CN114644339A - Method for removing impurities in silicon by adopting inorganic zinc salt - Google Patents
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- CN114644339A CN114644339A CN202210463853.3A CN202210463853A CN114644339A CN 114644339 A CN114644339 A CN 114644339A CN 202210463853 A CN202210463853 A CN 202210463853A CN 114644339 A CN114644339 A CN 114644339A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
Abstract
The invention discloses a method for removing impurities in silicon by adopting inorganic zinc salt, which relates to the technical field of silicon purification and comprises the steps of heating, refining and impurity removal. The invention utilizes the characteristics of high melting point, high boiling point and high density of zinc oxide, inorganic zinc salt is added into silicon melt and decomposed into gas and zinc oxide, the zinc oxide reacts with impurities in the silicon melt to form a compound, the compound with low melting point overflows from the silicon melt, and then the compound with high melting point is condensed to remove impurities. The method of the invention does not need extra heating, and can realize the removal of partial impurity compounds by utilizing the high temperature of the silicon melt; the invention only adds zinc oxide, and does not introduce new impurities; the gas generated by decomposing the inorganic zinc salt can stir the silicon melt, so that the reaction is more complete, and the impurity removal effect is obvious.
Description
Technical Field
The invention relates to the technical field of silicon purification, in particular to a method for removing impurities in silicon by adopting inorganic zinc salt.
Background
The metallurgical method is a method for gradually removing impurities and purifying cheap industrial silicon until solar-grade silicon is obtained, namely, on the basis of not changing the chemical properties of silicon, the impurities in the silicon are removed by adopting a certain method through the difference of the physical characteristics (steam pressure, solubility, oxidation-reduction potential, phase change characteristic and the like) of the base silicon, the impurities and the compounds thereof, so that the effects of separation and purification are achieved. The basic purification method adopted in the existing metallurgical method is as follows: wet pickling, oxidation slagging, electron beam refining, directional solidification and the like. The impurities in the silicon mainly refer to non-metallic impurities such as B, P and the like and metallic impurities such as Fe, Al, Ti and the like, most of the metallic impurities have large difference of equilibrium solubility in a silicon solid/liquid phase, so the segregation coefficient is very low, the impurities can segregate at a crystal boundary or a defect position in the solidification process of metallurgical silicon, although the impurities can be pretreated through an acid washing process, the removal rate of the metals is difficult to achieve an ideal effect due to the influence of the impurity phase in the silicon, and multi-step and long-period combined leaching of several sections or even longer procedures is generally carried out.
Chinese patent publication No. CN111762786A discloses a method for removing impurity elements by controlled solidification of silicon melt, which comprises continuously adding silicon melt into a directional solidification fixed casting device at a constant speed, controlling the temperature, flow rate and solidification speed of the silicon melt to realize segregation and enrichment of impurity elements, obtaining silicon ingot products with gradient distribution of impurity element content, sampling and detecting the silicon ingot products, determining the nodes of the gradient distribution of impurity element content, and performing classification processing on the silicon ingot to obtain industrial silicon products of various grades with different total mass contents of impurity elements, wherein the impurity elements include one or more of Al, Ca, Mn, Ti, Mg, P, B, S, V, Cr, Ni, Cu, Zn and Zr. Although the invention is combined with the existing industrial silicon smelting and the process of the external refining and purification of the silicon melt, the silicon melt is directly and efficiently purified, the synchronous and efficient removal of the impurity elements in the silicon melt is realized, and the grade of the silicon product can be improved by 2-3 grades after refining and purification. However, the main principle is to remove impurities by segregation and enrichment of impurity elements, and the temperature, flow rate and solidification speed of the silicon melt need to be controlled, so that a large amount of heat energy needs to be consumed, the cost is high, and the method is not environment-friendly.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for removing impurities in silicon by adopting inorganic zinc salt, which has low cost, simple operation and environmental friendliness.
The purpose of the invention is realized by the following technical scheme: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, and adding inorganic zinc salt into the industrial silicon melt in the ladle, wherein the inorganic zinc salt can be decomposed to generate zinc oxide by heating;
s3, impurity removal: and after the silicon melt is cooled and solidified, removing the silicon melt by acid washing after crushing or cutting off a deposition layer at the bottom of the silicon ingot.
Further, the inorganic zinc salt is one or more of zinc carbonate, zinc silicate, zinc sulfate, zinc nitrate, zinc oxalate or zinc hydroxide.
