth monocrystalline silicon rod, under the condition that the difference value is larger than the preset value, the first time of crystal pulling operation is carried out in the mixed silicon liquid according to the first crystal pulling parameter so as to obtain the first section of monocrystalline silicon rod with the preset length. The first pulling parameter may be continuously the pulling parameter of the previous N-1 stage, or may be a resistivity (first resistivity) actually required for the first stage of the single crystal silicon rod product, for example, the first resistivity is distributed between 0.8 and 3 Ω -cm, and the specific value of the first pulling parameter is not limited in the embodiment of the invention.
Step 104: and performing a second crystal pulling operation according to the second crystal pulling parameters, and continuing to connect a second section of the monocrystalline silicon rod on the first section of the monocrystalline silicon rod to obtain a first monocrystalline silicon rod with the target length.
In the embodiment of the invention, first, the first pulling parameter should be adjusted to the second pulling parameter; and then, carrying out a second crystal pulling operation according to the second crystal pulling parameters to obtain a second section of the monocrystalline silicon rod. Specifically, the second section of the single crystal silicon rod is continuously pulled on the first section of the single crystal silicon rod, and the second section of the single crystal silicon rod is continuously pulled on the first section of the single crystal silicon rod to obtain the first single crystal silicon rod with the target length. It should be noted that, in order to ensure that the quality of each part of the single crystal silicon rod during the pulling process meets the actual requirements, the adjustment of the first crystal pulling parameter to the second crystal pulling parameter is performed step by step, that is, the first crystal pulling parameter is adjusted to the second crystal pulling parameter a plurality of times.
In actual production, because the segregation of the dopant can be inhibited by low crucible rotation, low furnace pressure, large argon flow and low pulling speed, the content of the dopant in the second section of the monocrystalline silicon rod is reduced, wherein the low crucible rotation and the low furnace pressure have a forward effect on the reduction of the oxygen content, and the large argon flow and the low pulling speed have a forward effect on the improvement of the carbon content, so that the quality of the second section of the monocrystalline silicon rod pulled according to the second crystal pulling parameter can meet the quality of the actually required monocrystalline silicon core. Therefore, in the second crystal pulling parameter of the embodiment of the present invention, the pot rotation, the furnace pressure and the pulling rate in the first crystal pulling parameter are adjusted to be lower and the argon flow is adjusted to be higher than the first crystal pulling parameter.
Specifically, the first section of single crystal silicon rod is pulled completely, and ending operation can be omitted, so as to reduce waste of invalid working hours, that is, the first section of single crystal silicon rod is pulled completely, and a second section of single crystal silicon rod is pulled continuously, and the furnace is stopped after ending the pulling of the second section of single crystal silicon rod.
In an embodiment of the present invention, the crucible may be heated by a first heater and a second heater to melt the polysilicon material and the dopant in the crucible to obtain the mixed silicon liquid, specifically, the first heater may be correspondingly disposed on a sidewall of the crucible, and a heating power of the first heater is 40-110kw, the second heater may be correspondingly disposed on a bottom of the crucible, and a heating power of the second heater is 40-110kw. In actual production, under the condition that the heating power of the first heater is 40-110kw and the heating power of the second heater is 40-110kw, the melting speed of the mixed silicon material in the crucible is higher, the manufacturing efficiency of the single crystal silicon rod is improved, and the damage to the crucible wall in the melting process can be reduced.
In summary, the method for manufacturing a single crystal silicon rod according to the embodiment of the present invention at least includes the following advantages:
the embodiment of the invention provides a method for manufacturing silicon single crystal rods, wherein mixed silicon liquid is used for drawing N silicon single crystal rods, and according to the segregation effect of a doping agent, the quality of the N-1 silicon single crystal rods obtained by drawing is better, so that the silicon single crystal rods can be used for manufacturing solar cells. Since the product drawn by the nth single crystal silicon rod depends on the difference between the weight of the mixed silicon solution in the crucible and the weight of the crucible bed charge, in this embodiment, when the nth single crystal silicon rod is drawn, a first pulling operation is performed in the mixed silicon solution according to a first pulling parameter to obtain a first section of single crystal silicon rod with a preset length, and the first section of single crystal silicon rod can be used for manufacturing solar cell slices. And performing a second crystal pulling operation according to the second crystal pulling parameters, and continuously connecting a second section of monocrystalline silicon rod on the first section of monocrystalline silicon rod to obtain a first monocrystalline silicon rod with the target length, wherein the second section of monocrystalline silicon rod can be used for manufacturing monocrystalline silicon cores or polycrystalline silicon. That is to say, according to the segregation effect of the dopant, the N single crystal silicon rods obtained by pulling can be utilized by switching the crystal pulling parameters in this embodiment, so that the waste of materials is avoided, the production cost is reduced, and the availability of the whole single crystal silicon rod is improved.
