CN104445208A - Method for removing impurities from polycrystalline silicon cast ingot leftovers - Google Patents

Method for removing impurities from polycrystalline silicon cast ingot leftovers Download PDF

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Publication number
CN104445208A
CN104445208A CN201410733691.6A CN201410733691A CN104445208A CN 104445208 A CN104445208 A CN 104445208A CN 201410733691 A CN201410733691 A CN 201410733691A CN 104445208 A CN104445208 A CN 104445208A
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polycrystalline silicon
acid
silicon material
ingot casting
edge skin
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CN201410733691.6A
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Chinese (zh)
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付红平
章金兵
刘渝龙
彭也庆
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LDK Solar Co Ltd
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LDK Solar Co Ltd
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Priority to CN201410733691.6A priority Critical patent/CN104445208A/en
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Abstract

The invention discloses a method for removing impurities from polycrystalline silicon cast ingot leftovers. The method comprises the following steps: crushing the polycrystalline silicon cast ingot leftovers to obtain a polycrystalline silicon material with a targeted size; soaking the polycrystalline silicon material with the targeted size in an acidic corrosive solution or an alkaline corrosive solution to remove the impurities such as silicon carbide, silicon nitride and metals from the surface of the polycrystalline silicon material; washing the soaked polycrystalline silicon material with pure water until the solution is neutral; drying the polycrystalline silicon material. According to the method, the sliced or blocky polycrystalline silicon leftovers are firstly crushed by a jaw crusher to obtain a granular polycrystalline silicon material, so that more embedded impurities can be exposed from the surface of the polycrystalline silicon material, and then the impurities are corroded by the acidic solution or the alkaline solution to remove the embedded impurities from the surface of the polycrystalline silicon material, and thus an impurity removal effect is achieved.

Description

The decon method of polycrystalline silicon ingot casting edge skin material
Technical field
The present invention relates to polysilicon process field, particularly relate to a kind of decon method of polycrystalline silicon ingot casting edge skin material.
Background technology
Due to the impact of polycrystalline silicon raw material and ingot casting environment, some impurity are produced as silicon carbide and silicon nitride inclusions in polycrystalline silicon ingot casting process, this kind of impurity is gathered in silicon ingot upper and lower surface and surrounding under the effect of directional freeze impurities removal, silicon ingot can produce a large amount of edge skin materials containing above-mentioned impurity (silicon carbide, silicon nitride etc.) after evolution, tail of decaptitating, this part silicon material due to foreign matter content too much, can not directly melt down, and being embedded in polycrystalline silicon ingot casting edge skin material due to impurity, recovery method traditional at present cannot reach the object of impurity elimination.
The recovery method of polycrystal silicon ingot edge skin material traditional at present generally adopts the method for pickling or alkali cleaning, namely under the high temperature conditions silico briquette surface is corroded by nitric acid/hydrofluoric acid or concentrated base, by constantly corroding, impurities on surface of silicon chip is come off from silico briquette matrix, thus realize the recycling of silico briquette.Adopt aforesaid method, good impurity elimination effect can be played for the polycrystal silicon ingot edge skin material that surface is impure, but for the polysilicon edge skin material of embedded solid impurity, cannot process, thus cause the waste of this type of resource.
Summary of the invention
The object of the present invention is to provide a kind of decon method that can remove the polycrystalline silicon ingot casting edge skin material of the embedded impurity of polysilicon.
In order to solve the problems of the technologies described above, the invention provides a kind of decon method of polycrystalline silicon ingot casting edge skin material, wherein, comprising the following steps:
(1) break process is carried out to polycrystalline silicon ingot casting edge skin material, obtain the polycrystalline silicon material of target size;
(2) polycrystalline silicon material of target size is positioned in acid etching solution or alkaline corrosion liquid soaks, remove the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities;
(3) by the polycrystalline silicon material pure water rinsing after soaking to solution in neutral;
(4) polycrystalline silicon material is dried.