Further, the addition amount of the inorganic zinc salt is 0.5 to 1 percent of the mass of the industrial silicon calculated by the equivalent of the zinc oxide.
Furthermore, the aeration pressure of the argon is 0.2MPa to 0.3MPa, the gas flow is 800L/h to 1200L/h, and the aeration time is 20min to 60 min.
Further, adding inorganic zinc salt and reacting for 50-80 min.
Further, the inorganic zinc salt is added with compressed gas or directly added.
Further, the acid in step S3 is hydrochloric acid, sulfuric acid, or nitric acid.
The principle of the invention is as follows:
the invention adopts inorganic zinc salt as impurity removing medium for industrial silicon refining outside the furnace, and the types of the inorganic zinc salt comprise zinc carbonate, zinc silicate, zinc sulfate, zinc nitrate, zinc oxalate, zinc hydroxide and other zinc salts which can be decomposed to generate zinc oxide. The products decomposed by the inorganic zinc salt in the heating process all contain zinc oxide, the melting point is 1975 ℃, the boiling point is 2360 ℃ and the density is 5.606 g/cm, the zinc oxide is high in melting point, boiling point and density, the zinc oxide can not melt or decompose in silicon melt and can exist in a solid mode, the zinc oxide can be finally deposited at the bottom of the silicon melt, the solubility of silicon in zinc is low, the solubility of zinc in silicon is low, the zinc and silicon are basically incompatible at normal temperature, gas generated by heating decomposition of the inorganic zinc salt can generate gas stirring effect on the silicon melt, impurities can generate chemical reaction at a solid-liquid interface of zinc oxide and melt silicon to generate compounds in the process of contacting the decomposed zinc oxide with the silicon melt, and the low-melting-point compounds can volatilize and escape from the industrial silicon melt at the temperature of 1700 ℃ of the external refining of the industrial silicon furnace, thereby achieving the purpose of removing, and the high melting point compound is segregated and is positioned at the grain boundary after the silicon is solidified, can be removed by acid cleaning after being crushed, or is coated on the surface of the zinc oxide and sinks to the bottommost part of the silicon melt. After the silicon melt is solidified, the deposited zinc oxide layer at the bottom of the silicon ingot is removed by cutting.
The invention has the following advantages:
the invention utilizes the characteristics of high melting point, high boiling point and high density of zinc oxide, inorganic zinc salt is added into silicon melt to be decomposed into gas and zinc oxide, the zinc oxide reacts with impurities in the silicon melt to form a compound, the compound with low melting point overflows from the silicon melt, and then the compound with high melting point is condensed to remove impurities. The method of the invention does not need extra heating, and can realize the removal of partial impurity compounds by utilizing the high temperature of the silicon melt; the invention only adds zinc oxide, and does not introduce new impurities; the gas generated by the decomposition of the inorganic zinc salt can stir the silicon melt, so that the reaction is more sufficient and the impurity removal effect is obvious.
Detailed Description
The invention is further described below with reference to examples, without limiting the scope of the invention to the following:
example 1: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.2MPaMPa, the gas flow is 800L/hL/h, and the aeration time is 20 min; adding zinc carbonate into the industrial silicon melt in the two-man ladle, adding the zinc carbonate along with the compressed gas, and reacting for 50 min; wherein the addition amount of the inorganic zinc salt is 0.5 percent of the mass of the industrial silicon calculated by the equivalent of the zinc oxide;
s3, impurity removal: and removing the silicon melt by adopting a hydrochloric acid washing method after crushing after cooling and solidifying.
Example 2: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.3MPa, the gas flow is 1200L/h, and the aeration time is 60 min; directly adding inorganic zinc salt into the industrial silicon melt in the two-man ladle, adding the inorganic zinc salt along with compressed gas, and reacting for 60 min; wherein the addition amount of the inorganic zinc salt is 0.6 percent of the mass of the industrial silicon calculated by the equivalent of zinc oxide, and the inorganic zinc salt is a mixture of zinc silicate and zinc sulfate;
s3, impurity removal: and after the silicon melt is cooled and solidified, removing the silicon melt by a nitric acid washing method after crushing.
Example 3: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 900L/h, and the aeration time is 30 min; adding inorganic zinc salt into the industrial silicon melt in the two-man ladle, adding the inorganic zinc salt along with compressed gas, and reacting for 55 min; wherein the addition amount of the inorganic zinc salt is 0.7 percent of the mass of the industrial silicon calculated by the equivalent of zinc oxide, and the inorganic zinc salt is a mixture of zinc oxalate, zinc hydroxide and zinc oxalate;
s3, impurity removal: and removing the silicon melt by adopting a sulfuric acid washing method after crushing after cooling and solidifying.
