CN109734099B - Impurity removal method for silicon material - Google Patents
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- CN109734099B CN109734099B CN201910191402.7A CN201910191402A CN109734099B CN 109734099 B CN109734099 B CN 109734099B CN 201910191402 A CN201910191402 A CN 201910191402A CN 109734099 B CN109734099 B CN 109734099B
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Abstract
The invention provides an impurity removal method of a silicon material, which comprises the following steps: taking a silicon material to be subjected to impurity removal, and mixing the silicon material to be subjected to impurity removal and a grinding material to obtain a mixture; stirring the mixture, adding water into the mixture in the stirring process, and separating impurities in the silicon material to be subjected to impurity removal from the silicon material by the grinding material in the stirring process; and cleaning and sorting the stirred mixture to obtain the silicon material after impurity removal. The silicon material to be purified and the grinding material are mixed and stirred. Therefore, the abrasive can continuously rub the silicon material to be subjected to impurity removal in the stirring process, impurities on the surface of the silicon material to be subjected to impurity removal can be separated from the surface of the silicon material to be subjected to impurity removal by the abrasive, and the impurities are removed when the silicon material is finally cleaned and sorted, so that the silicon material subjected to impurity removal is obtained. The impurity removal method provided by the invention can effectively remove impurities in the silicon material, and is simple and low in cost.
Description
Technical Field
The invention belongs to the technical field of silicon material production, and particularly relates to a method for removing impurities from a silicon material.
Background
Hard impurities such as silicon carbide and silicon nitride are inevitably generated in the production process of the silicon material. And the impurities can seriously affect the subsequent processing technology of the silicon material. For example, in the cutting process of silicon ingots, silicon wafers are scrapped due to the existence of impurities caused by line marks, even the silicon wafers are damaged due to line breakage and shutdown, silicon blocks are scrapped, and the like. Therefore, how to reduce and remove the hard impurities in the silicon material becomes one of the key points in the field of silicon material production.
At present, silicon materials to be subjected to impurity removal with high impurity content are generally treated by the steps of grinding, acid cleaning, sorting, grinding and acid cleaning. However, the above-mentioned treatment process is time-consuming and labor-consuming, and the effect of removing impurities is not ideal, and the treated silicon material can only be treated as waste silicon material at a very low price.
Disclosure of Invention
In view of the above, the invention provides an impurity removal method for a silicon material, which comprises mixing and stirring a silicon material to be subjected to impurity removal and a grinding material. Therefore, the abrasive can continuously rub the silicon material to be subjected to impurity removal in the stirring process, impurities on the surface of the silicon material to be subjected to impurity removal can be separated from the surface of the silicon material to be subjected to impurity removal by the abrasive, and the impurities are removed when the silicon material is finally cleaned and sorted, so that the silicon material subjected to impurity removal is obtained. The impurity removing method provided by the invention can effectively remove impurities in the silicon material, and has the advantages of simple method, low cost and strong practicability.
The invention provides a method for removing impurities from a silicon material, which comprises the following steps:
taking a silicon material to be subjected to impurity removal, and mixing the silicon material to be subjected to impurity removal and a grinding material to obtain a mixture;
stirring the mixture, and adding water into the mixture in the stirring process, wherein the grinding material can separate impurities in the silicon material to be subjected to impurity removal from the silicon material in the stirring process;
and cleaning and sorting the stirred mixture to obtain the silicon material after impurity removal.
Wherein the mass ratio of the grinding material to the silicon material to be subjected to impurity removal is (0.1-0.5): 1.
wherein the particle size of the grinding material is 50-150 meshes.
Wherein the abrasive comprises one or both of a first abrasive and a second abrasive.
Wherein the particle size of the first grinding material is 50-100 meshes, and the particle size of the second grinding material is 100-150 meshes.