The decon method of polycrystalline silicon ingot casting edge skin material provided by the invention, by first carrying out fragmentation to polycrystalline silicon ingot casting edge skin material, obtain granular polycrystalline silicon material, thus make more embedded impurity be exposed to polycrystalline silicon material surface, and then utilize acid solution or alkaline solution to corrode polycrystalline silicon material, make embedded impurity from polycrystalline silicon material sur-face peeling, reach the effect of removing impurity.
Present invention also offers a kind of decon method of polycrystalline silicon ingot casting edge skin material, wherein, comprise the following steps:
(1) break process is carried out to polycrystalline silicon ingot casting edge skin material, obtain the polycrystalline silicon material of target size;
(2) polycrystalline silicon material of target size is positioned in acid etching solution soaks, remove the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities;
(3) the polycrystalline silicon material pure water rinsing after being soaked by acid etching solution to solution is neutral;
(4) polycrystalline silicon material after rinsing is positioned in alkaline corrosion liquid and soaks, remove the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities further;
(5) the polycrystalline silicon material pure water rinsing after alkaline corrosion immersion being steeped to solution is neutral;
(6) polycrystalline silicon material is dried.
The decon method of polycrystalline silicon ingot casting edge skin material provided by the invention, by first utilizing acid etching solution, granular polycrystalline silicon material is once corroded, after removing silicon carbide, silicon nitride or metallic impurity, polycrystalline silicon material is cleaned, and then utilize alkaline corrosion liquid further to remove impurity to polycrystalline silicon material, make the purity of polycrystalline silicon material higher, effectively improve the efficiency of removing impurity.
Accompanying drawing explanation
In order to be illustrated more clearly in technical scheme of the present invention, be briefly described to the accompanying drawing used required in embodiment below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the schema of decon method first embodiment of polycrystalline silicon ingot casting edge skin material provided by the invention;
Fig. 2 is the schema of decon method second embodiment of polycrystalline silicon ingot casting edge skin material provided by the invention;
Fig. 3 is the schema of decon method the 3rd embodiment of polycrystalline silicon ingot casting edge skin material provided by the invention.
Embodiment
Below in conjunction with the accompanying drawing in embodiment of the present invention, the technical scheme in embodiment of the present invention is clearly and completely described.
Refer to Fig. 1, the decon method of a kind of polycrystalline silicon ingot casting edge skin material in the first embodiment provided by the invention.The method comprises the following steps:
Step 101: carry out break process to polycrystalline silicon ingot casting edge skin material, obtains the granulated polycrystalline silicon material of target size.
Because polycrystalline silicon ingot casting can form the polycrystalline silicon ingot casting edge skin material of bulk or sheet after evolution, tail of decaptitating, after utilizing jaw crusher to carry out fragmentation to described polycrystalline silicon ingot casting edge skin material, obtain granular polycrystalline silicon material, thus make more embedded impurity be exposed to polycrystalline silicon material surface.In the present embodiment, the mean value of the diameter target size of described polycrystalline silicon material is 5 ~ 50mm, concrete, and as preferred value, the mean value of described target size is 30mm.Namely, when to obtain granulated polycrystalline silicon material mean diameter after fragmentation be 30mm, stop broken.In other embodiments, described target size also can be 40mm, or 10mm.
Step 102: be positioned in acid etching solution by the polycrystalline silicon material of target size and soak, removes the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities.
In the present embodiment, before described granulated polycrystalline silicon material is corroded, first described polycrystalline silicon material is placed in pure water groove and cleans, remove some as the impurity such as mud, dust, then silicon material is placed in described acidic corrosion solution, and utilize ultrasonic wave or whipping appts to accelerate the corrosion of described granulated polycrystalline silicon material, control the temperature of described acidic corrosion solution between 20 DEG C-50 DEG C, concrete, can be 40 DEG C, continue the cleaning of Preset Time.