Example 4: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.3MPa, the gas flow is 1000L/h, and the aeration time is 40 min; directly adding inorganic zinc salt into the industrial silicon melt in the two-man ladle, and reacting for 65 min; wherein the addition amount of the inorganic zinc salt is 0.8 percent of the mass of the industrial silicon calculated by the equivalent of zinc oxide, and the inorganic zinc salt is a mixture of zinc carbonate, zinc silicate, zinc sulfate, zinc nitrate and zinc hydroxide;
s3, impurity removal: and after the silicon melt is cooled and solidified, removing the part enriched with zinc oxide at the bottom of the solid silicon by adopting a method of cutting.
Example 5: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.2MPa, the gas flow is 1100L/h, and the aeration time is 50 min; adding inorganic zinc salt into the industrial silicon melt in the two-man ladle, adding the inorganic zinc salt along with compressed gas, and reacting for 60 min; wherein the addition amount of the inorganic zinc salt is 1 percent of the mass of the industrial silicon calculated by the equivalent of zinc oxide, and the inorganic zinc salt is a mixture of zinc carbonate, zinc sulfate, zinc nitrate and zinc oxalate;
s3, impurity removal: and removing the silicon melt by adopting a sulfuric acid washing method after crushing after cooling and solidifying.
Example 6: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 800L/h, and the aeration time is 25 min; adding inorganic zinc salt into the industrial silicon melt in the two-man ladle, adding the inorganic zinc salt along with the compressed gas, and reacting for 80 min; the addition amount of the inorganic zinc salt is 0.9 percent of the mass of the industrial silicon calculated by the equivalent of zinc oxide, and the inorganic zinc salt is a mixture of zinc carbonate, zinc silicate, zinc sulfate, zinc nitrate, zinc oxalate and zinc hydroxide;
s3, impurity removal: and after the silicon melt is cooled and solidified, removing the part enriched with zinc oxide at the bottom of the solid silicon by adopting a method of cutting.
Example 1: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to 1700 ℃ to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 1000L/h, and the aeration time is 20 min; adding zinc carbonate into the industrial silicon melt in the two-man ladle, quickly adding the zinc carbonate along with the compressed gas, and reacting for 50 min; the addition amount of the inorganic zinc salt is 0.5 percent of the mass of the industrial silicon calculated by the equivalent of the zinc oxide;
s3, impurity removal: and removing the silicon melt by adopting a hydrochloric acid washing method after crushing after the silicon melt is cooled and solidified.
The impurity contents of iron, aluminum, calcium, boron and phosphorus in the silicon melt before impurity removal are respectively 330ppm, 220ppm, 100ppm, 25ppm and 35 ppm; the contents of impurities such as iron, aluminum and calcium after impurity removal are 140ppm, 85ppm, 45ppm, 20ppm and 25 ppm.
Example 2: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to 1700 ℃ to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 1000L/h, and the aeration time is 20 min; adding zinc carbonate into the industrial silicon melt in the two-man ladle, quickly adding the zinc carbonate along with the compressed gas, and reacting for 50 min; the addition amount of the inorganic zinc salt is 0.8 percent of the mass of the industrial silicon calculated by the equivalent of the zinc oxide;
s3, removing impurities: and removing the silicon melt by adopting a hydrochloric acid washing method after crushing after cooling and solidifying.
The impurity contents of iron, aluminum, calcium, boron and phosphorus in the silicon melt before impurity removal are respectively 330ppm, 220ppm, 100ppm, 25ppm and 35 ppm; the contents of impurities such as iron, aluminum and calcium after impurity removal are 110ppm, 65ppm, 35ppm, 16ppm and 20 ppm.
Example 3: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to 1700 ℃ to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 1000L/h, and the aeration time is 20 min; adding zinc carbonate into the industrial silicon melt in the two-man ladle, slowly and uniformly adding the zinc carbonate along with the compressed gas, and reacting for 60 min; the addition amount of the inorganic zinc salt is 0.8 percent of the mass of the industrial silicon calculated by the equivalent of the zinc oxide;
s3, impurity removal: and removing the silicon melt by adopting a hydrochloric acid washing method after crushing after cooling and solidifying.
The impurity contents of iron, aluminum, calcium, boron and phosphorus in the silicon melt before impurity removal are respectively 330ppm, 220ppm, 100ppm, 25ppm and 35 ppm; the contents of impurities such as iron, aluminum and calcium after impurity removal are 100ppm, 55ppm, 30ppm, 13ppm and 16 ppm.
