CN114408927A - Preparation method and preparation device of high-purity silicon core - Google Patents
Preparation method and preparation device of high-purity silicon core Download PDFInfo
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- CN114408927A CN114408927A CN202111592084.9A CN202111592084A CN114408927A CN 114408927 A CN114408927 A CN 114408927A CN 202111592084 A CN202111592084 A CN 202111592084A CN 114408927 A CN114408927 A CN 114408927A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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- B28D5/045—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools by cutting with wires or closed-loop blades
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Abstract
The invention provides a preparation method and a preparation device of a high-purity silicon core, which relate to the technical field of polycrystalline silicon production, and the preparation method of the high-purity silicon core comprises the following steps: a starting stage: placing a silicon core in a reaction container, and increasing the surface temperature of the silicon core; introducing a preheated material into the reaction container to enable the silicon core to grow; and (3) growth stage: introducing a preheated material into the reaction container, and raising the surface temperature of the silicon core to enable the silicon rod to grow rapidly; and (3) adjusting: repairing the silicon rod; taking out the repaired silicon rod from the reaction container, and cutting to form a plurality of high-purity silicon cores; wherein, the flow rate of the preheating material in the starting stage is 800-1200kg/h, and the flow rate of the preheating material in the growth stage is 4000-5500 kg/h. The preparation method of the high-purity silicon core can relieve the problems of impurity introduction and uneven silicon core quality in the preparation process of the silicon core, thereby improving the production quality.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon production, in particular to a preparation method and a preparation device of a high-purity silicon core.
Background
At present, in the production of polycrystalline silicon, the following methods are often employed: a plurality of thin silicon cores are arranged in a Chemical Vapor Deposition (CVD) reactor to be used as carriers, and a silicon core beam is built to form a conductive loop. When the CVD reactor is in operation, the surface of the silicon rod is maintained in a certain temperature range in an electric heating mode, silicon-containing gas and reducing gas are introduced into the furnace to achieve reaction conditions, and elemental silicon is deposited on the surface of the silicon rod to realize the growth of the polycrystalline silicon rod. Because carrier thin silicon cores prepared by polycrystalline silicon in the reduction furnace cannot be completely separated in finished products, the impurity content of the silicon cores can directly influence the quality of the polycrystalline silicon rods of the products.
Generally, a silicon core carrier used in a CVD reactor for preparing polycrystalline silicon is prepared by a czochralski silicon single crystal rod cutting process or a polycrystalline silicon masterbatch zone-melting drawing process. Common to both processes is that: the raw silicon rod needs to be melted, silicon in a molten state is active in chemical property, is easy to react with contact substances to introduce pollution, and impurities are easy to diffuse and permeate to form impurities in a body. In addition, impurity segregation phenomena exist in the processes of straight pulling and zone melting, namely concentration gradients exist at the upper end and the lower end of the prepared silicon core due to the impurity content, the quality of the silicon core is uneven, and the final classification of the polycrystalline silicon product is complicated.
Disclosure of Invention
The invention aims to provide a preparation method and a preparation device of a high-purity silicon core, which are used for solving the technical problems that impurities are easy to introduce in the preparation process of the silicon core and the quality of the silicon core is not uniform in the prior art.
The preparation method of the high-purity silicon core provided by the invention comprises the following steps: a starting stage: placing a silicon core in a reaction container, and increasing the surface temperature of the silicon core; introducing a preheated material into the reaction container to enable the silicon core to grow; and (3) growth stage: introducing a preheated material into the reaction container, and raising the surface temperature of the silicon core to enable the silicon rod to grow rapidly; and (3) adjusting: repairing the silicon rod; taking out the repaired silicon rod from the reaction container, and cutting to form a plurality of high-purity silicon cores; wherein, the flow rate of the preheating material in the starting stage is 800-1200kg/h, and the flow rate of the preheating material in the growth stage is 4000-5500 kg/h.
Further, silicon rods are cut by adopting three rows of cutting lines in a mode that the included angle of each row is 60 degrees, so that a plurality of high-purity silicon cores with regular triangular cross sections are formed.
Further, the preheated material includes a reducing gas and a silicon-containing gas.
Furthermore, in the growth stage, the molar ratio of the reducing gas to the silicon-containing gas is 2-3.
Furthermore, in the adjusting stage, the molar ratio of the reducing gas to the silicon-containing gas is 5-8.
Further, in the starting stage, the surface temperature of the silicon core is raised to be more than 1000 ℃.
