CN109734099A - A kind of impurity-removing method of silicon material - Google Patents
A kind of impurity-removing method of silicon material Download PDFInfo
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- CN109734099A CN109734099A CN201910191402.7A CN201910191402A CN109734099A CN 109734099 A CN109734099 A CN 109734099A CN 201910191402 A CN201910191402 A CN 201910191402A CN 109734099 A CN109734099 A CN 109734099A
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Abstract
The present invention provides a kind of impurity-removing methods of silicon material, comprising: takes silicon material to be cleaned, silicon material to be cleaned and abrasive are mixed, mixture is obtained；Mixture is stirred, and adds water into mixture during stirring, abrasive can will be separated wait the impurity in the silicon material that cleans with silicon material during stirring；Mixture after stirring is cleaned and sorted, the silicon material after being cleaned.By the way that silicon material to be cleaned is mixed and stirred for abrasive.Therefore, abrasive can constantly rub with silicon material to be cleaned during stirring, and then the impurity on silicon material surface to be cleaned can be detached from by abrasive from silicon material surface to be cleaned, and when finally being cleaned and sorted again, impurity be removed, the silicon material after being cleaned.Impurity-removing method provided by the invention, the impurity that can be effectively removed in silicon material, and method is simple, and it is low in cost.
Description
Technical field
The invention belongs to the production technical fields of silicon material, and in particular to a kind of impurity-removing method of silicon material.
Background technique
The hard impurities such as silicon carbide, silicon nitride are inevitably generated in the production process of silicon material.And these impurity
The subsequent machining technology of silicon material can be seriously affected.Such as the presence in the cutting process of silicon ingot due to impurity causes silicon wafer to occur
Stria and scrap, or even broken string is caused to shut down, silico briquette such as scraps at the loss.Therefore how to reduce, remove hard impurity in silicon material
At one of the emphasis of silicon material production field.
Currently, the silicon material to be cleaned of high impurity content usually passes through polishing-pickling-sorting-polishing-pickling the step of progress
Processing.But above-mentioned treatment process is not only time-consuming and laborious, but also the effect to clean is also unsatisfactory, and silicon material that treated can only be with pole
Low price is when the processing of waste product silicon material.
Summary of the invention
In consideration of it, the present invention provides a kind of impurity-removing method of silicon material, by the way that silicon material to be cleaned is mixed with abrasive
Merge stirring.Therefore, abrasive can constantly rub with silicon material to be cleaned during stirring, and then abrasive can incite somebody to action
The impurity on silicon material surface to be cleaned is detached from from silicon material surface to be cleaned, and when finally being cleaned and sorted again, impurity is removed, is obtained
Silicon material after to removal of impurities.Impurity-removing method provided by the invention, the impurity that can be effectively removed in silicon material, and method is simple, at
This is low, has very strong practicability.
First aspect present invention provides a kind of impurity-removing method of silicon material, comprising:
Silicon material to be cleaned is taken, the silicon material to be cleaned and abrasive are mixed, mixture is obtained；
The mixture is stirred, and adds water into the mixture during stirring, it is described to grind
Abrasive material can separate the impurity wait in the silicon material that cleans with silicon material during the stirring；
The mixture after stirring is cleaned and sorted, the silicon material after being cleaned.
Wherein, the abrasive and the mass ratio of the silicon material to be cleaned are (0.1-0.5): 1.
Wherein, the partial size of the abrasive is 50-150 mesh.
Wherein, the abrasive includes one or both of the first abrasive and the second abrasive.
Wherein, the partial size of first abrasive is 50-100 mesh, and the partial size of second abrasive is 100-150 mesh.
Wherein, the abrasive includes first abrasive and second abrasive, first abrasive and institute
The mass ratio for stating the second abrasive is (3-5): 1.
Wherein, the material of the abrasive includes one or both of aluminium oxide and silicon carbide.
Wherein, the time of the stirring is 10-60min.
Wherein, the impurity-removing method of the silicon material further include:
The mixture after stirring is cleaned and sorted, the silicon material that part does not clean is also obtained；
The silicon material to be cleaned separately is taken, the silicon material not cleaned, the silicon material to be cleaned and the abrasive are mixed,
Obtain mixture；
The mixture is stirred, and adds water into the mixture during stirring, it is described to grind
Abrasive material can remove the impurity wait in the silicon material that cleans during the stirring；
The mixture after stirring is cleaned and sorted, the silicon material after being cleaned.
Wherein, the quality of the silicon material not cleaned accounts for the 1-35% of the quality of the silicon material to be cleaned.
