CN108687029A - A kind of cleaning of silicon material - Google Patents
A kind of cleaning of silicon material Download PDFInfo
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- CN108687029A CN108687029A CN201810488733.2A CN201810488733A CN108687029A CN 108687029 A CN108687029 A CN 108687029A CN 201810488733 A CN201810488733 A CN 201810488733A CN 108687029 A CN108687029 A CN 108687029A
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- silicon material
- cleaning
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- acid
- mass fraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
Abstract
The present invention is a kind of cleaning of silicon material.A kind of cleaning of silicon material, including:(1) pickling:Silicon material is immersed in acid blistering reagent;(2) spray rinsing:Silicon material after pickling is taken out into simultaneously spray rinsing;(3) alkali cleaning:Silicon material after spray rinsing is immersed in alkaline cleaner solution and is cleaned by ultrasonic;(4) it neutralizes:Silicon material after alkali cleaning is immersed in acid acceptor solution and is cleaned by ultrasonic;(5) it is cleaned by ultrasonic:Silicon material after neutralization is immersed in ultra-pure water and is cleaned by ultrasonic;(6) it rinses:Silicon material after ultrasonic cleaning is repeated to impregnate, is rinsed;(7) by the silicon material drying after flushing, packaging.A kind of cleaning of silicon material of the present invention, the discharge of the exhaust gas such as nitrogenfree oxide, use is biodegradable, good environmental protection cleaning agent component, and chemical attack reaction, no silicon material loss does not occur in cleaning process;Also this is simple for process easy to operate, and cleaning yield rate can reach 99.8%, and crystal forming rate can improve 5%.
Description
Technical field
Present invention relates particularly to a kind of cleanings of silicon material.
Background technology
In photovoltaic industry or technical field of semiconductors, when producing silicon chip, butt processing carried out to silicon rod or silicon ingot, remained
Under cry end to end, edge skin material.These occur end to end, due to oxide on surface, surface impurity on edge skin material and in logistics, storage
Impurity intrusion and cutting when the transfer of metal ion, cutting liquid reasons, the surface such as residual can accumulate some dirts.When
These end to end, edge skin material re-use when, need the dirt that will be accumulated thereon to clean up.
Traditional cleaning method is cleaned using sour, is had using nitration mixture (HF and HNO3) cleaning 30-45s;Also use
Strong acid is cleaned, and is neutralized with highly basic after cleaning.It is efficient since sour is simple for process, once by the blueness of people
It looks at, but still has the following disadvantages:1. in etching process, a large amount of acid mist will be generated, acid mist treatment process is complicated, is easy
Safety accident occurs, causes personnel safety accident, it is harmful to the health of people;2. the acid-base waste fluid after silicon material corrosion:Exhaust gas gives up
Liquid emission treatment is of high cost, and a large amount of HF is used when due to sour, and the washings of waste gas containing fluoride are handled with washing method, are discharged into
After environment, the pollution of water body and soil, fluorine-containing flue dust sedimentation or water wash of accepting a surrender can be caused, due to that can not be recycled after its use,
Fluorine-containing material will be directed into inside plants, soil, meadow, water system, soil and groundwater can be made contaminated in animal body etc., right
Our living environment causes most directly to influence;3. acid, caustic corrosion silicon material principle are that silicon material entire surface is made to peel off one layer, deeply
Degree reaches 100-300 μm, and silicon material loss reaches 1-5%, and waste is big.
In view of this, it is necessary to propose that a kind of proportion of goods damageds are low, silicon material cleaning of environmental protection.
Invention content
The purpose of the present invention is to provide a kind of cleaning methods of silicon material, and the cleaning method is easy to operate, weak using weak acid
Alkali is cleaned, and cost is reduced, and the harm of high degree reduced to environment and people has achieved the effect that environmental protection.