Further, the diameter difference of the two ends of the silicon rod is less than or equal to 15 mm.
Further, the diameter difference between the thickest diameter and the thinnest diameter of the eccentric position of the silicon rod is less than or equal to 15 mm.
Further, the invention also provides a high-purity silicon core preparation device, which comprises a reduction furnace; an air inlet, an air outlet and a monitoring mechanism are arranged on a chassis of the reduction furnace; the monitoring mechanism is used for monitoring internal flow field data and temperature field data in the reduction furnace.
Further, the high-purity silicon core preparation device also comprises a current controller and an airflow controller; the monitoring mechanism is respectively connected with the current controller and the airflow controller to realize linkage.
According to the preparation method of the high-purity silicon core, the preheating material with small flow is introduced in the starting stage, so that the conditions of lodging and burr growth of the silicon core in the growth process are avoided; a large flow of preheated material is introduced in the growth stage to enable the silicon rod to grow rapidly, so that the primary conversion rate is improved; in the adjusting stage, the silicon rod can be more compact and uniform through fine adjustment and repair, and the apparent appearance and the like meet the subsequent cutting requirements. The large-diameter high-purity compact polycrystalline silicon rod obtained by the steps has high mechanical strength and strong machinability, and compared with the prior art, the large-diameter high-purity compact polycrystalline silicon rod improves the efficiency of preparing a silicon core and the utilization rate of the silicon core, can save the production cost and reduce the energy consumption. On the other hand, the method avoids the possible pollution in the process of preparing the silicon core in the prior art, avoids the problem of introducing impurities into the silicon rod, and improves the quality of the polysilicon product; and the problems of uneven silicon core quality and complicated classification of the grades of the polysilicon products are avoided.
Therefore, the preparation method of the high-purity silicon core can relieve the problems of impurity introduction and uneven quality of the silicon core in the preparation process of the silicon core, thereby improving the production quality.
According to the high-purity silicon core preparation device provided by the invention, in the using process, a user places the silicon core in the reduction furnace, the preheated material is introduced from the air inlet, and the monitoring mechanism is used for monitoring the internal flow field data and the temperature field data in the reduction furnace so as to adjust the current and the air flow according to actual requirements. The silicon rod generated in the reducing furnace can be directly cut in a cutting mode, so that the efficiency and the utilization rate of silicon cores are improved, the production cost can be saved, and the energy consumption can be reduced. On the other hand, the method can also avoid possible pollution in the process of preparing the silicon core in the prior art, avoid the problem of impurity introduction, improve the quality of the polysilicon product, and simultaneously avoid the problems of uneven quality of the silicon core and complicated classification of the grade of the polysilicon product.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a block diagram illustrating steps of a method for manufacturing a high purity silicon core according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a high purity silicon core cut into a plurality of regular triangular cross sections according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a high-purity silicon core preparation apparatus according to an embodiment of the present invention.
Icon: 1-a reduction furnace; 2-a chassis; 3-an air inlet; 4-air outlet; 5-a monitoring mechanism; 6-a current controller; 7-air flow controller.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
FIG. 1 is a block diagram illustrating steps of a method for manufacturing a high purity silicon core according to an embodiment of the present invention; as shown in fig. 1, the method for preparing a high-purity silicon core according to the embodiment of the present invention includes the following steps: a starting stage: placing a silicon core in a reaction container, and increasing the surface temperature of the silicon core; introducing a preheated material into the reaction container to enable the silicon core to grow; and (3) growth stage: introducing a preheated material into the reaction container, and raising the surface temperature of the silicon core to enable the silicon rod to grow rapidly; and (3) adjusting: repairing the silicon rod; taking out the repaired silicon rod from the reaction container, and cutting to form a plurality of high-purity silicon cores; wherein, the flow rate of the preheating material in the starting stage is 800-1200kg/h, and the flow rate of the preheating material in the growth stage is 4000-5500 kg/h.
Wherein the running time of the starting phase is 10-25 h.
Furthermore, 5000-.
Further, in the starting stage, the surface temperature of the silicon core is raised to be more than 1000 ℃.
Furthermore, the running time of the growth phase is 50-80 h.
Furthermore, the running time of the adjusting stage is 10-20 h.
Further, in the adjustment stage, the appearance and the compactness of the silicon rod need to be repaired.
Further, the preheated material includes a reducing gas and a silicon-containing gas.
The reducing gas can be hydrogen, and the silicon-containing gas can be trichlorosilane or dichlorosilane.