Described acid etching solution is the mixing solutions of mixing acid and strong oxidizer, the surface silicon molecule of described acid etching solution and described granulated polycrystalline silicon material is utilized to react, thus the impurity making silicon carbide and silicon nitride etc. be difficult to decompose is peeled off from silicon material, reaches removal of impurity object.As the more excellent scheme of one, first embodiment is provided, being configured to of described acid etching solution: get hydrofluoric acid, the volumetric concentration nitric acid that is 60% ~ 80%, volumetric concentration be 25% ~ 45% hydrogen peroxide and the pure water that volumetric concentration is 40% ~ 60%, concrete, get hydrofluoric acid, the volumetric concentration nitric acid that is 68%, volumetric concentration be 35% hydrogen peroxide and the pure water that volumetric concentration is 49%.In described acid etching solution, the volume ratio of each component is hydrofluoric acid: nitric acid: hydrogen peroxide: pure water=1: 1: 1: 2.
In the present embodiment, provide the first embodiment, described Preset Time is 0.1 ~ 1.2 hour, concrete, and described Preset Time is 0.5 hour.Certainly, in other embodiments, described acid etching solution can also be the mixed solution of nitric acid, hydrofluoric acid and acetic acid; Hydrofluoric acid, the volumetric concentration nitric acid that is 75%, volumetric concentration be 40% hydrogen peroxide and the pure water that volumetric concentration is 42% can also be got in the mixing solutions of mixing acid and strong oxidizer; Can also be control described acidic corrosion solution temperature between 50 DEG C-80 DEG C, described Preset Time can also be 1.2 ~ 2.0 hours.
In the present embodiment, provide the second embodiment, the second embodiment is roughly the same with the first embodiment, also comprises mineral acid unlike described mixing acid, and described mineral acid is hydrochloric acid, and in other embodiments, described mineral acid can also be phosphoric acid or sulfuric acid.
In the present embodiment, 3rd embodiment is provided, 3rd embodiment is roughly the same with the first embodiment, also mineral acid is comprised unlike described mixing acid, described mineral acid is the combination of hydrochloric acid and phosphoric acid, in other embodiments, described mineral acid can also be the combination of hydrochloric acid and sulfuric acid, or the combination of phosphoric acid and sulfuric acid.
In the present embodiment, provide the 4th embodiment, the 4th embodiment is roughly the same with the first embodiment, also comprises mineral acid unlike described mixing acid, and described mineral acid is the combination of hydrochloric acid, phosphoric acid and sulfuric acid.
In the present embodiment, provide the 5th embodiment, the 5th embodiment is roughly the same with the first embodiment, also comprises organic acid unlike described mixing acid, and described organic acid is formic acid, and in other embodiments, described organic acid can also be acetic acid or propionic acid.
In the present embodiment, 6th embodiment is provided, 6th embodiment is roughly the same with the first embodiment, also organic acid is comprised unlike described mixing acid, described organic acid is the combination of formic acid and acetic acid, in other embodiments, described organic acid can also be the combination of formic acid and propionic acid, or the combination of acetic acid and propionic acid.
In the present embodiment, provide the 7th embodiment, the 7th embodiment is roughly the same with the first embodiment, also comprises organic acid unlike described mixing acid, and described organic acid is the combination of formic acid, acetic acid and propionic acid.
In the present embodiment, 8th embodiment is provided, 8th embodiment is roughly the same with the first embodiment, unlike, described mixing acid also comprises the mixing of organic acid and mineral acid, described organic acid is the combination of formic acid, acetic acid and propionic acid, and described mineral acid is the combination of hydrochloric acid, phosphoric acid and sulfuric acid.In other embodiments, described organic acid can also be the combination of formic acid and acetic acid, or the combination of formic acid and propionic acid, or the combination of acetic acid and propionic acid, or any one of formic acid, acetic acid and propionic acid; Described mineral acid can also be the combination of hydrochloric acid and phosphoric acid, or the combination of hydrochloric acid and sulfuric acid, or the combination of phosphoric acid and sulfuric acid, or hydrochloric acid, phosphoric acid, sulfuric acid any one.
In the present embodiment, provide the 9th embodiment, the 9th embodiment is roughly the same with the first embodiment, unlike, described strong oxidizer is the oxygenant of Standard Electrode Potentials higher than nitric acid, such as: described strong oxidizer is persulphate.
