CN115323491B - Device and method for preparing high-purity silicon through directional solidification of silicon copper - Google Patents
Device and method for preparing high-purity silicon through directional solidification of silicon copper Download PDFInfo
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- CN115323491B CN115323491B CN202210896817.6A CN202210896817A CN115323491B CN 115323491 B CN115323491 B CN 115323491B CN 202210896817 A CN202210896817 A CN 202210896817A CN 115323491 B CN115323491 B CN 115323491B
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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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
Abstract
The invention discloses a device and a method for preparing high-purity silicon by directional solidification of silicon copper, wherein the device comprises a solidification heater consisting of a fixed box and a crucible, a placing ring is fixedly arranged in the fixed box through two connecting rods, the crucible is clamped and placed in the placing ring, a bottom tray is fixedly arranged in the placing ring through a plurality of reset spring ropes, and a lifting rod is arranged in the placing ring through a sliding mechanism. The advantages are that: the invention provides a method for mainly using industrialization and effectively purifying industrial silicon, which comprises the steps of firstly putting industrial silicon and metallic copper into a directional solidification furnace for smelting for a period of time, then carrying out different directional solidification for two times to obtain a high-purity silicon cast ingot, and carrying out different treatments on different parts of the subsequent high-purity silicon cast ingot to make maximum chemical utilization of raw materials.
Description
Technical Field
The invention relates to the technical field of high-purity silicon preparation, in particular to a device and a method for preparing high-purity silicon by directional solidification of silicon copper.
Background
With the development of human society, the energy problem becomes a great difficulty to be solved in the current urgent need, and the solar energy is used as a novel renewable clean energy source, so that the characteristics of green, environment protection and health are widely paid attention to.
The main raw materials of the solar cell are crystalline silicon materials, wherein polysilicon occupies the market of the main solar cell, and at present, two main purification methods of high-purity silicon used by the polysilicon solar cell are available;
one is a chemical method, which is to gasify industrial silicon into silicon vapor by chemical reaction, then remove impurities step by chemical reaction, and finally reduce the purified silicon vapor into high-purity silicon;
one is a metallurgical process, the so-called physical process, which uses the difference in the physical properties of impurities in silicon to remove them, and typical removal methods include pickling leaching, vacuum refining, directional solidification, and the like.
However, in the purification process of the chemical method, the intermediate product needs to be rectified for many times due to the complex production process, so that the cost is high, and the tail gas treatment after the purification of the chemical method is also a great difficulty;
it is therefore desirable to devise an apparatus for producing high purity silicon by directional solidification of copper-silicon and a method thereof that solves the above problems by employing a method of removing impurities in industrial silicon by a combination of different kinds of processes during the purification by metallurgy.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a device and a method for preparing high-purity silicon by directional solidification of silicon copper.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the utility model provides a device through directional solidification of silico-copper preparation high purity silicon, includes the solidification heater of constituteing by fixed box, crucible, fixed incasement is through two connecting rods fixed mounting place the ring, and the crucible block is placed in placing the ring, place the intra-annular through a plurality of reset spring rope fixed mounting and have the collet, place intra-annular through slide mechanism installs the lifter, through fixed ring fixed mounting heating ring on the lifter, and install the marking mechanism between heating pipe and the fixed box.
In the device for preparing high-purity silicon by directional solidification of silicon copper, the sliding mechanism comprises a trapezoid chute arranged in the fixed box, a trapezoid sliding block is fixedly arranged on the lifting rod, and the trapezoid sliding block is clamped and arranged in the trapezoid chute.
In the device for preparing high-purity silicon by directional solidification of silicon copper, the marking mechanism comprises a scale mark post fixedly arranged in the fixed box, a first marking post matched with the scale mark post is fixedly arranged on the bottom tray, and a second marking post matched with the scale mark post is fixedly arranged on the fixed ring.
In the device for preparing high-purity silicon by directional solidification of silicon copper, the pull rod is slidably arranged between the lifting rod and the fixed box, the fixed box is provided with the sealing cover in a clamping manner, and the side part of the fixed box is fixedly provided with the plurality of heat dissipation nets.