Furthermore, when repairing, the molar ratio of the reducing gas and the silicon-containing gas is adjusted, and the flow rate of the reducing gas is increased.
Furthermore, in the growth stage, the molar ratio of the reducing gas to the silicon-containing gas is 2-3.
Furthermore, in the adjusting stage, the molar ratio of the reducing gas to the silicon-containing gas is 5-8.
Further, the diameter Φ of the silicon rod: the diameter phi 1 of the root part is 100mm above the graphite chuck, the diameter phi 2 of the top part is 100mm below the connection part of the cross beam, and phi is equal to (phi 1+ phi 2)/2 and is not less than 150 mm. In the using process, the silicon rod at the root part contains the graphite clamping flap, and the silicon rod at the top part is rough and cannot be used, so the silicon rod is cut off at the two positions to ensure the quality of the silicon core.
Further, the diameter difference between the thickest diameter and the thinnest diameter of the eccentric position of the silicon rod is less than or equal to 15 mm.
Wherein the surface of the silicon rod is uneven, and bulges and depressions exist; a reference line is defined for the silicon rod in a direction parallel to the surface of the silicon rod. The position above the reference line is called a protrusion and the position below the reference line is called a depression. The distance between the convex peak point and the concave valley point respectively and the reference line is less than or equal to 3 mm.
In addition, the minimum distance between adjacent protrusions, and the minimum distance between adjacent depressions, should each be less than or equal to 3 mm.
Further, the silicon rod bending and straightening degree: the diameter phi 3 of the thinnest eccentric position and the diameter phi 4 of the thickest eccentric position are as follows: and delta phi 4-phi 3 is less than or equal to 15 mm.
Furthermore, the diameter difference of the two ends of the silicon rod is less than or equal to 15mm, namely the big end delta phi of the silicon rod is phi 2-phi 1 and is less than or equal to 15 mm.
Furthermore, in the cutting process, the silicon rod can be cut into silicon cores with different shapes and sizes by adopting cutting equipment such as diamond wires and the like according to the requirements of users.
According to the preparation method of the high-purity silicon core, provided by the embodiment of the invention, a small-flow preheating material is introduced in the starting stage, so that the conditions of lodging and burr growth of the silicon core in the growth process are avoided; a large flow of preheated material is introduced in the growth stage to enable the silicon rod to grow rapidly, so that the primary conversion rate is improved; in the adjusting stage, the silicon rod can be more compact and uniform through fine adjustment and repair, and the apparent appearance and the like meet the subsequent cutting requirements. The large-diameter high-purity compact polycrystalline silicon rod obtained by the steps has high mechanical strength and strong machinability, and compared with the prior art, the large-diameter high-purity compact polycrystalline silicon rod improves the efficiency of preparing a silicon core and the utilization rate of the silicon core, can save the production cost and reduce the energy consumption. On the other hand, the method avoids the possible pollution in the process of preparing the silicon core in the prior art, avoids the problem of introducing impurities into the silicon rod, improves the quality of the polysilicon product, and avoids the problems of uneven quality of the silicon core and complicated classification of the grade of the polysilicon product.
Therefore, the preparation method of the high-purity silicon core can relieve the problems of impurity introduction and uneven quality of the silicon core in the preparation process of the silicon core, thereby improving the production quality.
FIG. 2 is a schematic diagram of a high purity silicon core cut into a plurality of regular triangular cross sections according to an embodiment of the present invention; as shown in fig. 2, in addition to the above-mentioned examples, the silicon rod was further cut using three rows of cutting lines, each row having a pinch angle of 60 °, to form a plurality of high purity silicon cores having a regular triangular cross section.
In the embodiment, the cutting method can obtain the regular-triangular high-purity silicon cores, so that the utilization rate of the silicon rods can be improved through covering, and more high-purity silicon cores can be obtained.
FIG. 3 is a schematic structural diagram of a high purity silicon core preparation apparatus provided in an embodiment of the present invention; as shown in fig. 3, on the basis of the above embodiment, further, the embodiment of the present invention further provides a high purity silicon core preparation apparatus, which includes a reduction furnace 1; an air inlet 3, an air outlet 4 and a monitoring mechanism 5 are arranged on a chassis 2 of the reducing furnace 1; the monitoring mechanism 5 is used for monitoring internal flow field data and temperature field data inside the reduction furnace 1.
The current and airflow regulation and control parameters of the reduction furnace 1 can be obtained through simulation calculation according to actual requirements.