In the present embodiment, provide the tenth embodiment, the tenth embodiment is roughly the same with the first embodiment, unlike, described strong oxidizer is superoxide, such as: described strong oxidizer is hydrogen peroxide.In other embodiments, described strong oxidizer can also be Peracetic Acid, or the combination of hydrogen peroxide and hydrogen peroxide.
In the present embodiment, provide the 11 embodiment, the 11 embodiment is roughly the same with the first embodiment, unlike, described strong oxidizer is metal oxide, such as: described strong oxidizer is plumbic oxide.In other embodiments, described strong oxidizer can also be Manganse Dioxide or cobalt dioxide, or described reinforcer can also be plumbic oxide and Manganse Dioxide, or the combination of plumbic oxide and cobalt dioxide, or the combination of Manganse Dioxide and cobalt dioxide, or the combination of plumbic oxide, Manganse Dioxide and cobalt dioxide.
In the present embodiment, provide the 12 embodiment, the 12 embodiment is roughly the same with the first embodiment, unlike, described strong oxidizer is salt, such as: described strong oxidizer is potassium permanganate.In other embodiments, described strong oxidizer can also be potassium bichromate or Potcrate, or the combination of potassium permanganate and potassium bichromate, or the combination of potassium permanganate and Potcrate, or the combination of potassium bichromate and Potcrate, or the combination of potassium permanganate, potassium bichromate and Potcrate.
In the present embodiment, provide the 13 embodiment, the 13 embodiment is roughly the same with the first embodiment, unlike, described strong oxidizer is gas, such as: described strong oxidizer is ozone.In other embodiments, described strong oxidizer can also be chlorine or fluorine gas, or the combination of ozone and chlorine, or the combination of ozone and fluorine gas, or the combination of chlorine and fluorine gas, or the combination of ozone, chlorine and fluorine gas.
In the present embodiment, described mixing acid and described strong oxidizer can also be combining of the various ways of above embodiment.
Step 103: by the polycrystalline silicon material pure water rinsing after soaking to solution in neutral.
In the present embodiment, described polycrystalline silicon material is picked up and is placed in drainage trap, and by pure water rinsing, when the solution of polysilicon surface is in neutrality, again described polycrystalline silicon material is picked up, be positioned in container.
Step 104: polycrystalline silicon material is dried.
In the present embodiment, be positioned in roasting plant by the described polycrystalline silicon material be positioned in container, arrange storing temperature at 100 DEG C-150 DEG C, baking time, at 12 hours-30 hours, is dried, and is packed by the polycrystalline silicon material after drying, for subsequent use.
Refer to Fig. 2, the invention provides the decon method of a kind of polycrystalline silicon ingot casting edge skin material in the second embodiment.The method comprises the following steps:
Step 201: carry out break process to polycrystalline silicon ingot casting edge skin material, obtains the polycrystalline silicon material of target size.
In the present embodiment, adjust the reduction ratio of described jaw crusher, after making described sheet or chunk polysilicon ingot casting edge skin material carry out fragmentation, obtain the granulated polycrystalline silicon material that target size is 20mm ~ 100mm.As preferred value, the mean value of described target size is 60mm.Namely, when to obtain granulated polycrystalline silicon material mean diameter after fragmentation be 60mm, stop broken.In other embodiments, the mean value of described target size also can be 50mm, or 90mm.
Step 202: be positioned over by granulated polycrystalline silicon material in alkaline corrosion liquid, soaks Preset Time.
In the present embodiment, before described granulated polycrystalline silicon material is corroded, first described polycrystalline silicon material is placed in pure water groove and cleans, remove some as the impurity such as mud, dust, then silicon material is placed in described alkaline corrosion solution, and utilize ultrasonic wave or whipping appts to accelerate the corrosion of described granulated polycrystalline silicon material, control the temperature of described alkaline corrosion solution between 58 DEG C ~ 75 DEG C, concrete, can be 70 DEG C, continue the cleaning of described Preset Time.