In the above method for preparing high purity silicon by directional solidification of silicon copper, the method comprises the following steps:
s1, placing industrial silicon and metallic copper to be purified into a directional solidification furnace, introducing argon into the furnace, raising the temperature in the furnace to 1500-1700 ℃, and preserving heat for 2-4 hours;
s2, carrying out first directional solidification on the molten silicon-copper alloy obtained in the step S1 after heat preservation to obtain a first directional solidified silicon cast ingot, wherein the solidification mode is that the molten silicon-copper alloy is placed in a crucible, the crucible is clamped on a placing ring, a heating ring is started to heat the crucible, a pull rod is pulled to drive a lifting rod, a fixing ring and the heating ring to move from bottom to top during heating, and the molten silicon-copper alloy can be shaped and solidified, and the heating ring is a heating source in a solidification heater;
s3, carrying out secondary directional solidification on the primary directional solidification cast ingot obtained in the step S2 in a solidification heater, wherein the solidification mode is that a pull rod is pulled to drive a lifting rod, a fixed ring and a heating ring to move, the heating ring is lowered to a position which is one third away from the bottom end of the crucible according to the scale marking positions of a first marking rod and a second marking rod on a scale marking rod, and the heating ring is started and is moved upwards, so that the secondary directional solidification can be started;
s4, cutting the high-purity silicon ingot obtained in the step S3 after the secondary directional solidification into three sections averagely, and carrying out different treatments on different parts, wherein the specific operation is as follows:
(1) recovering the high-purity silicon ingot at the bottom and directly using the high-purity silicon ingot for production;
(2) the silicon ingot in the middle part is used for production after being subjected to mixed acid pickling of hydrochloric acid and hydrofluoric acid;
(3) the top ingot is mixed with other raw materials for remelting.
In the above method for preparing high purity silicon by directional solidification of silicon copper, in the step S1, the industrial silicon and the metallic copper are used in the form of silicon blocks and copper blocks, respectively, and the mass ratio of the addition amounts of the industrial silicon and the copper blocks is (1-1.2): 1; the purity of the industrial silicon is 2-3N, and the purity of the copper block is 3-4N; argon purity was 4N and aeration flow was 400ml/min.
In the method for preparing the high-purity silicon by directional solidification of the silicon copper, the temperature of a heating source in the step S2 is 1400-1600 ℃, the vertical upward temperature gradient of the directional solidification is set to be 15-50 ℃/cm, and the speed of the heating source moving from bottom to top is 10-20 mm/h.
In the method for preparing the high-purity silicon by directional solidification of the silicon copper, the heating temperature in the step S3 is 1300-1500 ℃, the vertical upward temperature gradient of the directional solidification is set to be 15-50 ℃/cm, and the speed of the heating source moving from bottom to top is 10-20 mm/h.
In the method for preparing high-purity silicon by directional solidification of silicon copper, the concentration of hydrofluoric acid in the mixed solution in the step S4 is 2-3 mol/L, the concentration of hydrochloric acid is 1-3 mol/L, the pickling temperature is 50-80 ℃, and the time is 3-6 h.
Compared with the prior art, the invention has the advantages that: the invention provides a method for mainly using industrialization and effectively purifying industrial silicon, which comprises the steps of firstly putting industrial silicon and metallic copper into a directional solidification furnace for smelting for a period of time, then carrying out different directional solidification for two times to obtain a high-purity silicon ingot, and carrying out different treatments on different parts of the subsequent high-purity silicon ingot so as to maximally utilize raw materials.
Drawings
The invention is described in further detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic diagram of an apparatus for preparing high purity silicon by directional solidification of copper silicon and a method thereof according to the present invention;
FIG. 2 is a top view of the placement ring of FIG. 1 with a portion of the attachment structure thereon;
FIG. 3 is a flow chart of the preparation of high purity silicon according to the present invention.
In the figure: the device comprises a fixed box 1, a connecting rod 2, a placing ring 3, a crucible 4, a lifting rod 5, a fixed ring 6, a heating ring 7, a tray 8, a marking rod 9I, a marking rod 10 II, a graduation scale 11, a heat dissipation net 12 and a return spring rope 13.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1-2, a device for preparing high purity silicon by directional solidification of silicon copper comprises a solidification heater composed of a fixed box 1 and a crucible 4, wherein a placing ring 3 is fixedly installed in the fixed box 1 through two connecting rods 2, the crucible 3 is clamped and placed in the placing ring 3, a bottom tray 8 is fixedly installed in the placing ring 3 through a plurality of reset spring ropes 13, a lifting rod 5 is installed in the placing ring 3 through a sliding mechanism, a heating ring 7 is fixedly installed on the lifting rod 5 through a fixed ring 6, and a marking mechanism is installed between the heating pipe 7 and the fixed box 1;
the sliding mechanism comprises a trapezoid chute arranged in the fixed box 1, a trapezoid slider is fixedly arranged on the lifting rod 5 and is clamped and arranged in the trapezoid chute, and the sliding mechanism is used for enabling the lifting rod 5 to move up and down only in the fixed box 1 without being deviated from the lifting rod 5.