Wherein the grinding material comprises the first grinding material and the second grinding material, and the mass ratio of the first grinding material to the second grinding material is (3-5): 1.
wherein, the material of the abrasive comprises one or two of aluminum oxide and silicon carbide.
Wherein the stirring time is 10-60 min.
The impurity removal method of the silicon material further comprises the following steps:
cleaning and sorting the stirred mixture to obtain part of silicon materials without impurities;
taking the silicon material to be subjected to impurity removal, and mixing the silicon material without impurity removal, the silicon material to be subjected to impurity removal and the grinding material to obtain a mixture;
stirring the mixture, and adding water into the mixture during the stirring, wherein the grinding material removes impurities in the silicon material to be subjected to impurity removal during the stirring;
and cleaning and sorting the stirred mixture to obtain the silicon material after impurity removal.
Wherein the mass of the silicon material without impurity removal accounts for 1-35% of the mass of the silicon material to be subjected to impurity removal.
According to the impurity removal method for the silicon material, the silicon material to be subjected to impurity removal and the grinding material are mixed and stirred. Therefore, the abrasive can continuously rub the silicon material to be subjected to impurity removal in the stirring process, impurities on the surface of the silicon material to be subjected to impurity removal can be separated from the surface of the silicon material to be subjected to impurity removal by the abrasive, and the impurities are removed when the silicon material is finally cleaned and sorted, so that the silicon material subjected to impurity removal is obtained. In addition, water is added in the stirring process, and the grinding material can be uniformly dispersed in the silicon material to be subjected to impurity removal under the action of the water, so that the impurity removal effect and the impurity removal quality are further improved. The impurity removing method provided by the invention can effectively remove impurities in the silicon material, and has the advantages of simple method, low cost and strong practicability.
Drawings
In order to more clearly illustrate the technical solution in the embodiment of the present invention, the drawings required to be used in the embodiment of the present invention will be described below.
FIG. 1 is a process flow diagram of a method for removing impurities from a silicon material according to an embodiment of the present invention.
Detailed Description
The following is a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements are also considered to be within the scope of the present invention.
Hard impurities such as silicon carbide and silicon nitride are inevitably generated in the production process of the silicon material. Among these, silicon nitride is the main one, because currently, when preparing silicon ingots, a nitrogen-containing coating is formed on the inner surface of the crucible to prevent the silicon ingot from contacting the crucible surface. Therefore, inevitably, the nitrogen element in the nitrogen-containing coating layer enters the silicon liquid and forms silicon nitride with the silicon element when the silicon ingot is prepared. Silicon nitride impurities are formed in the silicon ingot. And the entire silicon ingot includes a high impurity content region and a low impurity content region. The low impurity region may be used without treatment or with only grinding and acid washing. And the silicon material in the high impurity content area can not be used, and even after polishing and acid washing, impurities in the silicon material can not be effectively removed, and the silicon material can only be treated as waste.
According to the impurity removing method of the silicon material provided by the invention, the impurity on the surface of the silicon material to be removed can be separated from the silicon material only by mixing and stirring the silicon material to be removed and the grinding material, so that the impurity removing effect is achieved.
The impurity removing method for the silicon material provided by the embodiment of the invention comprises the steps of S101, S102 and S103. Wherein S101, S102, S103 are described in detail as follows.
S101: and (3) taking the silicon material to be subjected to impurity removal, and mixing the silicon material to be subjected to impurity removal and the grinding material to obtain a mixture.
The ingot is affected by the preparation process and equipment, and the side of the prepared ingot facing away from the bottom of the crucible (head stock) and the side wall of the ingot (side skin) is usually the most contaminated, while the rest belongs to the region of no contamination or low contamination. Therefore, the silicon material to be purified of the invention mainly refers to the head material and the flaw-piece part. Abrasives are primarily particulate materials of relatively high hardness, such as alumina or silicon carbide and the like.