Described alkaline corrosion liquid is the mixing solutions of alkali and water, the mass percentage concentration of described alkaline corrosion liquid is 0.5%-35%, the surface silicon molecule of described alkaline corrosion liquid and described granulated polycrystalline silicon material is utilized to react, thus the impurity making silicon carbide and silicon nitride etc. be difficult to decompose is peeled off from silicon material, reaches removal of impurity object.As the more excellent embodiment of one, this alkaline corrosion liquid is mixed by alkali lye and water, and wherein alkali lye is sodium hydroxide, and wherein the mass percentage concentration of sodium hydroxide (NaOH) is 0.5%-20%.Concrete, the mass percentage concentration of described sodium hydroxide is 15%, and described Preset Time is 1 hour-3 hours.Described Preset Time is 1.5 hours, is placed in described alkaline corrosion solution reaction 1.5 hours by described granulated polycrystalline silicon material.In other embodiments, the mass percentage concentration of described sodium hydroxide and water can also be 20%-35%; Described alkali lye can also be potassium hydroxide, and described alkali lye can also be the mixed solution of sodium hydroxide and potassium hydroxide, and can also control the temperature of described alkaline corrosion solution between 80 DEG C ~ 90 DEG C, described Preset Time can also be 2 hours-4 hours.
Step 203: by the polycrystalline silicon material pure water rinsing after soaking to solution in neutral.
In the present embodiment, described polycrystalline silicon material is picked up to be placed in drainage trap and rinses, when the surface solution of polycrystalline silicon material is in neutrality, again described polycrystalline silicon material is picked up, be positioned in container.
Step 204: polycrystalline silicon material is dried.
In the present embodiment, be positioned in roasting plant by the described polycrystalline silicon material be positioned in container, arrange storing temperature at 80 DEG C-120 DEG C, baking time, at 24 hours-48 hours, is dried, and is packed by the polycrystalline silicon material after drying, for subsequent use.
The decon method of polycrystalline silicon ingot casting edge skin material provided by the invention, by first carrying out fragmentation to polycrystalline silicon ingot casting edge skin material, obtain granular polycrystalline silicon material, thus make more embedded impurity be exposed to polycrystalline silicon material surface, and then utilize acid solution or alkaline solution to corrode polycrystalline silicon material, make embedded impurity from polycrystalline silicon material sur-face peeling, reach the effect of removing impurity.
Refer to Fig. 3, the decon method of the polycrystalline silicon ingot casting edge skin material of the 3rd embodiment provided by the invention.The method comprising the steps of:
Step 301: carry out break process to polycrystalline silicon ingot casting edge skin material, obtains the polycrystalline silicon material of target size.
In the present embodiment, step 301 is roughly the same with the step 101 in the first embodiment, and the mean value unlike described target size is 5-100mm.As preferred value, the mean value of described target size is 80mm.Namely, when to obtain granulated polycrystalline silicon material mean diameter after fragmentation be 80mm, stop broken.In other embodiments, the mean value of described target size can also be 20mm, or 70mm.
Step 302: be positioned in acid etching solution by the polycrystalline silicon material of target size and soak, removes the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities;
In the present embodiment, step 302 is roughly the same with the step 102 in the first embodiment, gets unlike described acid etching solution hydrofluoric acid, the volumetric concentration nitric acid that is 65%, volumetric concentration be 30% hydrogen peroxide and the pure water that volumetric concentration is 50%.The Preset Time that described polycrystalline silicon material soaks in acid etching solution can be 0.5-3 hour, concrete, can be 2.5 hours.The temperature of described acid etching solution can be 40 DEG C-60 DEG C, concrete, can be 45 DEG C.Utilize described acid etching solution the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities to be peeled off, the purity of polycrystalline silicon material is improved.
Step 303: the polycrystalline silicon material pure water rinsing after being soaked by acid etching solution to solution is neutral;
In the present embodiment, step 303 is identical with the step 103 in the first embodiment, and object washes the acid etching solution on polycrystalline silicon material surface off, so that the recovery of polycrystalline silicon material.
Step 304: the polycrystalline silicon material after flushing is positioned in alkaline corrosion liquid and soaks, remove the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities further.