The marking mechanism comprises a scale marking rod 11 fixedly arranged in the fixed box 1, a marking rod I9 matched with the scale marking rod 11 is fixedly arranged on the bottom tray 8, a marking rod II 10 matched with the scale marking rod 11 is fixedly arranged on the fixed ring 6, and the relative position between the heating ring 7 and the crucible 4 can be judged through the relative positions of the scales of the marking rod I9 and the marking rod II 10 on the scale marking rod 11.
A pull rod is slidably arranged between the lifting rod 5 and the fixed box 1, a sealing cover is arranged on the fixed box 1 in a clamping manner, and a plurality of heat dissipation nets 12 are fixedly arranged on the side part of the fixed box 1.
The solidification mode of one-time directional solidification is that the silicon-copper molten alloy is put into a crucible 4, the crucible 4 is clamped on a placement ring 3, a heating ring 7 is started to heat the crucible 4, a pull rod is pulled to drive a lifting rod 5, a fixing ring 6 and the heating ring 7 to move from bottom to top during heating, and the silicon-copper molten alloy can be shaped and solidified, and the heating ring 7 is a heating source in a solidification heater;
the solidification mode of the secondary directional solidification is that the pull rod is pulled to drive the lifting rod 5, the fixed ring 6 and the heating ring 7 to move, the heating ring 7 is lowered to a position which is one third away from the bottom end of the crucible 4 according to the scale marking positions of the marking rod I9 and the marking rod II 10 on the scale marking rod 11 as the reference, and the heating ring 7 is started to move upwards, so that the secondary directional solidification can be started
Example 1
Referring to fig. 1-3, a method for preparing high purity silicon by directional solidification of silicon copper, comprising the steps of:
s1, placing 15kg of industrial silicon to be purified (with the purity of 99.8%) and 15kg of metal copper blocks (with the purity of 99.99%) into a directional solidification furnace, introducing 4N argon into the furnace at 400ml/min, heating the furnace to 1500 ℃, and preserving heat for 2 hours;
s2, after the silicon-copper molten alloy obtained in the step S2 is insulated, setting the temperature gradient in the vertical direction of directional solidification to be 15 ℃/cm, and starting a directional solidification lifting device to enable a heating source to move from bottom to top at a speed of 10mm/h for performing first directional solidification, so as to obtain a first directional solidification silicon cast ingot;
s3, performing second directional solidification on the primary directional solidification cast ingot obtained in the step S2, and lowering the heating source to a position which is one third away from the bottom end of the crucible to start the second directional solidification. Setting the temperature gradient in the vertical direction of directional solidification to be 15 ℃/cm, starting a directional solidification lifting device to enable a heating source to move from bottom to top at a speed of 10mm/h for performing second directional solidification, and obtaining a second directional solidification cast ingot;
s4, cutting the high-purity silicon ingot obtained in the step S3 after the secondary directional solidification into three sections averagely, and carrying out different treatments on different parts, wherein the specific operation is as follows:
(1) recovering the high-purity silicon ingot at the bottom and directly using the high-purity silicon ingot for production;
(2) pickling the silicon ingot in the middle by using mixed acid consisting of 2mol/L hydrochloric acid and 2mol/L hydrofluoric acid, pickling for 3 hours at 50 ℃, filtering, and washing with deionized water for production;
(3) the top ingot is mixed with other raw materials for remelting.
The bottom silicon purity was 99.99924% as determined by Glow Discharge Mass Spectrometry (GDMS). The silicon purity in the middle was 99.99917%.
Example 2
Referring to fig. 1-3, a method for preparing high purity silicon by directional solidification of silicon copper, comprising the steps of:
s1, placing 15kg of industrial silicon to be purified (with the purity of 99.8%) and 15kg of metal copper blocks (with the purity of 99.99%) into a directional solidification furnace, introducing 4N argon into the furnace at 400ml/min, heating the furnace to 1600 ℃, and preserving heat for 3 hours;
s2, after the silicon-copper molten alloy obtained in the step S1 is insulated, setting the temperature gradient in the vertical direction of directional solidification to be 20 ℃/cm, and starting a directional solidification lifting device to enable a heating source to move from bottom to top at a speed of 15mm/h for performing first directional solidification, so as to obtain a first directional solidification silicon cast ingot;
s3, performing second directional solidification on the primary directional solidification cast ingot obtained in the step S2, and lowering the heating source to a position which is one third away from the bottom end of the crucible to start the second directional solidification. Setting the temperature gradient in the vertical direction of directional solidification as 20 ℃/cm, starting a directional solidification lifting device to enable a heating source to move from bottom to top at a speed of 15mm/h for performing second directional solidification, and obtaining a second directional solidification cast ingot;
s4, cutting the high-purity silicon ingot obtained in the step S3 after the secondary directional solidification into three sections averagely, and carrying out different treatments on different parts, wherein the specific operation is as follows:
(1) recovering the high-purity silicon ingot at the bottom and directly using the high-purity silicon ingot for production;
(2) pickling the silicon ingot in the middle by using mixed acid consisting of 3mol/L hydrochloric acid and 1mol/L hydrofluoric acid, pickling for 6 hours at 50 ℃, filtering, and washing with deionized water for production;
(3) the top ingot is mixed with other raw materials for remelting.