S102: stirring the mixture, and adding water into the mixture in the stirring process, wherein the grinding material can separate impurities in the silicon material to be subjected to impurity removal from the silicon material in the stirring process;
the mixture is stirred, so that the abrasive can be continuously contacted, rubbed, impacted and the like with the silicon material to be subjected to impurity removal in the stirring process, and the abrasive is usually a material with higher hardness and has hardness higher than that of impurities in the silicon material to be subjected to impurity removal, so that the impurities on the surface of the silicon material to be subjected to impurity removal are separated from the surface of the silicon material to be subjected to impurity removal in the stirring process of the abrasive. Thus, the impurities are successfully separated from the silicon material. In addition, water is added in the stirring process, and the grinding material can be uniformly dispersed in the silicon material to be subjected to impurity removal under the action of the water, so that the impurity removal effect and the impurity removal quality are further improved.
S103: and cleaning and sorting the stirred mixture to obtain the silicon material after impurity removal.
The impurities and the silicon materials after impurity removal can be better separated through cleaning, and the impurities can be finally removed through sorting, so that the silicon materials after impurity removal are obtained.
According to the impurity removal method for the silicon material provided by the embodiment of the invention, the silicon material to be subjected to impurity removal and the grinding material are mixed and stirred. Therefore, the abrasive can continuously rub the silicon material to be subjected to impurity removal in the stirring process, impurities on the surface of the silicon material to be subjected to impurity removal can be separated from the surface of the silicon material to be subjected to impurity removal by the abrasive, and the impurities are removed when the silicon material is finally cleaned and sorted, so that the silicon material subjected to impurity removal is obtained. In addition, water is added in the stirring process, and the grinding material can be uniformly dispersed in the silicon material to be subjected to impurity removal under the action of the water, so that the impurity removal effect and the impurity removal quality are further improved. The impurity removing method provided by the invention can effectively remove impurities in the silicon material, and has the advantages of simple method, low cost and strong practicability.
In one embodiment of the invention, the mass ratio of the grinding material to the silicon material to be subjected to impurity removal is (0.1-0.5): 1. the content of the grinding material has great influence on the impurity removal effect. If the amount of the grinding material is too small, the effect of removing impurities is not good. If the grinding material is too much, not only impurities can be removed, but also partial surface silicon material can be removed, so that the content of the silicon material after impurity removal can be greatly reduced. Therefore, the grinding amount and the silicon material to be removed need to have a proper mass ratio. Preferably, the mass ratio of the grinding material to the silicon material to be subjected to impurity removal is (0.2-0.4): 1. more preferably, the mass ratio of the grinding material to the silicon material to be subjected to impurity removal is (0.24-0.35): 1.
in one embodiment of the present invention, the particle size of the abrasive is 50 to 150 mesh. The particle size of the grinding amount in the present invention also affects the effect of removing impurities. If the particle size of the abrasive is too small, the abrasive and the silicon material to be subjected to impurity removal are stirred in the stirring process, the grinding effect is too poor, and therefore, the impurities on the surface of the silicon material to be subjected to impurity removal cannot be effectively removed due to too small friction force and too small impact force. However, if the particle size of the abrasive is too large, the abrasive not only can remove impurities, but also can remove partial surface silicon materials in the stirring process, so that the content of the silicon materials after impurity removal can be greatly reduced. Therefore, the particle size of the abrasive needs to have a suitable size. Preferably, the particle size of the abrasive is 70-130 mesh. More preferably, the particle size of the abrasive is 90-110 mesh.
In one embodiment of the present invention, the abrasive includes one or both of a first abrasive and a second abrasive. The invention can use one abrasive or two abrasives mixed together.
In an embodiment of the present invention, the particle size of the first abrasive is 50-100 mesh, and the particle size of the second abrasive is 100-150 mesh. When the invention adopts two grinding materials to be mixed for use, the grain diameter of the first grinding material is smaller than that of the second grinding material. The first grinding material with small particle size and the second grinding material with large particle size are mixed for use, so that the impurity removal effect can be further improved. Preferably, the particle size of the first abrasive is 60-90 meshes, and the particle size of the second abrasive is 110-140 meshes. More preferably, the particle size of the first abrasive is 70-80 mesh, and the particle size of the second abrasive is 120-130 mesh.
