CN110965120A - Method for separating primary silicon in hypereutectic aluminum-silicon alloy - Google Patents
Method for separating primary silicon in hypereutectic aluminum-silicon alloy Download PDFInfo
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 72
- 239000010703 silicon Substances 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910000676 Si alloy Inorganic materials 0.000 title claims abstract description 30
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000003723 Smelting Methods 0.000 claims abstract description 34
- 230000006698 induction Effects 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000004857 zone melting Methods 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 20
- 239000011863 silicon-based powder Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 6
- 239000000956 alloy Substances 0.000 abstract description 6
- 238000007711 solidification Methods 0.000 abstract description 5
- 230000008023 solidification Effects 0.000 abstract description 5
- 238000007670 refining Methods 0.000 abstract description 4
- 239000000155 melt Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
-
- 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
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
-
- 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 method for separating primary silicon from hypereutectic aluminum-silicon alloy, which adopts an induction heating area smelting process to melt and solidify the aluminum-silicon alloy, realizes the enrichment of the primary silicon at the bottom of a sample and achieves the aim of high-efficiency separation; the method specifically comprises the steps of preparing an aluminum-silicon alloy ingot by using industrial silicon and industrial aluminum as raw materials, and carrying out induction heating area smelting on the ingot by adopting an area smelting process. And taking out the sample after zone melting, and intercepting the primary silicon enriched part at the bottom of the sample to carry out acid washing so as to recover the high-purity silicon. The method solves the problems of difficult separation and low separation efficiency of primary silicon from the melt in the alloy solidification refining process, can realize high-efficiency separation of the primary silicon in the aluminum-silicon alloy, can enlarge or prolong the diameter and the length of a sample along with the actual condition, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of preparing solar grade polysilicon by a metallurgical method, and particularly relates to a method for separating primary silicon in hypereutectic aluminum-silicon alloy by adopting a zone melting process.
Background
Solar grade polysilicon is the main raw material of silicon solar cells, and the preparation process thereof is always the key point of research in the solar energy field. Among the methods for preparing solar grade polysilicon by purifying metallurgical silicon, the Al-Si alloy solidification refining method has attracted extensive attention because of its advantages of low smelting temperature, high impurity removal efficiency and the like. However, the primary silicon in the solid Al-Si alloy is dispersed and distributed, the recovery of the silicon is difficult, and the recovery efficiency is not high. How to separate and improve the recovery efficiency of primary silicon is an urgent problem to be solved by an alloy solidification refining method. At present, technologies such as an induction heating fixed alternating magnetic field, a rotating magnetic field, supergravity and the like are adopted to separate silicon from Al-Si alloy, and the enrichment of silicon can be beneficial to subsequent recovery and can also reduce the acid consumption. These techniques have been successful on a laboratory scale, but continuous quantitative production is difficult to achieve.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for separating primary silicon from hypereutectic aluminum-silicon alloy, which solves the problems of difficult separation and low separation efficiency of the primary silicon from a melt in the process of alloy solidification and refining.
The method adopts a zone melting process to separate Al and Si; because Al and Si are infinitely mutually soluble in a liquid phase and the solubility of Al in solid Si is almost zero, the separation of primary silicon and aluminum can be realized by zone melting theoretically; when the melt temperature reaches the eutectic temperature, the aluminum-silicon alloy of the hypereutectic composition can be separated into primary silicon and eutectic silicon melt; therefore, the separation of silicon from the eutectic melt can be realized by controlling the technological parameters of zone melting, thereby realizing the purpose of improving the recovery rate of primary silicon; in addition, the smelting process of the induction heating area has the advantages of simple process, low equipment requirement, capability of enlarging or prolonging the diameter and the length of a sample according to actual conditions and the like, and is easy to realize large-scale quantitative production.
The method is realized by smelting in the induction heating area, realizes the high-efficiency enrichment of the primary silicon by controlling the conditions of zone-melting speed, smelting times and the like, and has the advantages of simple process, low equipment requirement, sample prolongability and the like, and is easy to realize large-scale quantitative production and the like.
The method for separating primary silicon from hypereutectic aluminum-silicon alloy comprises the following steps:
(1) melting industrial aluminum and industrial silicon into an aluminum-silicon alloy solution in an induction furnace, wherein the mass percentage of silicon in the aluminum-silicon alloy solution is 30-80%, and casting the aluminum-silicon alloy solution into a cylindrical ingot;
(2) placing the cylindrical cast ingot in a graphite crucible, and smelting in an induction heating area; the smelting vacuum degree of the induction heating area is less than 10Pa, the zone smelting temperature is controlled to be 800-1350 ℃, and the zone smelting speed is controlled to be 1-10 mm/min;
(3) after zone melting is finished, intercepting a primary silicon enriched part from the bottom of a sample, removing an aluminum matrix between silicon crystals by using 3-6mol/L HCl, and recovering primary silicon; washing the primary silicon with deionized water until the solution is neutral, drying, grinding until the particle size is less than 50 μm, and washing with a mixed solution of concentrated hydrochloric acid and concentrated nitric acid for 6-12 h; and (3) washing the silicon powder by using deionized water until the solution is neutral, filtering, collecting and drying to obtain the high-purity silicon powder.