In the embodiment, in the using process, a user places the silicon core inside the reduction furnace 1, the preheated material is introduced from the air inlet 3, and the monitoring mechanism 5 is used for monitoring internal flow field data and temperature field data inside the reduction furnace 1 so as to adjust the flow of current and air flow according to actual requirements. The silicon rod generated in the reducing furnace 1 can be cut directly by adopting a cutting mode, so that the silicon core preparation efficiency and the silicon core utilization rate are improved, the production cost can be saved, and the energy consumption is reduced. On the other hand, the method can also avoid possible pollution in the process of preparing the silicon core in the prior art, avoid the problem of impurity introduction, improve the quality of the polysilicon product, and simultaneously avoid the problems of uneven quality of the silicon core and complicated classification of the grade of the polysilicon product.
As shown in fig. 3, on the basis of the above embodiment, further, the high purity silicon core preparation apparatus further comprises a current controller 6 and a gas flow controller 7; the monitoring mechanism 5 is respectively connected with a current controller 6 and an air current controller 7 so as to realize linkage.
In this embodiment, the monitoring mechanism 5 is configured to monitor internal flow field data and temperature field data inside the reduction furnace 1, and transmit the two data to the current controller 6 and the airflow controller 7, respectively, so as to adjust the current and the airflow, thereby more accurately controlling the silicon rod growth environment in the reduction furnace 1, improving the quality of the silicon rod, and further improving the quality of the polysilicon product.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a high-purity silicon core is characterized by comprising the following steps:
a starting stage: placing a silicon core in a reaction container, and increasing the surface temperature of the silicon core; introducing a preheated material into the reaction container to enable the silicon core to grow;
and (3) growth stage: introducing a preheated material into the reaction container, and raising the surface temperature of the silicon core to enable the silicon rod to grow rapidly;
and (3) adjusting: repairing the silicon rod;
taking out the repaired silicon rod from the reaction container, and cutting to form a plurality of high-purity silicon cores;
wherein, the flow rate of the preheating material in the starting stage is 800-1200kg/h, and the flow rate of the preheating material in the growth stage is 4000-5500 kg/h.
2. The method for preparing high-purity silicon cores according to claim 1, wherein the silicon rod is cut by three rows of cutting lines, and the included angle of each row is 60 degrees, so as to form a plurality of high-purity silicon cores with regular triangular cross sections.
3. The method for preparing high purity silicon core according to claim 1 or 2, wherein the pre-heated material comprises reducing gas and silicon-containing gas.
4. The method for preparing high-purity silicon cores according to claim 3, wherein the molar ratio of the reducing gas to the silicon-containing gas is 2-3 in the growth stage.
5. The method for preparing high-purity silicon cores according to claim 3, wherein the molar ratio of the reducing gas to the silicon-containing gas is 5-8 in the adjusting stage.
6. The method for preparing high purity silicon core according to claim 1, wherein the temperature of the surface of the silicon core is raised to 1000 ℃ or higher in the start-up stage.
7. The method for preparing high-purity silicon cores according to claim 1, wherein the difference between the diameters of the two ends of the silicon rod is less than or equal to 15 mm.
8. The method for preparing high-purity silicon cores according to claim 1, wherein the diameter difference between the thickest diameter and the thinnest diameter of the eccentric position of the silicon rod is less than or equal to 15 mm.
9. The high-purity silicon core preparation device is characterized by comprising a reduction furnace;
an air inlet, an air outlet and a monitoring mechanism are arranged on a chassis of the reduction furnace; the monitoring mechanism is used for monitoring internal flow field data and temperature field data in the reduction furnace.
10. The apparatus of claim 9, wherein the apparatus further comprises a current controller and a gas flow controller; the monitoring mechanism is respectively connected with the current controller and the airflow controller to realize linkage.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020277A (en) * | 2010-12-24 | 2011-04-20 | 中科协鑫（苏州）工业研究院有限公司 | Method for depositing polycrystalline silicon by adopting surface microstructure silicon core |
| CN104118879A (en) * | 2014-08-06 | 2014-10-29 | 四川永祥多晶硅有限公司 | Preparation method of silicon core master batch |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020277A (en) * | 2010-12-24 | 2011-04-20 | 中科协鑫（苏州）工业研究院有限公司 | Method for depositing polycrystalline silicon by adopting surface microstructure silicon core |
| CN104118879A (en) * | 2014-08-06 | 2014-10-29 | 四川永祥多晶硅有限公司 | Preparation method of silicon core master batch |
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