Example two
Referring to fig. 2, a flow chart of steps of another embodiment of a method for manufacturing a single crystal silicon rod according to the present invention is shown, and specifically, the method may include the following steps:
step 201: heating and melting a mixed silicon material in a crucible to obtain a mixed silicon liquid, wherein the mixed silicon material comprises a doping agent and a polycrystalline silicon material, the mixed silicon liquid is used for drawing N monocrystalline silicon rods, and N is an integer greater than or equal to 1.
Specifically, the mixed silicon liquid includes a dopant and a polysilicon material, and according to performance requirements of the solar cell on conversion efficiency, service life, resistance to a severe environment and the like, the dopant commonly used in the polysilicon material is a boron dopant or a gallium dopant, the dopant is not limited thereto, and other dopants can be selected according to actual requirements.
In practical application, after a monocrystalline silicon rod drawn from a gallium-doped polycrystalline silicon material is manufactured into a solar cell, no light-induced attenuation is generated in subsequent use, and the conversion efficiency is high, the service life is long, and the adverse environment resistance is good, so that the gallium dopant is preferably selected as the dopant in the embodiment, the gallium dopant can be a pure gallium dopant, the purity of the pure gallium dopant can be determined according to the resistivity actually required by the monocrystalline silicon rod, and the purity of the pure dopant is not specifically limited in the embodiment.
In the embodiment of the present invention, the gallium dopant and the polysilicon material may be configured from the mixed silicon material according to a preset ratio, the preset ratio of the gallium dopant and the polysilicon material may be set according to the weight and the resistivity of the single crystal silicon rod to be pulled, and the preset ratio of the gallium dopant and the polysilicon material may not be specifically limited in this embodiment.
Step 202: and when the Nth single crystal silicon rod is pulled, calculating the difference value between the weight of the mixed silicon liquid and the weight of the crucible bed charge, wherein the crucible bed charge is the reserved silicon liquid in the crucible.
Specifically, the specific implementation process of this step may be implemented by referring to step 102 in the first embodiment, which is not described herein again.
Step 203: and under the condition that the difference is larger than a preset value, performing first crystal pulling operation in the mixed silicon liquid according to a first crystal pulling parameter to obtain a first section of monocrystalline silicon rod with a preset length.
In the embodiment of the invention, the first crystal pulling parameter comprises a first crucible rotation, a first furnace pressure, a first argon flow and a first pulling speed, and the embodiment can set the first crucible rotation to be 10r/min, the first furnace pressure to be 15torr, the first argon flow to be 100slpm and the first pulling speed to be 100mm/h. In this embodiment, the resistivity (first resistivity) of the first section of single crystal silicon rod being pulled can be distributed between 0.8 and 3 Ω -cm, depending on the segregation effect of gallium and the first pulling parameter during the actual pulling operation. In practical application, the first section of the monocrystalline silicon rod can be cut to form a square monocrystalline silicon piece, and then a monocrystalline cell piece and a monocrystalline component can be prepared for photovoltaic power generation.
In this embodiment of the present invention, the step 203 may include:
step 2031: under the condition that the difference is larger than a preset value, sequentially performing temperature adjustment, seeding, shouldering and diameter equalization operations in the mixed silicon liquid according to a first crystal pulling parameter to obtain a single crystal silicon rod with a switched length;
in actual production, temperature regulation, seeding, shouldering and isometric operations can be performed in the mixed silicon liquid to obtain the first section of the single crystal silicon rod. Specifically, the operation of temperature adjustment may be: after the mixed silicon material in the crucible is melted, the mixed silicon material is stabilized to a proper seeding temperature so that the seed crystal is fused with the melt. The seeding operation may be: and (3) extending the seed crystal into the silicon liquid, and leading out a thin neck with a certain length and a diameter of 3-5 mm to eliminate crystal dislocation. The shouldering operation can be as follows: and (3) enlarging the diameter of the thin neck to a target diameter, and when the thin neck grows to a sufficient length and reaches the first pulling rate of 100mm/h, reducing the pulling speed for shouldering. The operation of the equal diameter can be specifically as follows: when the crystal basically realizes the equal diameter growth and reaches the target diameter, the first section of the single crystal silicon rod can be formed by drawing.