The bottom silicon purity was 99.99967% as determined by Glow Discharge Mass Spectrometry (GDMS). The silicon purity in the middle was 99.99956%.
Example 3
Referring to fig. 1-3, a method for preparing high purity silicon by directional solidification of silicon copper, comprising the steps of:
s1, placing 15kg of industrial silicon to be purified (with the purity of 99.8%) and 15kg of metal copper blocks (with the purity of 99.99%) into a directional solidification furnace, introducing 4N argon into the furnace at 400ml/min, heating the furnace to 1700 ℃, and preserving heat for 4 hours;
s2, after the silicon-copper molten alloy obtained in the step S1 is insulated, setting the temperature gradient in the vertical direction of directional solidification to be 50 ℃/cm, and starting a directional solidification lifting device to enable a heating source to move from bottom to top at a speed of 20mm/h for performing first directional solidification, so as to obtain a first directional solidification silicon cast ingot;
s3, performing second directional solidification on the primary directional solidification cast ingot obtained in the step S2, and lowering the heating source to a position which is one third away from the bottom end of the crucible to start the second directional solidification. Setting the temperature gradient in the vertical direction of directional solidification to be 50 ℃/cm, starting a directional solidification lifting device to enable a heating source to move from bottom to top at a speed of 20mm/h for performing second directional solidification, and obtaining a second directional solidification cast ingot;
s4, cutting the high-purity silicon ingot obtained in the step S3 after the secondary directional solidification into three sections averagely, and carrying out different treatments on different parts, wherein the specific operation is as follows:
(1) recovering the high-purity silicon ingot at the bottom and directly using the high-purity silicon ingot for production;
(2) pickling the silicon ingot in the middle by using mixed acid consisting of 3mol/L hydrochloric acid and 3mol/L hydrofluoric acid, pickling for 6 hours at 80 ℃, filtering, and washing with deionized water for production;
(3) the top ingot is mixed with other raw materials for remelting.
The bottom silicon purity was 99.99988% as determined by Glow Discharge Mass Spectrometry (GDMS). The silicon purity in the middle was 99.99967%.
Further, the above-described fixed connection is to be understood in a broad sense, unless explicitly stated and defined otherwise, as being, for example, welded, glued, or integrally formed, as is well known to those skilled in the art.
It is noted that relational terms such as first and second, and the like are 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. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus 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 apparatus.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (5)
1. The use method of the device for preparing the high-purity silicon through directional solidification of the silicon copper comprises a solidification heater consisting of a fixed box (1) and a crucible (4), and is characterized in that a placement ring (3) is fixedly installed in the fixed box (1) through two connecting rods (2), the crucible (4) is clamped and placed in the placement ring (3), a bottom tray (8) is fixedly installed in the placement ring (3) through a plurality of reset spring ropes (13), a lifting rod (5) is installed in the placement ring (3) through a sliding mechanism, a heating ring (7) is fixedly installed on the lifting rod (5) through a fixed ring (6), and a marking mechanism is installed between the heating ring (7) and the fixed box (1); the sliding mechanism comprises a trapezoid chute arranged in the fixed box (1), a trapezoid sliding block is fixedly arranged on the lifting rod (5), and the trapezoid sliding block is clamped and arranged in the trapezoid chute; the marking mechanism comprises a scale mark post (11) fixedly arranged in the fixed box (1), a first marking post (9) matched with the scale mark post (11) is fixedly arranged on the bottom tray (8), and a second marking post (10) matched with the scale mark post (11) is fixedly arranged on the fixed ring (6); a pull rod is slidably arranged between the lifting rod (5) and the fixed box (1), a sealing cover is arranged on the fixed box (1) in a clamping manner, and a plurality of heat dissipation nets (12) are fixedly arranged on the side part of the fixed box (1);
the application method of the device for preparing the high-purity silicon by directional solidification of the silicon copper comprises the following steps:
s1, placing industrial silicon and metallic copper to be purified into a directional solidification furnace, introducing argon into the furnace, raising the temperature in the furnace to 1500-1700 ℃, and preserving heat for 2-4 hours;