The diameter of the cylindrical ingot is 10-100 mm.
The volume ratio of the concentrated hydrochloric acid to the concentrated nitric acid in the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid is 3: 1.
The smelting of the induction heating area in the step (2) can be repeated more than once.
The invention has the beneficial effects that:
(1) the invention adopts the zone melting process, thus improving the separation efficiency of the primary silicon in the aluminum-silicon alloy melt;
(2) the induction heating area smelting provided by the invention has the advantages of simple process, low equipment requirement, sample prolongability and the like, and is easy to realize large-scale quantitative production.
Drawings
FIG. 1 is a longitudinal sectional view of an aluminum-silicon alloy ingot prepared in example 1;
FIG. 2 is a longitudinal section profile of a zone-melted Al-Si alloy solidification sample in example 1;
FIG. 3 is a longitudinal section profile of a zone-melted Al-Si alloy solidified sample in example 2;
FIG. 4 is a longitudinal section profile of a zone-melted Al-Si alloy solidified sample in example 3.
Detailed Description
The invention will be described in more detail with reference to the following figures and examples, but the scope of the invention is not limited thereto. Any changes or substitutions that can be easily made by those skilled in the art within the technical scope of the present disclosure are intended to be covered by the scope of the present disclosure.
Example 1: the separation method of primary silicon in hypereutectic aluminum-silicon alloy comprises the following steps:
(1) weighing industrial silicon (purity 95%) and pure aluminum (purity 99%) according to Al-45wt% Si alloy components, smelting by using an induction heating smelting furnace, casting into a rod-shaped ingot with the diameter of 10mm after smelting, wherein the longitudinal section appearance of the rod-shaped ingot is shown in figure 1;
(2) placing the rod-shaped cast ingot in a graphite crucible, and smelting in an induction heating area; the smelting vacuum degree of the induction heating area is less than 10Pa, the zone melting temperature is controlled to be 1050 +/-50 ℃, and the zone melting speed is 3 mm/min;
(3) after the experiment is finished, turning off the power supply and the servo motor, waiting for 10min, and waiting for the temperature of the crucible to be reduced; opening the zone melting induction furnace to take out an alloy sample; cutting along the longitudinal section of the sample by using a wire cutting machine, grinding, polishing, and shooting the appearance of the longitudinal section of the sample by using a digital camera, wherein the appearance is shown in FIG. 2; as can be seen from the figure, the primary silicon is enriched at the bottom of the sample, and the difference with the longitudinal section morphology figure 1 of the ingot sample in the step (1) is obvious; intercepting a primary silicon enrichment part from the bottom of a sample, dissolving aluminum included in silicon crystals by using 6mol/L HCl, recovering primary silicon, washing the primary silicon by using deionized water until the solution is neutral, and filtering and drying the solution; grinding the primary silicon to particles with the particle size of less than 50 mu m, and washing the particles for 6 hours by aqua regia solution of concentrated hydrochloric acid (HCl) and concentrated nitric acid (the volume ratio is 3: 1); and finally, cleaning the silicon powder by using deionized water until the solution is neutral, filtering, collecting the silicon powder, and drying to obtain the high-purity silicon powder. The content of main impurities of the silicon powder is detected by adopting an inductively coupled plasma atomic emission spectrometer (ICP-OES) as shown in table 1, and the removal effect is obvious as shown in table 1;
TABLE.1: main impurity content of metallurgical silicon and purified silicon
Example 2: the separation method of primary silicon crystals in hypereutectic aluminum-silicon alloy comprises the following steps:
(1) weighing industrial silicon (with the purity of 95%) and pure aluminum (with the purity of 99%) according to Al-45wt% of Si alloy components, smelting by using an induction heating smelting furnace, and casting into a rod-shaped ingot with the diameter of 10mm after smelting;
(2) placing the rod-shaped ingot in a graphite crucible, and carrying out induction heating area smelting, wherein the smelting vacuum degree in the induction heating area is less than 10Pa, the zone-melting temperature is controlled at 1050 +/-50 ℃, and the zone-melting speed is 3 mm/min;
(3) after the first zone melting is finished, repeating the step (2) for 2 times, wherein the melting vacuum degree of the induction heating zone is less than 10Pa, the zone melting temperature is controlled to be 1050 +/-50 ℃, and the zone melting speed is 3 mm/min;
(4) after the experiment is finished, turning off the power supply and the servo motor, waiting for 10min, and waiting for the temperature of the crucible to be reduced; and opening the zone melting induction furnace to take out an alloy sample. The longitudinal section of the sample is cut along the longitudinal section of the sample by a wire cutting machine, ground and polished, and then the longitudinal section appearance of the sample is shot by a digital camera as shown in figure 3, and the following can be seen in the figure: compared with the primary zone melting figure 2, the enrichment degree of the primary silicon at the bottom of the sample is improved; intercepting a primary silicon enrichment part from the bottom of the sample, dissolving aluminum included in silicon crystals by using 6mol/L HCl, and recovering primary silicon; washing the primary silicon with deionized water until the solution is neutral, filtering and drying, grinding the primary silicon into particles with the particle size of less than 50 mu m, and washing for 10 hours with aqua regia solution of concentrated hydrochloric acid (HCl) and concentrated nitric acid (volume ratio is 3: 1); and finally, washing the silicon powder by deionized water until the solution is neutral, filtering, collecting and drying to obtain high-purity silicon powder, wherein the removal effect is obvious.