Step 2032: and adjusting the first crystal pulling parameter to a second crystal pulling parameter while performing the constant diameter operation on the single crystal silicon rod with the switched length to obtain a first section of single crystal silicon rod with a preset length.
In actual production, a first crystal pulling operation is carried out by using a first crystal pulling parameter, when the crystal is pulled to a switching length, the adjustment of a second crystal pulling parameter is completed in the process of the constant diameter operation just till the constant diameter operation, and the time for adjusting the first crystal pulling parameter to the second crystal pulling parameter is considered to be just matched with the time for the constant diameter operation of a first section of monocrystalline silicon rod, and the monocrystalline silicon rod with the length of a transition zone is pulled in the time for adjusting the second crystal pulling parameter, wherein the length of the transition zone = preset length-switching length, and the time for adjusting the second crystal pulling parameter is adjusted according to the actual process. As can be seen from the above, in the embodiment, the second crystal pulling parameter is switched during the isodiametric process of the first section of the single crystal silicon rod, so that not only can enough time be ensured for switching the first crystal pulling parameter to the second crystal pulling parameter, but also the quality of each part of the first section of the single crystal silicon rod can be ensured to meet the actual requirement.
Step 204: and performing a second crystal pulling operation according to the second crystal pulling parameters, and continuing to connect a second section of the monocrystalline silicon rod on the first section of the monocrystalline silicon rod to obtain a first monocrystalline silicon rod with the target length.
In an embodiment of the invention, the second crystal pulling parameter comprises a second crucible rotation, a second furnace pressure, a second argon flow and a second pulling speed, the second crucible rotation is 80% -90% of the first crucible rotation, the second furnace pressure is 80% -90% of the first furnace pressure, the second argon flow is 115% -130% of the first argon flow, and the second pulling speed is 80% -90% of the first pulling speed.
Specifically, in the embodiment, the first crucible rotation can be reduced by 10% -20%, the first furnace pressure can be reduced by 10% -20%, the first argon flow can be increased by 15% -30%, the first pulling speed can be reduced by 10% -20% to obtain the second pulling parameter, so that the second crucible rotation can be 8-9r/min, the second furnace pressure can be 13.5-2torr, the second argon flow can be 115-130slpm, and the second pulling speed can be 90-80mm/h. The resistivity (second resistivity) of the second section of the single crystal silicon rod obtained by drawing according to the crystal pulling parameters can be distributed in a range of 0.1-2 omega cm, the resistivity distribution is concentrated, and the content of gallium in the second section of the single crystal silicon rod is low, so that the second section of the single crystal silicon rod has good quality and low resistance.
In actual production, the second resistivity is lower than the first resistivity, the second section of the monocrystalline silicon rod can be used for preparing a low-resistance monocrystalline silicon core and can also be used as a conductor for preparing polycrystalline silicon in a deposition center of a reduction furnace, and the second section of the monocrystalline silicon rod has the characteristic of easy breakdown, so that the phenomenon that the second section of the monocrystalline silicon rod bends or breaks in the reduction furnace can be reduced, and the energy consumption of production can be reduced due to the low resistivity of the second section of the monocrystalline silicon rod. Compared with the prior art, the implementation changes the waste material part with unqualified resistivity in the gallium-doped single crystal silicon rod drawn by the prior art into the low-resistance single crystal silicon rod with better quality, so that the implementation can ensure that the availability of a single gallium-doped single crystal silicon rod obtained by drawing is high by switching the process parameters when the last single crystal silicon rod is drawn according to the segregation effect of gallium, thereby reducing the production cost.