In an embodiment of the present invention, the abrasives include the first abrasives and the second abrasives, and a mass ratio of the first abrasives to the second abrasives is (3-5): 1. when the two grinding materials are mixed for use, the mass ratio of the first grinding material with small particle size to the second grinding material with large particle size is (3-5): 1. the above description has said that the first abrasive having a small particle size and the second abrasive having a large particle size can improve the effect of removing impurities. And when the mass of the first grinding material with small particle size is 3-5 times of that of the second grinding material with large particle size, the impurity removal effect can be further improved. Preferably, the abrasive comprises the first abrasive and the second abrasive, and the mass ratio of the first abrasive to the second abrasive is (3-5): 1. more preferably, the abrasive comprises the first abrasive and the second abrasive, and the mass ratio of the first abrasive to the second abrasive is (3-5): 1.
in an embodiment of the present invention, the material of the abrasive includes one or two of aluminum oxide and silicon carbide. The abrasive in the invention can be alumina or silicon carbide, or silicon oxide and silicon carbide.
In one embodiment of the invention, the stirring time is 10-60 min. The longer the stirring time is, more impurities on the surface of the silicon material to be subjected to impurity removal can be removed, so that the impurity removal effect is better. However, the longer the stirring time, the less cost and the price of the silicon material after impurity removal become cost-effective. Therefore, the stirring time of the invention is 10-60 min. Preferably, the stirring time is 20-50 min. More preferably, the stirring time is 30-40 min.
In an embodiment of the present invention, the method for removing impurities from a silicon material further includes steps S104, S105, S106, and S107. Wherein S104, S105, S106, S107 are described in detail as follows.
S104: and cleaning and sorting the stirred mixture to obtain a part of silicon material without impurities.
After the step S103, most of the silicon material to be purified may be subjected to stirring to remove impurities on the surface of the silicon material to be purified, so that the silicon material to be purified becomes the silicon material after the impurity removal, but a part of the silicon material without the impurity removal may be obtained.
S105: and mixing the silicon material to be subjected to impurity removal, the silicon material without impurity removal, the silicon material to be subjected to impurity removal and the grinding material to obtain a mixture.
And mixing the obtained part of the silicon material without impurity removal with another silicon material to be subjected to impurity removal to perform another impurity removal process, so that the performance of equipment can be utilized to the maximum extent. If only equipment is used for processing part of silicon materials without impurity removal, the equipment is greatly wasted, and the impurity removal cost is increased.
S106: stirring the mixture, and adding water into the mixture during the stirring, wherein the grinding material removes impurities in the silicon material to be subjected to impurity removal during the stirring.
The mixture is stirred, so that the abrasive can be continuously contacted, rubbed, impacted and the like with the silicon material to be subjected to impurity removal in the stirring process, and the abrasive is usually a material with higher hardness and higher than the hardness of impurities in the silicon material to be subjected to impurity removal, so that the impurities on the surface of the silicon material to be subjected to impurity removal are separated from the surface of the silicon material to be subjected to impurity removal in the stirring process of the abrasive. Thus, the impurities are successfully separated from the silicon material. In addition, water is added in the stirring process, and the grinding material can be uniformly dispersed in the silicon material to be subjected to impurity removal under the action of the water, so that the impurity removal effect and the impurity removal quality are further improved.
S107: and cleaning and sorting the stirred mixture to obtain the silicon material after impurity removal.
The impurities and the silicon materials after impurity removal can be better separated through cleaning, and the impurities can be finally removed through sorting, so that the silicon materials after impurity removal are obtained.
In one embodiment of the invention, the mass of the silicon material without impurity removal accounts for 1-35% of the mass of the silicon material to be subjected to impurity removal.