In the present embodiment, step 304 is roughly the same with the step 202 in the second embodiment, mass percentage concentration unlike described alkaline corrosion liquid is 30%, and wherein alkali lye is potassium hydroxide, and wherein the mass percentage concentration of potassium hydroxide (KOH) is 1%-30%.Concrete, the mass percentage concentration of described sodium hydroxide is 25%, and described Preset Time is 2 hours-4 hours.Described Preset Time is 3.5 hours, is placed in described alkaline corrosion solution reaction 3.5 hours by described granulated polycrystalline silicon material.In other embodiments, the mass percentage concentration of described sodium hydroxide and water can also be 20%-45%; Described alkali lye can also be sodium hydroxide, and described alkali lye can also be the mixed solution of sodium hydroxide and potassium hydroxide, and can also control the temperature of described alkaline corrosion solution between 70 DEG C ~ 85 DEG C, described Preset Time can also be 3 hours-4.5 hours.
Described polycrystalline silicon material eliminates the magazines such as most of silicon carbide, silicon nitride or metal through acid etching solution in step 302, then acid etching solution is washed in step 303, the purity of polycrystalline silicon material increases, then the magazines such as more silicon carbide, silicon nitride or metal are got rid of further across alkaline corrosion liquid, the purity of polycrystalline silicon material is improved closer, to obtain highly purified polycrystalline silicon material, thus improve polycrystalline silicon ingot casting production efficiency.
Step 305: the polycrystalline silicon material pure water rinsing after alkaline corrosion immersion being steeped to solution is neutral.
In the present embodiment, step 305 is identical with the step 203 in the second embodiment, and object washes the alkaline corrosion liquid on polycrystalline silicon material surface off, so that the recovery of polycrystalline silicon material.
Step 306: polycrystalline silicon material is dried.
In the present embodiment, step 306 is identical with the step 104 in the first embodiment, and unlike arranging storing temperature at 150 DEG C-180 DEG C, baking time was at 20 hours-30 hours, and object is dried polycrystalline silicon material, and packaging, stores for future use.
The decon method of polycrystalline silicon ingot casting edge skin material provided by the invention, by first utilizing acid etching solution, granular polycrystalline silicon material is once corroded, after removing silicon carbide, silicon nitride or metallic impurity, polycrystalline silicon material is cleaned, and then utilize alkaline corrosion liquid further to remove impurity to polycrystalline silicon material, make the purity of polycrystalline silicon material higher, effectively improve the efficiency of removing impurity.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.

Claims (10)

1. a decon method for polycrystalline silicon ingot casting edge skin material, is characterized in that, comprise the following steps:
(1) break process is carried out to polycrystalline silicon ingot casting edge skin material, obtain the polycrystalline silicon material of target size;
(2) polycrystalline silicon material of target size is positioned in acid etching solution or alkaline corrosion liquid soaks, remove the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities;
(3) by the polycrystalline silicon material pure water rinsing after soaking to solution in neutral;
(4) polycrystalline silicon material is dried.
2. a decon method for polycrystalline silicon ingot casting edge skin material, is characterized in that, comprise the following steps:
(1) break process is carried out to polycrystalline silicon ingot casting edge skin material, obtain the polycrystalline silicon material of target size;
(2) polycrystalline silicon material of target size is positioned in acid etching solution soaks, remove the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities;
(3) the polycrystalline silicon material pure water rinsing after being soaked by acid etching solution to solution is neutral;
(4) polycrystalline silicon material after rinsing is positioned in alkaline corrosion liquid and soaks, remove the silicon carbide on polycrystalline silicon material surface, silicon nitride or metal impurities further;
(5) the polycrystalline silicon material pure water rinsing after alkaline corrosion immersion being steeped to solution is neutral;
(6) polycrystalline silicon material is dried.
3. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 1 and 2, is characterized in that, the polycrystalline silicon material diameter of described target size is 5mm-100mm.
4. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 1 and 2, is characterized in that, described acid etching solution is the mixing solutions of mixing acid and strong oxidizer.
5. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 4, it is characterized in that, described mixing acid comprises hydrofluoric acid and nitric acid, and mineral acid is or/and organic acid combination, and described mineral acid can be any one or multiple combination of hydrochloric acid, phosphoric acid, sulfuric acid; Described organic acid can be any one or multiple combination of formic acid, acetic acid, propionic acid.
6. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 4, is characterized in that, described strong oxidizer is the oxygenant of Standard Electrode Potentials higher than nitric acid; Or described strong oxidizer is that hydrogen peroxide is or/and the superoxide of Peracetic Acid; Or described strong oxidizer is any one or multiple metal oxide of plumbic oxide, Manganse Dioxide, cobalt dioxide; Or described strong oxidizer is any one or multiple salt of potassium permanganate, potassium bichromate, Potcrate; Or described strong oxidizer is any one or multiple gas of ozone, chlorine, fluorine gas.
7. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 4, it is characterized in that, being configured to of described acid etching solution: get hydrofluoric acid, the volumetric concentration nitric acid that is 60% ~ 80%, volumetric concentration be 25% ~ 45% hydrogen peroxide and the pure water that volumetric concentration is 40% ~ 60%, the volume ratio of each component is hydrofluoric acid: nitric acid: hydrogen peroxide: pure water=1: 1: 1: 2.
8. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 1 and 2, is characterized in that, described alkaline corrosion liquid is that sodium hydroxide is or/and the aqueous solution of potassium hydroxide.
9. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 6, is characterized in that, the mass percentage concentration of described alkaline corrosion liquid is 0.5%-35%.
10. the decon method of polycrystalline silicon ingot casting edge skin material according to claim 1 and 2, it is characterized in that, the described polycrystalline silicon material by target size is positioned in the step in acid etching solution or alkaline corrosion liquid, also comprises the corrosion utilizing ultrasonic wave or whipping appts to accelerate polycrystalline silicon material.
CN201410733691.6A 2014-12-05 2014-12-05 Method for removing impurities from polycrystalline silicon cast ingot leftovers Pending CN104445208A (en)

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Cited By (5)

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CN106000993A (en) * 2016-05-12 2016-10-12 大工(青岛)新能源材料技术研究院有限公司 Pollution-free silicon material crushing and cleaning method
CN106365170A (en) * 2016-08-25 2017-02-01 泗阳瑞泰光伏材料有限公司 Method of removing impurities from silicon ingot circulating material
CN107572533A (en) * 2017-09-07 2018-01-12 晶科能源有限公司 The minimizing technology of impurity in a kind of silicon material flaw-piece
CN111139076A (en) * 2018-11-06 2020-05-12 中国科学院电工研究所 Chemical corrosive liquid and application thereof
CN112547663A (en) * 2020-11-24 2021-03-26 昆山硅瑞自动化设备有限公司 Silicon edge leather cleaning process

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CN102757051A (en) * 2012-04-19 2012-10-31 镇江环太硅科技有限公司 Method for performing recovery treatment on waste layer silicon material

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Publication number Priority date Publication date Assignee Title
CN102757051A (en) * 2012-04-19 2012-10-31 镇江环太硅科技有限公司 Method for performing recovery treatment on waste layer silicon material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106000993A (en) * 2016-05-12 2016-10-12 大工(青岛)新能源材料技术研究院有限公司 Pollution-free silicon material crushing and cleaning method
CN106365170A (en) * 2016-08-25 2017-02-01 泗阳瑞泰光伏材料有限公司 Method of removing impurities from silicon ingot circulating material
CN107572533A (en) * 2017-09-07 2018-01-12 晶科能源有限公司 The minimizing technology of impurity in a kind of silicon material flaw-piece
CN111139076A (en) * 2018-11-06 2020-05-12 中国科学院电工研究所 Chemical corrosive liquid and application thereof
CN111139076B (en) * 2018-11-06 2021-04-16 中国科学院电工研究所 Application of chemical corrosion liquid in texturing of surface of silicon wafer
CN112547663A (en) * 2020-11-24 2021-03-26 昆山硅瑞自动化设备有限公司 Silicon edge leather cleaning process

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