CN101428252B - Classification method for waste silicon material mixed with foreign matter - Google Patents

Classification method for waste silicon material mixed with foreign matter Download PDF

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CN101428252B
CN101428252B CN 200810136530 CN200810136530A CN101428252B CN 101428252 B CN101428252 B CN 101428252B CN 200810136530 CN200810136530 CN 200810136530 CN 200810136530 A CN200810136530 A CN 200810136530A CN 101428252 B CN101428252 B CN 101428252B
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silicon material
impurity
mixed
separating
solution
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CN101428252A (en
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章金兵
王志辉
叶淳超
郭扬飞
王平军
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LDK Solar Co Ltd
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LDK Solar Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/002Inorganic compounds

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Abstract

The invention relates to a sorting method for a waste silicon material mixed with impurities in the technical field of semiconductors and solar energy, particularly to a separation method for a fine crushing silicon material mixed with impurities, and aims to provide an efficient sorting method for the waste silicon material mixed with impurities. The sorting method for the waste silicon mixture mixed with impurities is characterized in that the waste silicon material mixed with impurities is thrown into a carbonate solution; gas generated from the reaction of the carbonate solution and the silicon material drives the residual silicon material to float; the floating silicon mixture is obtained; and the impurities are separated from the silicon material. Therefore, the sorting of the waste silicon material mixed with impurities is completed. The invention adopts the carbonate solution for silicon material sorting with high sorting efficiency, so that the invention is applicable to the scale sorting, and can completely replace the traditional hand-sorting method.

Description

A kind of method for separating that is mixed with the useless silicon material of impurity
Technical field
The present invention relates to a kind of method for separating that is mixed with the useless silicon material of impurity of semiconductor and field of solar energy, particularly a kind of method for separating that is mixed with the in small, broken bits useless silicon material of impurity, the silicon material after sorting process is mainly used in the photovoltaic field.
Background technology
The recovery of useless silicon material mainly refers to the recovery of the discarded object that contains silicon of appearance in semiconductor and the photovoltaic processing.The target that useless silicon material reclaims refers to silicon be separated from discarded object and clean out, and makes its raw material that can be used as photovoltaic cell, thereby reduces raw-material cost.Be mixed with a lot of impurity in the useless silicon material that reclaims, at first must carry out sorting to it.
Mainly be to carry out sorting by manually pursuing piecewise grain ground for these processing methods that are mixed with very polymictic useless silicon material at present, this method for separating need consume a large amount of manpowers.Especially for particle diameter less than the useless silicon material of 10mm, 5mm, granularity is less, and be mixed with the impurity such as a large amount of dust, mud, assorted bits, broken collodion silk, quartz, adopt artificial separation not only to expend sizable manpower, and the efficiency of separation is low, on average sorting silicon material amount only has 1-3Kg for each person every day, and this obviously is disadvantageous for reducing life cycle of the product.Particularly wash the silicon material and mainly refer to solar energy polycrystalline silicon sheet producer when cleaning the raw silicon material for picking up the sorting of washing the silicon material, picking up, remain at Pickling-shop, clean the disintegrating slag of mill floor, trench, cleaning equipment inside etc.This disintegrating slag granularity is less, generally be lower than 1mm, and be mixed with the various impurity such as a large amount of dust, mud, assorted bits, broken collodion silk, adopt inefficient at present artificial separation technology to process these and pick up that to wash the silicon material very difficult, can not solve the ten sorting problems of washing the silicon material at all, cause picking up of whole semiconductor applications to wash the silicon material and overstock in a large number.
Summary of the invention
The object of the present invention is to provide a kind of high efficiency method for separating that is mixed with the useless silicon material of impurity.The present invention utilizes carbonate solution and silicon material generated reactive gas, and gas drives remaining silicon material come-up to be separated impurity with the silicon material, thereby realizes being mixed with the sorting of the useless silicon material of impurity, has efficiency of separation height, handling safety and the advantage such as simple.
Technical scheme of the present invention is:
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: comprise following operating procedure:
The useless silicon material that (1) will be mixed with impurity drops in the carbonate solution;
(2) gas of carbonate solution and silicon material reaction generation drives remaining silicon material come-up;
(3) fish for the silicon material of come-up, realize separating of impurity and silicon material, finish the sorting of the useless silicon material that is mixed with impurity.