According to the impurity removal method provided by the invention, the influence of the impurity removal process of the silicon material without impurity removal, the impurity removal time and the selection of the grinding material is avoided, wherein the mass of the silicon material without impurity removal accounts for 1-35% of the mass of the silicon material to be subjected to impurity removal. The mass of the silicon material after impurity removal accounts for 65-99% of that of the silicon material to be subjected to impurity removal. Preferably, the mass of the silicon material without impurity removal accounts for 5-30% of the mass of the silicon material to be subjected to impurity removal. More preferably, the mass of the silicon material without impurity removal accounts for 10-20% of the mass of the silicon material to be impurity removed.
In the following, the above embodiments will be further explained by being divided into a plurality of embodiments.
Example 1
The invention provides an impurity removal method of a silicon material, which comprises the following steps:
step 1: and separating the silicon ingot into a silicon material with low impurity content and a silicon material with high impurity content, wherein the silicon material with high impurity content is the silicon material to be subjected to impurity removal.
Step 2: the silicon material with low impurity content can be normally used after being sequentially subjected to polishing and acid washing processes.
And step 3: 1500kg of silicon material to be subjected to impurity removal is taken, the silicon material to be subjected to impurity removal is put into a roller stirring device, and the mass ratio of the grinding material to the silicon material to be subjected to impurity removal is 0.3: adding a grinding amount of alumina corundum according to the mass ratio of 1, wherein the grain diameter of the alumina corundum is 50 meshes.
And 4, step 4: continuously adding water into the stirring device in the rolling process of the silicon material to be removed and the alumina corundum, wherein the stirring time is 20 min.
And 5: and cleaning and sorting the stirred mixture to obtain 1125kg of impurity-removed silicon material, and removing 75% of the silicon material to be subjected to impurity removal by a primary impurity removal process of the rest 375kg of silicon material without impurity removal.
Step 6: 1125kg of silicon material to be purified is taken, the rest 375kg of silicon material without impurities is added, and 1500kg of silicon material to be purified is prepared again. Repeating the steps 3 to 5 to finally obtain 1125kg of silicon material after impurity removal.
Example 2
The invention provides an impurity removal method of a silicon material, which comprises the following steps:
step 1: and separating the silicon ingot into a silicon material with low impurity content and a silicon material with high impurity content, wherein the silicon material with high impurity content is the silicon material to be subjected to impurity removal.
Step 2: the silicon material with low impurity content can be normally used after being sequentially subjected to polishing and acid washing processes.
And step 3: 1500kg of silicon material to be subjected to impurity removal is taken, the silicon material to be subjected to impurity removal is put into a roller stirring device, and the mass ratio of the grinding material to the silicon material to be subjected to impurity removal is 0.3: adding a grinding amount of alumina corundum according to the mass ratio of 1, wherein the grain diameter of the alumina corundum is 150 meshes.
And 4, step 4: continuously adding water into the stirring device in the rolling process of the silicon material to be removed and the alumina corundum, wherein the stirring time is 20 min.
And 5: cleaning and sorting the stirred mixture to obtain 975kg of silicon material after impurity removal, and removing 65% of silicon material to be subjected to impurity removal by a one-time impurity removal process from the rest 525kg of silicon material without impurity removal.
Step 6: 975kg of silicon material to be subjected to impurity removal is taken, and the rest 525kg of silicon material without impurity removal is added to prepare 1500kg of silicon material to be subjected to impurity removal again. Repeating the steps 3 to 5, and finally obtaining 975kg of silicon material after impurity removal.
Example 3
The invention provides an impurity removal method of a silicon material, which comprises the following steps:
step 1: and separating the silicon ingot into a silicon material with low impurity content and a silicon material with high impurity content, wherein the silicon material with high impurity content is the silicon material to be subjected to impurity removal.