The impurity-removing method for a kind of silicon material that first aspect present invention provides, by mixing with abrasive silicon material to be cleaned
Merge stirring.Therefore, abrasive can constantly rub with silicon material to be cleaned during stirring, and then abrasive can incite somebody to action
The impurity on silicon material surface to be cleaned is detached from from silicon material surface to be cleaned, and when finally being cleaned and sorted again, impurity is removed, is obtained
Silicon material after to removal of impurities.In addition, add water during stirring, abrasive can be evenly dispersed under the action of water to
The inside for the silicon material that cleans, further increases the effect of removal of impurities and the quality of removal of impurities.Impurity-removing method provided by the invention, can be effectively
The impurity in silicon material is removed, and method is simple, it is at low cost, there is very strong practicability.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to required in the embodiment of the present invention
The attached drawing used is illustrated.
Fig. 1 is the process flow chart of the impurity-removing method of silicon material in the embodiment of the present invention.
Specific embodiment
It is the preferred embodiment of the present invention below, it is noted that for those skilled in the art,
Various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as this hair
Bright protection scope.
The hard impurities such as silicon carbide, silicon nitride are inevitably generated in the production process of silicon material.Wherein, mainly
Silicon nitride, because at present when preparing silicon ingot one layer of nitrogenous coating can be formed in inner surface of crucible, to avoid silicon ingot and crucible
The contact on surface.Therefore, inevitably, when preparing silicon ingot, the nitrogen in nitrogenous coating can enter in silicon liquid and and silicon
Element forms silicon nitride.Therefore silicon nitride inclusions be will form in silicon ingot.And entire silicon ingot includes high impurity content area and low miscellaneous
Matter content area.Low impurity content area can not have to processing or only need to polish can be used with pickling.And high impurity content area
Silicon material chance cannot use, and after polishing and pickling, impurity in the silicon material that still can not effectively go out can only be regarded
Waste disposal.
In the impurity-removing method of the silicon material provided according to the present invention, it is only necessary to mix silicon material to be cleaned with abrasive
And stir, the impurity on silicon material surface to be cleaned can be separated with silicon material, to achieve the effect that removal of impurities.
A kind of impurity-removing method of silicon material provided in an embodiment of the present invention includes step S101, S102, S103.Wherein S101,
S102, S103 are described in detail as follows.
S101: taking silicon material to be cleaned, and the silicon material to be cleaned and abrasive are mixed, mixture is obtained.
For silicon ingot due to being influenced by preparation process and equipment, the silicon ingot prepared is generally away from the side of crucible bottom
Side wall (flaw-piece) of (head material) and silicon ingot its impurity content is most, and other parts belong to free from admixture content area or low miscellaneous
Matter content area.Therefore silicon material to be cleaned of the invention generally refers to head material and flaw-piece part.It is higher that abrasive refers mainly to hardness
Granular material, such as aluminium oxide or silicon carbide etc..
S102: the mixture is stirred, and adds water into the mixture during stirring, institute
Stating abrasive can separate the impurity wait in the silicon material that cleans with silicon material during the stirring；
Mixture is stirred, therefore abrasive can constantly be connect with silicon material to be cleaned during stirring
Touching, friction, shock etc., and because abrasive is usually the higher material of hardness, hardness can be than wait impurity in the silicon material that cleans
Hardness want high, so abrasive takes off the impurity on silicon material surface to be cleaned from silicon material surface to be cleaned during stirring
From.It comes in this way, impurity just has successfully been isolated with silicon material.In addition, adding water during stirring, abrasive can be in water
It is homogeneously dispersed in the inside of silicon material to be cleaned under effect, further increases the effect of removal of impurities and the quality of removal of impurities.
S103: being cleaned the mixture after stirring and sorted, the silicon material after being cleaned.
Cleaning can preferably separate the silicon material after impurity and removal of impurities, and sort and can finally remove impurity, obtain
Silicon material after to removal of impurities.
The impurity-removing method of silicon material provided in an embodiment of the present invention, by with abrasive being mixed and being stirred silicon material to be cleaned
It mixes.Therefore, abrasive can constantly rub with silicon material to be cleaned during stirring, and then abrasive can will be wait clean
The impurity on silicon material surface is detached from from silicon material surface to be cleaned, and when finally being cleaned and sorted again, impurity is removed, is cleaned
Silicon material afterwards.In addition, adding water during stirring, abrasive can be evenly dispersed in silicon to be cleaned under the action of water
The inside of material further increases the effect of removal of impurities and the quality of removal of impurities.Impurity-removing method provided by the invention can be effectively removed silicon
Impurity in material, and method is simple, it is at low cost, there is very strong practicability.