Be deposited on solution bottom the silicon material will be weakly alkaline carbonate solution slight reaction arranged, the gas that silicon material and carbonate solution reaction produce directly drives remaining silicon material come-up itself, its reacting phenomenon is that silicon material surface produces a lot of bubbles, in the time of on one side with the carbonate solution generated reactive gas, gas drives remaining silicon material and floats on one side, and the impurity that is mixed with in the silicon material can not participate in reaction, still is sunken to the bottom of solution, realizes that the silicon material separates with the whole of impurity.
Because carbonic acid (hydrogen) radical ion and steeping in water for reconstitution are given birth to faint reaction and are produced carbon dioxide and hydroxide ion OH, so that carbonate solution is alkalescent, before the silicon material does not drop into, chemical reaction between carbonic acid (hydrogen) radical ion and the water is balance, and in silicon material input carbonate solution, the hydroxide ion OH in silicon material and the carbonate solution -Will react, consume OH -, so that OH -Concentration reduce, according to chemical equilibrium theory, OH -Concentration reduce, chemical reaction equilibrium state before will having destroyed between carbonic acid (hydrogen) radical ion and the water, reaction between carbonic acid (hydrogen) radical ion and the water can move right, and what promote reaction carries out carbon dioxide and hydroxide ion OH to the right -Will constantly produce the hydroxide ion OH that constantly produces -Can constantly react again with the silicon material, so that carbon dioxide constantly produces, the carbon dioxide that constantly produces drives remaining silicon material come-up, and impurity is separated with the silicon material.With the carbonate solution reaction equation be: 2Si+3CO 3 2-+ 3H 2O====3CO 2↑+2SiO 3 2-+ 3H 2↑, its reaction mechanism equation is:
Figure G2008101365303D00021
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 50-100 ℃.Because when the temperature of carbonate solution is lower than 50 ℃ and during greater than 40 ℃, the reaction of silicon material and carbonate solution is too faint, the time that silicon material come-up needs is long, and the weight ratio that the silicon material of come-up accounts for total silicon material is little, and the temperature of carbonate solution is when being lower than 40 ℃, silicon material and carbonate solution react hardly, and the silicon material is non-rising; When the temperature of carbonate solution during greater than 100 ℃, carbonate solution boiling, the solution that impurity also can be seethed with excitement in the time of silicon material come-up is brought up, and silicon material and impurity can not obtain effective separation.The temperature of carbonate solution is 50-100 ℃ and reaches by heater means.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is the 1.05-1.6 grams per milliliter.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described carbonate solution can be any one or a few mixing of aqueous sodium carbonate, wet chemical, sodium bicarbonate aqueous solution, potassium bicarbonate aqueous solution.
Adopt the separating effect of technical scheme of the present invention and conventional solution relatively
Figure G2008101365303D00031
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: with silicon material process gravity treatment preliminary treatment.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: after (3) step, increase by (4) step: gravity treatment.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the operating procedure of gravity treatment is:
1. the silicon material being dropped into density is in the gravity treatment solution of 1.05-2.28 grams per milliliter;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on gravity treatment solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up.
Owing to may be mixed with simultaneously many various impurity in the useless silicon material (washing the silicon material as picking up) that has, such as dust, mud, assorted bits, broken collodion silk, quartzy, plastics, dust, broken collodion silk, the density of plastics is about 0.7-1.5 g/cc, quartzy density is about 2.1/ cubic centimetre, also has the density of some assorted bits at 2.4 g/ccs or greater than 2.4 g/ccs, and the density of silicon material is 2.33 g/ccs, because the scope of the density of carbonate solution is generally at the 1.05-1.6 grams per milliliter, if the density of the density ratio carbonate solution of some impurity that are mixed with in the silicon material hour, the impurity that the density of these density ratio carbonate solutions is little can be at the effect float downward of buoyancy, thereby cause the impurity of this part come-up and silicon material still to mix, fail to separate.In order to prevent this from occurring, can be before implementing this invention with the silicon material through the gravity treatment preliminary treatment or implement after this invention again increase and carry out (4) step: gravity treatment.