In the embodiment of the invention, due to the segregation effect of the gallium dopant and the requirements on the quality of the first section of the monocrystalline silicon rod and the second section of the monocrystalline silicon rod, in order to ensure that the resistivity of the first section of the monocrystalline silicon rod prepared by two crystal pulling operations is within the range of the actually required resistivity of 0.8-3 omega-cm and the resistivity of the second section of the monocrystalline silicon rod is within the range of the actually required resistivity of 0.1-2 omega-cm, the first crystal pulling parameter and the second crystal pulling parameter are reasonably set, so that the setting of the second crystal pulling parameter is very important for ensuring whether the quality and the resistivity of the two sections of the monocrystalline silicon rods meet the actual requirements. Therefore, in the actual crystal pulling operation, the switching time of the crystal pulling parameters needs to be determined, the switching time is the time for pulling the first single crystal silicon rod to the switching length, the first crystal pulling operation is pulled from the switching length to the preset length in the process of switching the first crystal pulling parameter to the second crystal pulling parameter, it can be seen that the time for adjusting the second crystal pulling parameter corresponds to the length of the transition zone, in the actual crystal pulling operation, the length of the transition zone = the preset length-the switching length, the length of the transition zone is between 100mm and 200mm, the length of the transition zone can be determined according to the time for switching the first crystal pulling parameter to the second crystal pulling parameter in the actual operation, and the specific length of the transition zone can not be limited in the embodiment.
Specifically, the preset length is the sum of the switching length and the transition interval length, and the switching length may be l 0 Is represented by 0 The calculation can be made with reference to the following formula:
l 0 ＝(m 1 -m 2 -(l 2 +l 3 )/a 2 )*a 1 -l 1
wherein m is 1 Represents the weight of the mixed silicon solution, m 2 Indicating the weight of the crucible bottom material, l 1 Denotes the transition section length,/ 2 The required length of the second section of the single crystal silicon rod is shown, the required length of the second section of the single crystal silicon rod is the usable effective length of the second section of the single crystal silicon rod, l 3 Representing a safety length which is a preset percentage of the target length, the preset percentage being between 8 and 10 percent, a 1 The conversion coefficient of the first section of the single crystal silicon rod is shown, the conversion coefficient of the second section of the single crystal silicon rod is the length of the second section of the single crystal silicon rod with the diameter corresponding to the required diameter of 1kg of mixed silicon material, a 2 The conversion coefficient of the second section of the single crystal silicon rod is shown, and the conversion coefficient of the first section of the single crystal silicon rod is the length of the first section of the single crystal silicon rod with the diameter corresponding to the required diameter of 1kg of mixed silicon material.
For example, the weight of the mixed silicon solution in the crucible is 450kg, the weight of the crucible bed charge is 20kg, the transformation coefficient of the first stage single crystal silicon rod with the required diameter of 215mm is 11.8mm/kg, the required length of the second stage single crystal silicon rod is 3000mm, the transformation coefficient of the second stage single crystal silicon rod with the required diameter of 215mm is 11.2mm/1kg, the safety length is 50mm, and the transition section length is 100mm.
According to the formula, the following formula can be obtained: l 0 = (450-20- (3000 + 50)/11.2)) × 11.8-100 ≈ 1760mm, and it can be seen that when the crystal is pulled according to the first crystal pulling parameter, if the length of the pulled crystal is 1760, the first crystal pulling parameter is adjusted. If the length of the transition interval is 100mm, the preset length =1760+100=1860, the target length = preset length + the required length of the second section of single crystal silicon rod + the safety length =1860+3000+50=4910, and the preset length is presetLength: target length =1860:4910= 0.38.
However, in order to set the time for adjusting the second pulling parameter more adequately during the actual pulling operation, the switching length may be set shorter, for example, the switching length may be 1700mm, since the transition interval length is determined according to the time required for the actual adjustment of the second pulling parameter, so that the present embodiment sets the ratio of the preset length to the target length within the range of (0.35-0.45): 1, i.e., the preset length is 35% -45% of the target length.
In the above formula of the switching length, since the switching length is not easily measured during actual pulling, the length generally needs to be calculated by converting the length into a weight by a predetermined conversion factor, in other words, the switching length corresponds to the weight of the mixed silicon liquid actually used for pulling the single crystal silicon rod of which the switching length is required, and the weight of the mixed silicon liquid actually used is the difference between the weight of the mixed silicon liquid currently used and the required weight of the second single crystal silicon rod product.