In an embodiment of the present invention, the mass ratio of the abrasive and the silicon material to be cleaned is (0.1-0.5): 1.It grinds
The content of abrasive material has a great impact to impurity-eliminating effect.If abrasive is very little, impurity-eliminating effect is bad.If abrasive is too many,
Impurity can not only be removed, can also will be greatly reduced in this way the content of silicon material after removal of impurities part of the surface silicon material to removal.Cause
This, amount of grinding and silicon material to be cleaned need a suitable mass ratio.Preferably, the abrasive and the silicon material to be cleaned
Mass ratio be (0.2-0.4): 1.It is highly preferred that the abrasive and the mass ratio of the silicon material to be cleaned are (0.24-
0.35): 1.
In an embodiment of the present invention, the partial size of the abrasive is 50-150 mesh.The partial size of amount of grinding is big in the present invention
It is small also to will affect impurity-eliminating effect.If the partial size of abrasive is too small, in whipping process, abrasive is stirred with silicon material to be cleaned
It mixes, grinding effect is excessively poor, to can not effectively remove the impurity on silicon material surface to be cleaned since frictional force and impact force are too small
It removes.But if the partial size of abrasive is excessive, and in whipping process, abrasive can not only be removed impurity, can also be part of the surface
Silicon material will be greatly reduced the content of silicon material after removal of impurities to removal in this way.Therefore, the partial size of abrasive needs one suitable big
It is small.Preferably, the partial size of the abrasive is 70-130 mesh.It is highly preferred that the partial size of the abrasive is 90-110 mesh.
In an embodiment of the present invention, the abrasive includes one of the first abrasive and the second abrasive or two
Kind.A kind of abrasive can be used in the present invention or two kinds of abrasives are used in mixed way.
In an embodiment of the present invention, the partial size of first abrasive is 50-100 mesh, the grain of second abrasive
Diameter is 100-150 mesh.When the present invention is used in mixed way using two kinds of abrasives, the partial size of the first abrasive is less than the second abrasive
Partial size.First abrasive of small particle and large-sized second abrasive are used in mixed way and can further improve impurity-eliminating effect.It is excellent
Selection of land, the partial size of first abrasive are 60-90 mesh, and the partial size of second abrasive is 110-140 mesh.It is highly preferred that
The partial size of first abrasive is 70-80 mesh, and the partial size of second abrasive is 120-130 mesh.
In an embodiment of the present invention, the abrasive includes first abrasive and second abrasive, described
The mass ratio of first abrasive and second abrasive is (3-5): 1.When the present invention is used in mixed way using two kinds of abrasives,
The mass ratio of first abrasive of small particle and large-sized second abrasive is (3-5): 1.Above-mentioned introduction said, small particle
The first abrasive and large-sized second abrasive impurity-eliminating effect can be improved.And when the quality of the first abrasive of small particle is
At 3-5 times of the quality of large-sized second abrasive, impurity-eliminating effect can be further improved.Preferably, the abrasive packet
Include first abrasive and second abrasive, the mass ratio of first abrasive and second abrasive is (3-
5): 1.It is highly preferred that the abrasive includes first abrasive and second abrasive, first abrasive and institute
The mass ratio for stating the second abrasive is (3-5): 1.
In an embodiment of the present invention, the material of the abrasive includes one or both of aluminium oxide and silicon carbide.
Abrasive can be aluminium oxide or silicon carbide or silica and silicon carbide in the present invention.
In an embodiment of the present invention, the time of the stirring is 10-60min.Mixing time is longer, can will more to
The impurity removal on removal of impurities silicon material surface, therefore impurity-eliminating effect is better.But mixing time is longer, time of removal of impurities, cost and removes
The price of silicon material but becomes not cost-effective after miscellaneous.Therefore, mixing time of the invention is 10-60min.Preferably, the stirring
Time be 20-50min.It is highly preferred that the time of the stirring is 30-40min.
In an embodiment of the present invention, the impurity-removing method of the silicon material further includes step S104, S105, S106, S107.Its
Middle S104, S105, S106, S107 are described in detail as follows.
S104: being cleaned the mixture after stirring and sorted, and the silicon material that part does not clean is also obtained.
After the S103 the step of, most of impurity that can make silicon material surface to be cleaned after stirring is had wait the silicon material that cleans
Removal to become the silicon material after removal of impurities, but can also obtain the silicon material that part does not clean.
S105: the silicon material to be cleaned separately is taken, by the silicon material not cleaned, the silicon material to be cleaned and the abrasive
Mixing, obtains mixture.