Adopting gravity treatment to come the principle that the silicon material is processed is to utilize the density variation of storeroom to produce separation, and the material that specifically density ratio gravity treatment solution density is large can not float, and the material that density ratio gravity treatment solution density is little can float, thereby reaches the purpose of separation.In the present invention, because gravity treatment is in order to remove these because and impurity that can float less than the density of carbonate solution, so the gravity treatment liquid density that adopts should be equal to or greater than the density of carbonate solution, also be less than the density of silicon material, can guarantee that so just these impurity that float can float in carbonate solution, and the silicon material can not float in gravity treatment solution.Because the scope of the density of carbonate solution is generally at the 1.05-1.6 grams per milliliter, the density of silicon material is 2.33 g/ccs, satisfies these requirements so density is the gravity treatment solution of 1.05-2.28 grams per milliliter.Take the density of carbonate solution as 1.05 grams per milliliters as example, if when being mixed with the little impurity of some density ratio 1.05 grams per milliliters in the silicon material, this part impurity also can float with the silicon material, in order to remove the impurity of this part come-up, the employing gravity treatment removes, and to select density be 1.05 grams per milliliters or just can remove these impurity less than the gravity treatment solution of 2.33 grams per milliliters greater than 1.05 grams per milliliters; And when the density of the carbonate solution that adopts is 1.2 grams per milliliter, if when being mixed with the little impurity of some density ratio 1.2 grams per milliliters in the silicon material, this part impurity also can float with the silicon material, the impurity that maybe may float in order to remove this part come-up, the employing gravity treatment removes, and to select density be 1.2 grams per milliliters or just can remove these impurity less than the gravity treatment solution of 2.33 grams per milliliters greater than 1.2 grams per milliliters.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described gravity treatment solution can be one or more mixing of solution of calcium bromide in water, the zinc bromide aqueous solution, the calcium iodide aqueous solution, the metatungstic acid aqueous solution, aqueous sodium carbonate, wet chemical, sodium bicarbonate aqueous solution, potassium bicarbonate aqueous solution or other organic or inorganic solution.
Gravity treatment among the present invention is to carry out not being higher than under 40 ℃ the temperature conditions, so when the carbonate solutions such as gravity treatment solution employing aqueous sodium carbonate, wet chemical, sodium bicarbonate aqueous solution or potassium bicarbonate aqueous solution, because the reaction of silicon material and carbonate solution generally needs just can react more than 40 ℃, so in the gravity treatment step, the silicon material can not react with carbonate solution, and carbonate solution also can be used as gravity treatment solution of the present invention.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution or gravity treatment solution is 1: 2-1: 50.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle size range that is mixed with the useless silicon material of impurity is 0.001-50mm.
A kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity can be any one or a few of dust, mud, assorted bits, broken collodion silk, plastics, quartz.
Operation principle of the present invention: the silicon material be weakly alkaline carbonate solution slight reaction arranged, the gas that reaction produces will drive remaining silicon material and promptly float, impurity will be sunken to the bottom of solution; And the little impurity of carbonate solution density that adopts for some density ratios, impurity can float at carbonate solution, utilizes gravity treatment that the impurity of these come-ups is separated with the silicon material.
Advantage of the present invention: the efficiency of separation is high, is applicable to the scale sorting, can replace traditional artificial separation fully.
The specific embodiment
Embodiment 1, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: comprise following operating procedure:
The useless silicon material that (1) will be mixed with impurity drops in the carbonate solution;
(2) gas of carbonate solution and silicon material reaction generation drives remaining silicon material come-up;
(3) fish for the silicon material of come-up, realize separating of impurity and silicon material, finish the sorting of the useless silicon material that is mixed with impurity.
Embodiment 2, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 1 ℃, and all the other are with embodiment 1.
Embodiment 3, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 10 ℃, and all the other are with embodiment 1.
Embodiment 4, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 25 ℃, and all the other are with embodiment 1.
Embodiment 5, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 40 ℃, and all the other are with embodiment 1.
Embodiment 6, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 50 ℃, and all the other are with embodiment 1.
Embodiment 7, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 60 ℃, and all the other are with embodiment 1.
Embodiment 8, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 70 ℃, and all the other are with embodiment 1.
Embodiment 9, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 80 ℃, and all the other are with embodiment 1.
Embodiment 10, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 90 ℃, and all the other are with embodiment 1.