Example 3: the method for separating primary silicon from hypereutectic aluminum-silicon alloy comprises the following specific steps:
(1) weighing industrial silicon (with the purity of 95%) and pure aluminum (with the purity of 99%) according to Al-65wt% of Si alloy components, smelting by using an induction heating smelting furnace, and casting into a 10mm rod-shaped ingot after smelting;
(2) placing the rod-shaped cast ingot in a graphite crucible, and smelting in an induction heating area; the smelting vacuum degree of the induction heating area is less than 10Pa, the zone-melting temperature is controlled at 1200 +/-50 ℃, and the zone-melting speed is 5 mm/min;
(3) after the experiment is finished, turning off the power supply and the servo motor, waiting for 10min, and waiting for the temperature of the crucible to be reduced; and opening the zone melting induction furnace to take out an alloy sample. Cutting the sample along the longitudinal section by using a wire cutting machine, grinding, polishing, and shooting the longitudinal section of the sample by using a digital camera as shown in figure 4; intercepting a primary silicon enrichment part from the bottom of a sample, dissolving aluminum included among silicon crystals by using 4mol/L HCl, recovering flaky primary silicon, washing the primary silicon by using deionized water until the solution is neutral, filtering and drying, grinding the primary silicon into particles with the particle size of less than 50 mu m, and washing for 12 hours by using aqua regia solution of concentrated hydrochloric acid (HCl) and concentrated nitric acid (the volume ratio is 3: 1); and finally, washing the silicon powder by using deionized water until the solution is neutral, filtering, collecting and drying to obtain high-purity silicon powder, wherein the removal effect is obvious.
Claims (5)
1. A method for separating primary silicon from hypereutectic aluminum-silicon alloy is characterized in that: an induction heating area smelting process is adopted to melt and solidify the aluminum-silicon alloy, so that the enrichment of primary silicon at the bottom of a sample is realized, and the purpose of high-efficiency separation is achieved.
2. The method for separating primary silicon from hypereutectic aluminum-silicon alloy according to claim 1, comprising the steps of:
(1) melting industrial aluminum and industrial silicon into an aluminum-silicon alloy solution in an induction furnace, wherein the mass percentage of silicon in the aluminum-silicon alloy solution is 30-80%, and casting the aluminum-silicon alloy solution into a cylindrical ingot;
(2) placing the cylindrical cast ingot in a graphite crucible, and smelting in an induction heating area; the smelting vacuum degree of the induction heating area is less than 10Pa, the zone smelting temperature is controlled to be 800-1350 ℃, and the zone smelting speed is controlled to be 1-10 mm/min;
(3) after zone melting is finished, intercepting a primary silicon enriched part from the bottom of a sample, removing an aluminum matrix between silicon crystals by using 3-6mol/L HCl, and recovering primary silicon; washing the primary silicon with deionized water until the solution is neutral, drying, grinding until the particle size is less than 50 μm, and washing with a mixed solution of concentrated hydrochloric acid and concentrated nitric acid for 6-12 h; and (3) washing the silicon powder by using deionized water until the solution is neutral, filtering, collecting and drying to obtain the high-purity silicon powder.
3. The method according to claim 1, characterized in that the separation of primary silicon in the hypereutectic aluminum-silicon alloy is performed by: the diameter of the cylindrical ingot is 10-100 mm.
4. The method according to claim 1, characterized in that the separation of primary silicon in the hypereutectic aluminum-silicon alloy is performed by: the volume ratio of the concentrated hydrochloric acid to the concentrated nitric acid in the mixed solution of the concentrated hydrochloric acid and the concentrated nitric acid is 3: 1.
5. The method according to claim 1, characterized in that the separation of primary silicon in the hypereutectic aluminum-silicon alloy is performed by: and (3) repeating the smelting of the induction heating area in the step (2) more than once.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112054186A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Preparation method and application of Al-MOF negative electrode material synthesized by solvothermal method |
| CN112054187A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Plate brick type Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
| CN112054178A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Porous silicon @ silicon oxide @ Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
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2019
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| CN112054187A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Plate brick type Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
| CN112054178A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Porous silicon @ silicon oxide @ Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
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