The silicon material that part obtained above does not clean is mixed with the silicon material to be cleaned separately taken again, Lai Jinhang removing again
General labourer's skill can farthest utilize the performance of equipment in this way.If only the silicon for going to processing part not clean using equipment
Material, will greatly waste equipment, and increase the cost of removal of impurities.
S106: the mixture is stirred, and adds water into the mixture during stirring, institute
The impurity wait in the silicon material that cleans can be removed during the stirring by stating abrasive.
Mixture is stirred, therefore abrasive can constantly be connect with silicon material to be cleaned during stirring
Touching, friction, shock etc., and because abrasive is usually the higher material of hardness, hardness can be than wait impurity in the silicon material that cleans
Hardness want high, so abrasive takes off the impurity on silicon material surface to be cleaned from silicon material surface to be cleaned during stirring
From.It comes in this way, impurity just has successfully been isolated with silicon material.In addition, adding water during stirring, abrasive can be in water
It is homogeneously dispersed in the inside of silicon material to be cleaned under effect, further increases the effect of removal of impurities and the quality of removal of impurities.
S107: being cleaned the mixture after stirring and sorted, the silicon material after being cleaned.
Cleaning can preferably separate the silicon material after impurity and removal of impurities, and sort and can finally remove impurity, obtain
Silicon material after to removal of impurities.
In an embodiment of the present invention, the quality of the silicon material not cleaned accounts for the 1- of the quality of the silicon material to be cleaned
35%.
Impurity-removing method provided by the invention, the silicon material that does not clean receive impurity removal process and the selection except miscellaneous time and abrasive
It influences, wherein the quality for the silicon material not cleaned accounts for the 1-35% of the quality of the silicon material to be cleaned.The silicon material quality to have cleaned accounts for
The 65-99% of silicon material quality to be cleaned.Preferably, the quality for the silicon material not cleaned accounts for the 5- of the quality of the silicon material to be cleaned
30%.It is highly preferred that the quality for the silicon material not cleaned accounts for the 10-20% of the quality of the silicon material to be cleaned.
In the following, being classified into multiple embodiments above-described embodiment is explained further.
Embodiment 1
The present invention provides a kind of impurity-removing methods of silicon material, comprising:
Step 1: silicon ingot being separated to the silicon material of low impurity content and the silicon material of high impurity content, wherein the silicon of high impurity content
Material is silicon material to be cleaned.
Step 2: successively can normal use by polishing and acid cleaning process by the silicon material of low impurity content.
Step 3: taking the silicon material to be cleaned of 1500kg, silicon material to be cleaned is put into drum agitation device, according to abrasive
Amount of grinding aluminum oxide corundum is added in the mass ratio that mass ratio with silicon material to be cleaned is 0.3:1, wherein aluminum oxide is rigid
Beautiful partial size is 50 mesh.
Step 4: water is constantly added into agitating device during rolling for silicon material to be cleaned and aluminum oxide corundum,
The time of stirring is 20min.
Step 5: the mixture after stirring is cleaned and sorted, the silicon material after obtaining the removal of impurities of 1125kg, and
The silicon material of remaining 375kg not cleaned, by an impurity removal process, can clean 75% silicon material to be cleaned.
Step 6: the silicon material for separately taking 1125kg to be cleaned is added the silicon material of remaining 375kg not cleaned, is made into again
The silicon material to be cleaned of 1500kg.Repeat step 3- step 5, the silicon material after the last removal of impurities that 1125kg can be obtained again.
Embodiment 2
The present invention provides a kind of impurity-removing methods of silicon material, comprising:
Step 1: silicon ingot being separated to the silicon material of low impurity content and the silicon material of high impurity content, wherein the silicon of high impurity content
Material is silicon material to be cleaned.
Step 2: successively can normal use by polishing and acid cleaning process by the silicon material of low impurity content.
Step 3: taking the silicon material to be cleaned of 1500kg, silicon material to be cleaned is put into drum agitation device, according to abrasive
Amount of grinding aluminum oxide corundum is added in the mass ratio that mass ratio with silicon material to be cleaned is 0.3:1, wherein aluminum oxide is rigid
Beautiful partial size is 150 mesh.
Step 4: water is constantly added into agitating device during rolling for silicon material to be cleaned and aluminum oxide corundum,
The time of stirring is 20min.
Step 5: the mixture after stirring is cleaned and sorted, the silicon material after obtaining the removal of impurities of 975kg, and remain
The silicon material of remaining 525kg not cleaned, by an impurity removal process, can clean 65% silicon material to be cleaned.
Step 6: the silicon material for separately taking 975kg to be cleaned is added the silicon material of remaining 525kg not cleaned, is made into again
The silicon material to be cleaned of 1500kg.Repeat step 3- step 5, the silicon material after the last removal of impurities that 975kg can be obtained again.