Embodiment 11, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 100 ℃, and all the other are with embodiment 1.
Embodiment 12, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the temperature of described carbonate solution is 105 ℃, and all the other are with embodiment 1.
Embodiment 13, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.02 grams per milliliters, and all the other are with embodiment 1.
Embodiment 14, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.05 grams per milliliters, and all the other are with embodiment 1.
Embodiment 15, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.1 grams per milliliters, and all the other are with embodiment 1.
Embodiment 16, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.2 grams per milliliters, and all the other are with embodiment 1.
Embodiment 17, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.3 grams per milliliters, and all the other are with embodiment 1.
Embodiment 18, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.4 grams per milliliters, and all the other are with embodiment 1.
Embodiment 19, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.5 grams per milliliters, and all the other are with embodiment 1.
Embodiment 20, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the density of described carbonate solution is 1.6 grams per milliliters, and all the other are with embodiment 1.
Embodiment 21, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described carbonate solution can be any one or a few mixing of aqueous sodium carbonate, wet chemical, sodium bicarbonate aqueous solution, potassium bicarbonate aqueous solution, and all the other are with embodiment 1.
Embodiment 22, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described carbonate solution is wet chemical, all the other are with embodiment 1.
Embodiment 23, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described carbonate solution is aqueous sodium carbonate, all the other are with embodiment 1.
Embodiment 24, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described carbonate solution is sodium bicarbonate aqueous solution, all the other are with embodiment 1.
Embodiment 25, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described carbonate solution is potassium bicarbonate aqueous solution, all the other are with embodiment 1.
Embodiment 26, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: through the gravity treatment preliminary treatment, all the other are respectively with any one embodiment among the embodiment 1-25 with the silicon material.
Embodiment 27, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: increase by the (4) step after (3) step: gravity treatment, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 28, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the operating procedure of gravity treatment is:
1. the silicon material being dropped into density is in the gravity treatment solution of 1.05-2.28 grams per milliliter;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on gravity treatment solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are respectively with embodiment 26,27.
Embodiment 29, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described gravity treatment solution can be one or more mixing of solution of calcium bromide in water, the zinc bromide aqueous solution, the calcium iodide aqueous solution, the metatungstic acid aqueous solution, aqueous sodium carbonate, wet chemical, sodium bicarbonate aqueous solution, potassium bicarbonate aqueous solution or other organic or inorganic solution, and all the other are with embodiment 28.
Embodiment 30, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material being dropped into density is in the aqueous sodium carbonate of 1.05 grams per milliliters;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 31, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material being dropped into density is in the potassium bicarbonate aqueous solution of 1.1 grams per milliliters;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 32, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material being dropped into density is in the sodium bicarbonate aqueous solution of 1.2 grams per milliliters;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 33, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material being dropped into density is in the aqueous sodium carbonate of 1.3 grams per milliliters;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 34, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material being dropped into density is in the wet chemical of 1.4 grams per milliliters;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 35, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material is dropped in the mixed solution of the metatungstic acid aqueous solution that density is 1.6 grams per milliliters, the calcium iodide aqueous solution, alcohol;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 36, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material is dropped in the mixed solution of solution of calcium bromide in water that density is 1.8 grams per milliliters, the zinc bromide aqueous solution;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 37, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material is dropped in the mixed solution of the calcium iodide aqueous solution that density is 2.0 grams per milliliters, the metatungstic acid aqueous solution, alcohol;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 38, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the step of gravity treatment is:
1. the silicon material is dropped in the mixed solution of the calcium iodide aqueous solution that density is 2.28 grams per milliliters, the metatungstic acid aqueous solution, solution of calcium bromide in water, alcohol;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on the solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up, all the other are with embodiment 28.
Embodiment 39, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 2, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 40, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 5, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 41, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 8, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 42, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 10, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 43, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 15, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 44, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 20, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 45, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 30, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 46, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 40, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 47, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and carbonate solution is 1: 50, all the other are respectively with any one embodiment among the embodiment 1-25.
Embodiment 48, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 2, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 49, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 5, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 50, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 8, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 51, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 10, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 51, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 15, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 53, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 20, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 54, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 30, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 55, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 40, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 56, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the weight ratio of silicon material and gravity treatment solution is 1: 50, all the other are respectively with any one embodiment among the embodiment 28-38.