Step 2: the silicon material with low impurity content can be normally used after being sequentially subjected to polishing and acid washing processes.
And step 3: 1500kg of silicon material to be subjected to impurity removal is taken, the silicon material to be subjected to impurity removal is put into a roller stirring device, and the mass ratio of the grinding material to the silicon material to be subjected to impurity removal is 0.3: adding a grinding amount of alumina corundum according to the mass ratio of 1, wherein the alumina corundum is divided into a first alumina corundum and a second alumina corundum. Wherein the grain diameter of the first alumina corundum is 50 meshes, the grain diameter of the second alumina corundum is 100 meshes, and the mass ratio of the first alumina corundum to the second alumina corundum is 4: 1.
And 4, step 4: continuously adding water into the stirring device in the rolling process of the silicon material to be removed and the alumina corundum, wherein the stirring time is 20 min.
And 5: and cleaning and sorting the stirred mixture to obtain 1275kg of silicon material after impurity removal, and removing 85% of silicon material to be subjected to impurity removal by the residual 225kg of silicon material without impurity removal through a primary impurity removal process.
Step 6: 1275kg of silicon material to be subjected to impurity removal is taken, the rest 225kg of silicon material without impurity removal is added, and 1500kg of silicon material to be subjected to impurity removal is prepared again. Repeating the steps 3 to 5 to finally obtain 1275kg of silicon material after impurity removal.
The foregoing detailed description is provided for the purposes of illustrating the embodiments of the present invention, and is provided for the purposes of illustrating the principles and embodiments of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. An impurity removal method of a silicon material is characterized by comprising the following steps:
taking a silicon material to be subjected to impurity removal, and mixing the silicon material to be subjected to impurity removal and a grinding material to obtain a mixture, wherein the hardness of the grinding material is greater than that of impurities in the silicon material to be subjected to impurity removal;
stirring the mixture, and adding water into the mixture in the stirring process, wherein the grinding material can be uniformly dispersed in the silicon material to be subjected to impurity removal under the action of water, and the grinding material can separate impurities in the silicon material to be subjected to impurity removal from the silicon material in the stirring process;
and cleaning and sorting the stirred mixture to obtain the silicon material after impurity removal.
2. An impurity removal method according to claim 1, wherein the mass ratio of the grinding material to the silicon material to be removed is (0.1-0.5): 1.
3. the impurity removing method according to claim 1, wherein the particle size of the abrasive is 50 to 150 mesh.
4. A method according to claim 3, wherein the abrasive comprises one or both of a first abrasive and a second abrasive.
5. The impurity removing method according to claim 4, wherein the particle size of the first abrasive is 50-100 mesh, and the particle size of the second abrasive is 100-150 mesh.
6. The impurity removing method according to claim 4, wherein the grinding material comprises the first grinding material and the second grinding material, and the mass ratio of the first grinding material to the second grinding material is (3-5): 1.
7. the method of removing impurities according to claim 1, wherein the material of the abrasive comprises one or both of alumina and silicon carbide.
8. An impurity removal method according to claim 1, wherein the stirring time is 10-60 min.
9. An impurity removal method according to claim 1, wherein the impurity removal method of the silicon material further comprises:
cleaning and sorting the stirred mixture to obtain part of silicon materials without impurities;
taking the silicon material to be subjected to impurity removal, and mixing the silicon material without impurity removal, the silicon material to be subjected to impurity removal and the grinding material to obtain a mixture;
stirring the mixture, and adding water into the mixture during the stirring, wherein the grinding material removes impurities in the silicon material to be subjected to impurity removal during the stirring;
and cleaning and sorting the stirred mixture to obtain the silicon material after impurity removal.
10. An impurity removal method according to claim 9, wherein the mass of the silicon material without impurity removal accounts for 1-35% of the mass of the silicon material to be impurity removed.
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| CN101683982B (en) * | 2008-09-22 | 2011-07-27 | 华南师范大学 | Method for refining metal silicon |
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