Step 205: and under the condition that the difference is smaller than or equal to the preset value, performing crystal pulling operation in the mixed silicon liquid according to a third crystal pulling parameter to obtain a second monocrystalline silicon rod.
In the embodiment of the invention, if the difference is less than or equal to the preset value, the operations of temperature regulation, seeding, shouldering and diameter equalization can be sequentially carried out in the mixed silicon liquid according to the third crystal pulling reference so as to obtain the second monocrystalline silicon rod. Wherein the third crystal pulling parameter comprises a third crucible rotation, a third furnace pressure, a third argon flow and a third pulling speed. In the actual production, after the N-1 single crystal silicon rods are pulled, the pulling parameters for pulling the N-1 single crystal silicon rods are adjusted to be third pulling parameters, in the third pulling parameters, a third crucible is changed to 8-9r/min, a third furnace pressure is 13.5-2torr, a third argon flow is 115-130slpm, and a third pulling speed is 90-80mm/h.
In summary, the method for manufacturing a single crystal silicon rod according to the embodiment of the present invention at least includes the following advantages:
the embodiment of the invention provides a method for manufacturing silicon single crystal rods, wherein mixed silicon liquid is used for drawing N silicon single crystal rods, and according to the segregation effect of a gallium dopant, the quality of the N-1 silicon single crystal rods obtained by drawing is better, so that the silicon single crystal rods can be used for manufacturing solar cells. Since the product drawn by the nth single crystal silicon rod depends on the difference between the weight of the mixed silicon liquid in the crucible and the weight of the crucible bottom material, in the embodiment, when the nth single crystal silicon rod is drawn, a first pulling operation is performed in the mixed silicon liquid according to a first pulling parameter to obtain a first section of single crystal silicon rod with a preset length, and since the first crucible in the first pulling parameter is changed to 10r/min, the first furnace pressure is 15torr, the first argon gas flow is 100slpm and the first pulling speed is 100mm/h, the resistivity of the first section of single crystal silicon rod obtained according to the first pulling parameter is between 0.8 and 3 Ω · cm, the first section of single crystal silicon rod can be used for manufacturing solar cell slices for photovoltaic power generation. And performing a second crystal pulling operation according to a second crystal pulling parameter, continuously connecting a second section of single crystal silicon rod to the first section of single crystal silicon rod to obtain a first single crystal silicon rod with a target length, wherein in the second crystal pulling parameter, the second crucible is changed into 80-90% of the first crucible rotation, the second furnace pressure is 80-90% of the first furnace pressure, the second argon flow is 115-130% of the first argon flow, and the second pulling speed is 80-90% of the first pulling speed. Therefore, according to the segregation effect of the gallium dopant, the N single crystal silicon rods obtained by drawing can be utilized by switching the crystal pulling parameters, so that the waste of materials is avoided, the production cost is reduced, and the availability of the whole single crystal silicon rod is improved.
It should be noted that, for simplicity of description, the method embodiments are described as a series of acts or combination of acts, but those skilled in the art will recognize that the present invention is not limited by the illustrated order of acts, as some steps may occur in other orders or concurrently in accordance with the embodiments of the present invention. Further, those of skill in the art will appreciate that the embodiments described in the specification are presently preferred and that no particular act is required to implement the embodiments of the invention.
The embodiments in the present specification are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
While preferred embodiments of the present invention have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the embodiments of the invention.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or terminal apparatus that comprises the element.