Example 4: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to 1700 ℃ to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 1000L/h, and the aeration time is 20 min; adding zinc carbonate into the industrial silicon melt in the two-man ladle, slowly and uniformly adding the zinc carbonate along with the compressed gas, and reacting for 80 min; the addition amount of the inorganic zinc salt is 0.8 percent of the mass of the industrial silicon calculated by the equivalent of the zinc oxide;
s3, impurity removal: and removing the silicon melt by adopting a hydrochloric acid washing method after crushing after cooling and solidifying.
The impurity contents of iron, aluminum, calcium, boron and phosphorus in the silicon melt before impurity removal are 330ppm, 220ppm, 100ppm, 25ppm and 35ppm respectively; the contents of impurities such as iron, aluminum and calcium after impurity removal are 95ppm, 50ppm, 25ppm, 10ppm and 12 ppm.
Example 5: a method for removing impurities in silicon by adopting inorganic zinc salt comprises the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to 1700 ℃ to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 1000L/h, and the aeration time is 30 min; adding zinc carbonate into the industrial silicon melt in the two-man ladle, slowly and uniformly adding the zinc carbonate along with the compressed gas, and reacting for 80 min; the addition amount of the inorganic zinc salt is 1.0 percent of the mass of the industrial silicon calculated by the equivalent of the zinc oxide;
s3, impurity removal: and removing the silicon melt by adopting a hydrochloric acid washing method after crushing after cooling and solidifying.
The impurity contents of iron, aluminum, calcium, boron and phosphorus in the silicon melt before impurity removal are respectively 330ppm, 220ppm, 100ppm, 25ppm and 35 ppm; the contents of impurities such as iron, aluminum and calcium after impurity removal are 85ppm, 45ppm, 20ppm, 5ppm and 7 ppm.
Comparative example: a method for removing impurities from silicon, comprising the steps of:
s1, heating: adding industrial silicon into a two-man ladle, and heating to 1700 ℃ to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, wherein the aeration pressure is 0.25MPa, the gas flow is 1000L/h, the aeration time is 20min, and standing for 50 min;
s3, impurity removal: and removing the silicon melt by adopting a hydrochloric acid washing method after crushing after cooling and solidifying.
The impurity contents of iron, aluminum, calcium, boron and phosphorus in the silicon melt before impurity removal are respectively 330ppm, 220ppm, 100ppm, 25ppm and 35 ppm; the contents of impurities such as iron, aluminum and calcium after impurity removal are 325ppm, 180ppm, 65ppm, 25ppm and 35 ppm.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept within the technical scope of the present invention.
Claims (7)
1. A method for removing impurities in silicon by adopting inorganic zinc salt is characterized by comprising the following steps:
s1, heating: adding industrial silicon into a two-man ladle, and heating to obtain silicon melt;
s2, refining: introducing compressed gas argon into the silicon melt, and adding inorganic zinc salt into the industrial silicon melt in the ladle, wherein the inorganic zinc salt can be decomposed to generate zinc oxide by heating;
s3, impurity removal: and after the silicon melt is cooled and solidified, removing the silicon melt by acid washing after crushing or cutting off a deposition layer at the bottom of the silicon ingot.
2. The method for removing impurities in silicon by using inorganic zinc salt according to claim 1, wherein the inorganic zinc salt is one or more of zinc carbonate, zinc silicate, zinc sulfate, zinc nitrate, zinc oxalate or zinc hydroxide.
3. The method for removing impurities in silicon by using inorganic zinc salt according to claim 1, wherein the inorganic zinc salt is added in an amount of 0.5-1% by mass of industrial silicon calculated as an equivalent of zinc oxide.
4. The method for removing impurities in silicon by using inorganic zinc salt according to claim 1, wherein the aeration pressure of the argon gas is 0.2MPa to 0.3MPa, the gas flow is 800L/h to 1200L/h, and the aeration time is 20min to 60 min.
5. The method for removing impurities in silicon by using inorganic zinc salt according to claim 1, wherein the reaction is carried out for 50min to 80min after the inorganic zinc salt is added.
6. The method for removing impurities from silicon using inorganic zinc salts according to claim 1, wherein the inorganic zinc salt is added with the compressed gas or directly.
7. The method for removing impurities from silicon using inorganic zinc salt according to claim 1, wherein the acid in step S3 is hydrochloric acid, sulfuric acid or nitric acid.
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