Embodiment 3
The present invention provides a kind of impurity-removing methods of silicon material, comprising:
Step 1: silicon ingot being separated to the silicon material of low impurity content and the silicon material of high impurity content, wherein the silicon of high impurity content
Material is silicon material to be cleaned.
Step 2: successively can normal use by polishing and acid cleaning process by the silicon material of low impurity content.
Step 3: taking the silicon material to be cleaned of 1500kg, silicon material to be cleaned is put into drum agitation device, according to abrasive
Amount of grinding aluminum oxide corundum is added in the mass ratio that mass ratio with silicon material to be cleaned is 0.3:1, wherein aluminum oxide is rigid
Jade is divided into the first aluminum oxide corundum and the second aluminum oxide corundum.Wherein, the partial size of the first aluminum oxide corundum is
50 mesh, the partial size of the second aluminum oxide corundum is 100 mesh, and the quality of the first aluminum oxide corundum is aoxidized with the two or three
The mass ratio of two aluminium corundum is 4:1.
Step 4: water is constantly added into agitating device during rolling for silicon material to be cleaned and aluminum oxide corundum,
The time of stirring is 20min.
Step 5: the mixture after stirring is cleaned and sorted, the silicon material after obtaining the removal of impurities of 1275kg, and
The silicon material of remaining 225kg not cleaned, by an impurity removal process, can clean 85% silicon material to be cleaned.
Step 6: the silicon material for separately taking 1275kg to be cleaned is added the silicon material of remaining 225kg not cleaned, is made into again
The silicon material to be cleaned of 1500kg.Repeat step 3- step 5, the silicon material after the last removal of impurities that 1275kg can be obtained again.
Content provided by embodiment of the present invention is described in detail above, herein to the principle of the present invention and reality
The mode of applying is expounded and illustrates, described above to be merely used to help understand method and its core concept of the invention；Meanwhile
For those of ordinary skill in the art, according to the thought of the present invention, has change in specific embodiments and applications
Become place, in conclusion the contents of this specification are not to be construed as limiting the invention.
Claims (10)
1. a kind of impurity-removing method of silicon material characterized by comprising
Silicon material to be cleaned is taken, the silicon material to be cleaned and abrasive are mixed, mixture is obtained；
The mixture is stirred, and adds water into the mixture during stirring, the abrasive
The impurity wait in the silicon material that cleans can be separated with silicon material during the stirring；
The mixture after stirring is cleaned and sorted, the silicon material after being cleaned.
2. impurity-removing method as described in claim 1, which is characterized in that the mass ratio of the abrasive and the silicon material to be cleaned
For (0.1-0.5): 1.
3. impurity-removing method as described in claim 1, which is characterized in that the partial size of the abrasive is 50-150 mesh.
4. impurity-removing method as claimed in claim 3, which is characterized in that the abrasive includes the first abrasive and the second grinding
One or both of material.
5. impurity-removing method as claimed in claim 4, which is characterized in that the partial size of first abrasive is 50-100 mesh, institute
The partial size for stating the second abrasive is 100-150 mesh.
6. impurity-removing method as claimed in claim 4, which is characterized in that the abrasive includes first abrasive and described
The mass ratio of second abrasive, first abrasive and second abrasive is (3-5): 1.
7. impurity-removing method as described in claim 1, which is characterized in that the material of the abrasive includes aluminium oxide and silicon carbide
One or both of.
8. impurity-removing method as described in claim 1, which is characterized in that the time of the stirring is 10-60min.
9. impurity-removing method as described in claim 1, which is characterized in that the impurity-removing method of the silicon material further include:
The mixture after stirring is cleaned and sorted, the silicon material that part does not clean is also obtained；
The silicon material to be cleaned separately is taken, the silicon material not cleaned, the silicon material to be cleaned and the abrasive are mixed, obtained
Mixture；
The mixture is stirred, and adds water into the mixture during stirring, the abrasive
The impurity wait in the silicon material that cleans can be removed during the stirring；
The mixture after stirring is cleaned and sorted, the silicon material after being cleaned.
10. impurity-removing method as claimed in claim 9, which is characterized in that the quality of the silicon material not cleaned accounts for described wait remove
The 1-35% of the quality of miscellaneous silicon material.
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| CN101659413A (en) * | 2008-08-27 | 2010-03-03 | 比亚迪股份有限公司 | Method for preparing ultra-metallurgical grade silicon |
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| JP2011144072A (en) * | 2010-01-14 | 2011-07-28 | Sumitomo Chemical Co Ltd | Method for producing refined silicon |
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