The method for manufacturing a silicon single crystal rod according to the present invention is described in detail above, and the principle and the embodiment of the present invention are explained in detail herein by using specific examples, which are only used to help understanding the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (8)
1. A method for producing a single crystal silicon rod, comprising:
heating and melting a mixed silicon material in a crucible to obtain a mixed silicon liquid, wherein the mixed silicon material comprises a doping agent and a polycrystalline silicon material, the mixed silicon liquid is used for drawing N single crystal silicon rods, and N is an integer greater than or equal to 1;
when the Nth single crystal silicon rod is pulled, calculating the difference value between the weight of the mixed silicon liquid and the weight of a crucible bed charge, wherein the crucible bed charge is the reserved silicon liquid in the crucible;
when the difference is larger than a preset value, performing first crystal pulling operation in the mixed silicon liquid according to a first crystal pulling parameter to obtain a first section of monocrystalline silicon rod with a preset length;
performing a second crystal pulling operation according to a second crystal pulling parameter, and continuously connecting a second section of the monocrystalline silicon rod to the first section of the monocrystalline silicon rod to obtain a first monocrystalline silicon rod with a target length;
performing crystal pulling operation in the mixed silicon liquid according to a third crystal pulling parameter under the condition that the difference is smaller than or equal to the preset value so as to obtain a second monocrystalline silicon rod;
the reserved silicon liquid is the mixed silicon liquid left in the crucible after the Nth single crystal silicon rod is pulled;
wherein the preset value is at least the required weight for manufacturing the monocrystalline silicon chip product;
the preset length is the sum of the switching length and the length of a transition section, and the length of the transition section is between 100 and 200 mm;
wherein the switching length is equal to (m) 1 -m 2 -(l 2 +l 3 )/a 2 )*a 1 -l 1 Wherein m is 1 Represents the weight of the mixed silicon liquid, m 2 Represents the weight of the crucible bottom material, l 1 Denotes the transition section length,/ 2 The required length of a second section of the silicon single crystal rod is shown, the required length of the second section of the silicon single crystal rod is the usable effective length of the second section of the silicon single crystal rod, l 3 Representing a safety length, the safety length being a preset percentage of the target length, the preset percentage being between 8% and 10%, a 1 Representing the conversion coefficient of a first section of single crystal silicon rod, wherein the conversion coefficient of the first section of single crystal silicon rod is the length of the first section of single crystal silicon rod with the diameter corresponding to the required diameter of 1kg of mixed silicon material, a 2 The conversion coefficient of a second section of single crystal silicon rod is expressed, and the conversion coefficient of the second section of single crystal silicon rod is the length of the second section of single crystal silicon rod with the diameter required by the 1kg of mixed silicon material;
wherein the first crystal pulling parameter comprises a first crucible rotation, a first furnace pressure, a first argon flow and a first pulling speed;
the second crystal pulling parameters comprise a second crucible rotation, a second furnace pressure, a second argon gas flow and a second pulling speed, the second crucible rotation is 80% -90% of the first crucible rotation, the second furnace pressure is 80% -90% of the first furnace pressure, the second argon gas flow is 115% -130% of the first argon gas flow, and the second pulling speed is 80% -90% of the first pulling speed;
the target length is the sum of the preset length, the required length of the second section of the silicon single crystal rod and the safety length;
wherein the third crystal pulling parameter comprises a third crucible rotation, a third furnace pressure, a third argon flow and a third pulling speed.
2. The method of claim 1, wherein the step of performing a first crystal pulling operation in the mixed silicon liquid according to first crystal pulling parameters to obtain a first segment of single crystal silicon ingot of a predetermined length comprises:
in the mixed silicon liquid, sequentially performing temperature adjustment, seeding, shouldering and diameter equalization operations according to a first preset parameter to obtain a monocrystalline silicon rod with a transition length;
and adjusting the first crystal pulling parameter to a second crystal pulling parameter while performing the isodiametric operation on the monocrystalline silicon rod with the transition length to obtain a first section of monocrystalline silicon rod with a preset length.
3. The method of claim 2, wherein the step of performing a second crystal pulling operation in accordance with second crystal pulling parameters to continue a second segment of the single crystal silicon ingot on the first segment of the single crystal silicon ingot to obtain a target length of the first single crystal silicon ingot comprises:
and sequentially performing temperature adjustment, seeding, shouldering and diameter equalization according to a second crystal pulling parameter, and continuously connecting a second section of single crystal silicon rod on the first single crystal silicon rod to obtain the first single crystal silicon rod with the target length.
4. The method of claim 1, wherein the resistivity of the first section of the single crystal silicon rod is a first resistivity and the resistivity of the second section of the single crystal silicon rod is a second resistivity, the second resistivity being less than the first resistivity.
5. The method of claim 4, wherein the first resistivity is between 0.8-3 Ω -cm and the second resistivity is between 0.1-2 Ω -cm.
6. The method of claim 1 wherein the second single crystal silicon rod has a resistivity of between 0.1 and 2 Ω -cm.
7. The method of claim 1, wherein the ratio of the preset length to the target length is between (0.35-0.45): 1.
8. The method of claim 1, wherein the dopant is a gallium dopant, and the gallium dopant and the polysilicon material are configured according to a predetermined ratio.
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