Embodiment 57, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 0.001mm, and all the other are with embodiment 1.
Embodiment 58, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 0.01mm, and all the other are with embodiment 1.
Embodiment 59, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 0.1mm, and all the other are with embodiment 1.
Embodiment 60, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 1mm, and all the other are with embodiment 1.
Embodiment 61, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 2mm, and all the other are with embodiment 1.
Embodiment 62, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 3mm, and all the other are with embodiment 1.
Embodiment 63, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 4mm, and all the other are with embodiment 1.
Embodiment 64, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 5mm, and all the other are with embodiment 1.
Embodiment 65, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 8mm, and all the other are with embodiment 1.
Embodiment 66, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 10mm, and all the other are with embodiment 1.
Embodiment 67, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 20mm, and all the other are with embodiment 1.
Embodiment 68, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 30mm, and all the other are with embodiment 1.
Embodiment 69, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 40mm, and all the other are with embodiment 1.
Embodiment 70, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: the described particle diameter that is mixed with the useless silicon material of impurity is 50mm, and all the other are with embodiment 1.
Embodiment 71, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity can be any one or a few of dust, mud, assorted bits, broken collodion silk, plastics, quartz, and all the other are respectively with any one embodiment among the embodiment 1-70.
Embodiment 72, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity is dust, all the other are respectively with any one embodiment among the embodiment 1-70.
Embodiment 73, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity is mud, all the other are respectively with any one embodiment among the embodiment 1-70.
Embodiment 74, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity is assorted bits, and all the other are respectively with any one embodiment among the embodiment 1-70.
Embodiment 75, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity is broken collodion silk, all the other are respectively with any one embodiment among the embodiment 1-70.
Embodiment 76, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity is plastics, all the other are respectively with any one embodiment among the embodiment 1-70.
Embodiment 77, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity is quartzy, and all the other are respectively with any one embodiment among the embodiment 1-70.
Embodiment 78, a kind of method for separating that is mixed with the useless silicon material of impurity, wherein: described impurity is dust, mud, assorted bits, broken collodion silk, plastics, and all the other are respectively with any one embodiment among the embodiment 1-70.

Claims (1)

1. method for separating that is mixed with the useless silicon material of impurity, wherein: comprise following operating procedure:
The useless silicon material that (1) will be mixed with impurity drops in the carbonate solution, and wherein the temperature of carbonate solution is 70 ℃, and density is 1.4 grams per milliliters, and the weight ratio of silicon material and carbonate solution is 1: 30;
(2) gas of carbonate solution and silicon material reaction generation drives remaining silicon material come-up;
(3) fish for the silicon material of come-up, realize separating of impurity and silicon material, finish the sorting of the useless silicon material that is mixed with impurity.
After (3) step, increase by (4) step: gravity treatment, its operating procedure is:
1. the silicon material that obtains in the step (3) being dropped into density is in the gravity treatment solution of 1.6 grams per milliliters, and gravity treatment solution is the mixed solution of the metatungstic acid aqueous solution, the calcium iodide aqueous solution, alcohol, and the weight ratio of silicon material and gravity treatment solution is 1: 20;
2. the impurity come-up that density ratio gravity treatment solution density is little in the silicon material is separated with the silicon material that is deposited on gravity treatment solution bottom;
3. remove the impurity of come-up, obtained removing the silicon material of the impurity of come-up.
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CN102040222B (en) * 2009-10-23 2012-09-19 上海九晶电子材料股份有限公司 Method for separating silicon material from heavily doped silicon material
CN101912809A (en) * 2010-08-26 2010-12-15 江西旭阳雷迪高科技股份有限公司 Method for separating semiconductor broken silicon wafers and guide bars
CN102247933A (en) * 2011-03-22 2011-11-23 江西赛维Ldk太阳能高科技有限公司 Method for purifying silicon powder
CN102814297A (en) * 2012-08-13 2012-12-12 安阳市凤凰光伏科技有限公司 Cleaning solution for separating silicon material in manner of sedimentation and preparation and application method of cleaning solution
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CN111232988B (en) * 2020-04-10 2022-07-29 昆明理工大学 Method for efficiently separating slag silicon from industrial silicon slag
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