s2, carrying out first directional solidification on the silicon-copper molten alloy obtained in the step S1 after heat preservation to obtain a first directional solidified silicon cast ingot, wherein the solidification mode is that the silicon-copper molten alloy is placed into a crucible (4), the crucible (4) is clamped on a placement ring (3), a heating ring (7) is started to heat the crucible (4), and when heating is carried out, a pull rod is pulled to drive a lifting rod (5), a fixing ring (6) and the heating ring (7) to move from bottom to top, so that the silicon-copper molten alloy can be shaped and solidified, and the heating ring (7) is a heating source in a solidification heater;
s3, carrying out secondary directional solidification on the primary directional solidification cast ingot obtained in the step S2 in a solidification heater, wherein the solidification mode is that a pull rod is pulled to drive a lifting rod (5), a fixed ring (6) and a heating ring (7) to move, the heating ring (7) is lowered to a position which is one third away from the bottom end of a crucible (4) according to the scale marking positions of a first marking rod (9) and a second marking rod (10) on a scale marking rod (11), and the heating ring (7) is started and is moved upwards, so that secondary directional solidification can be started;
s4, cutting the high-purity silicon ingot obtained in the step S3 after the secondary directional solidification into three sections averagely, and carrying out different treatments on different parts, wherein the specific operation is as follows:
(1) Recovering the high-purity silicon ingot at the bottom and directly using the high-purity silicon ingot for production;
(2) The silicon ingot in the middle part is used for production after being subjected to mixed acid pickling of hydrochloric acid and hydrofluoric acid;
(3) The top ingot is mixed with other raw materials for remelting.
2. The method of claim 1, wherein in the step S1, the industrial silicon and the metallic copper are used in the form of a silicon block and a copper block, respectively, and the mass ratio of the addition amounts of the industrial silicon and the copper block is (1-1.2): 1; the purity of the industrial silicon is 2-3N, and the purity of the copper block is 3-4N; argon purity was 4N and aeration flow was 400ml/min.
3. The use method of the device for preparing the high-purity silicon through directional solidification of the silicon copper according to claim 1, wherein the temperature of a heating source in the step S2 is 1400-1600 ℃, a directional solidification vertical upward temperature gradient is set to be 15-50 ℃/cm, and the speed of the heating source moving from bottom to top is 10-20 mm/h.
4. The use method of the device for preparing the high-purity silicon through directional solidification of the silicon copper according to claim 1, wherein in the step S3, the heating temperature is 1300-1500 ℃, the vertical upward temperature gradient of the directional solidification is set to be 15-50 ℃/cm, and the speed of the heating source moving from bottom to top is 10-20 mm/h.
5. The use method of the device for preparing the high-purity silicon through directional solidification of the silicon copper according to claim 1, wherein the concentration of hydrofluoric acid in the mixed solution of the step S4 is 2-3 mol/L, the concentration of hydrochloric acid is 1-3 mol/L, the pickling temperature is 50-80 ℃, and the pickling time is 3-6 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005162507A (en) * | 2003-11-28 | 2005-06-23 | Sharp Corp | Polycrystal semiconductor ingot and its manufacturing device and method |
| KR100916843B1 (en) * | 2009-01-13 | 2009-09-14 | 김영조 | Manufacturing high efficiency equipment for polysilicon ingot |
| CN101824650A (en) * | 2010-05-20 | 2010-09-08 | 上海太阳能电池研究与发展中心 | Purifying system of high purity polysilicon and purifying method |
| CN101928841A (en) * | 2010-03-24 | 2010-12-29 | 峨嵋半导体材料研究所 | Preparation process of hyperpure lead |
| JP2016124713A (en) * | 2014-12-26 | 2016-07-11 | 京セラ株式会社 | Method of producing polycrystalline silicon ingot |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005162507A (en) * | 2003-11-28 | 2005-06-23 | Sharp Corp | Polycrystal semiconductor ingot and its manufacturing device and method |
| KR100916843B1 (en) * | 2009-01-13 | 2009-09-14 | 김영조 | Manufacturing high efficiency equipment for polysilicon ingot |
| CN101928841A (en) * | 2010-03-24 | 2010-12-29 | 峨嵋半导体材料研究所 | Preparation process of hyperpure lead |
| CN101824650A (en) * | 2010-05-20 | 2010-09-08 | 上海太阳能电池研究与发展中心 | Purifying system of high purity polysilicon and purifying method |
| JP2016124713A (en) * | 2014-12-26 | 2016-07-11 | 京セラ株式会社 | Method of producing polycrystalline silicon ingot |
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