To achieve the goals above, used technical solution is:
A kind of cleaning of silicon material, includes the following steps:
(1) pickling:Silicon material is immersed in 25-35min in 25-35 DEG C of acid blistering reagent, obtains the silicon material after pickling;
(2) spray rinsing:Silicon material after pickling is taken out, and spray rinsing 2-3 times, obtains the silicon material after spray rinsing;Institute
It is spray, fast row, rinsing to state spray rinsing;
(3) alkali cleaning:Silicon material after spray rinsing is immersed in the alkaline cleaner solution that mass fraction is 2-4%,
At 30-60 DEG C, it is cleaned by ultrasonic 6-10min, obtains the silicon material after alkali cleaning;
(4) it neutralizes:Silicon material after alkali cleaning is immersed in the acid acceptor solution that mass fraction is 4-6%, in 30-60
At DEG C, it is cleaned by ultrasonic 6-10min, the silicon material after must neutralizing;
(5) it is cleaned by ultrasonic:Silicon material after neutralization is immersed in ultra-pure water, at 30-60 DEG C, is cleaned by ultrasonic 6-10min,
Silicon material after must being cleaned by ultrasonic;
(6) it rinses:Silicon material after ultrasonic cleaning is impregnated, is rinsed, and repeats the operation impregnated, rinsed, until after rinsing
The resistivity of water is not less than 8M Ω cm, the silicon material after must rinsing;
(7) by the silicon material drying after flushing, packaging.
Further, the acid blistering reagent includes:Hydrochloric acid, compound oil displacement agent and water.
Further, the mass fraction of the hydrochloric acid is less than 5%;
The mass fraction of the compound degreaser is less than 11%.
Further, in the step (1), the temperature of the acid blistering reagent is 30 DEG C, soaking time 30min;
In the step (3), the frequency of the ultrasonic cleaning is 35-45Hz;
In the step (4), the frequency of the ultrasonic cleaning is 35-45Hz;
In the step (5), the frequency of the ultrasonic cleaning is 35-45Hz;
In the step (6), immersion, the operation rinsed 3 times is repeated;
In the step (7), the drying temperature is more than 110 DEG C.
Further, in the step (7), the drying is that high-temperature blast is dried.
Further, in the step (1), the silicon material is bulk polycrystal material, end to end material and edge skin material.
Further, in the step (3), the mass fraction of the alkaline cleaner solution is 3%;
In the step (4), the mass fraction of the acid acceptor solution is 5%.
Further, in the step (3), the alkaline cleaner includes:Potassium hydroxide and water, the potassium hydroxide
Mass fraction is less than 5%.
Further, in the step (4), the acid acceptor solution includes:Organic acid, calcium oxide, magnesia, chela
The mixture and water of mixture;The organic acid includes:Acetic acid;
The mass fraction of the acetic acid is less than 10%.
Further, the cleaning further includes step (8) discharging of waste liquid:By step (1), step (3) and step (4)
Waste liquid be neutralized, make its pH value be 6-8 after, can direct emission.
Compared with prior art, the invention has the beneficial effects that:
A kind of cleaning of silicon material of the present invention,
1, the cleaning of a kind of silicon material of the present invention, by optimize cleaning, do not use pollution acid,
Caustic corrosion silicon material reduces cost, and the exhaust gas such as nitrogenfree oxide discharge, the harm of high degree reduced to environment and people,
Environmental protection is achieved the effect that.
2, the cleaning agent component of the cleaning of a kind of silicon material of the present invention, use is biodegradable, environmental-protecting performance
It is good, and chemical attack reaction does not occur in cleaning process, (loss of colliding with is disregarded) is lost in no silicon material.
3, the cleaning of a kind of silicon material of the present invention, which is SEH cleanings, simple to operation, cleaning
Yield rate can reach 99.8%;Crystal forming rate can be promoted to 5%, and cost is greatly lowered.
Specific implementation mode
In order to which the present invention is further explained, a kind of cleaning of silicon material, reaches expected goal of the invention, below in conjunction with preferable
Embodiment, to a kind of cleaning of the silicon material proposed according to the present invention, specific implementation mode, structure, feature and its effect,
It is described in detail as after.In the following description, what different " embodiment " or " embodiment " referred to is not necessarily the same embodiment.This
Outside, special characteristic, structure or the feature in one or more embodiments can be combined by any suitable form.
Before elaborating a kind of cleaning of silicon material of the present invention, it is necessary to the raw material referred in the present invention and side
Method etc. is described further, to reach better effect.
The raw material and equipment used in the embodiment of the present invention are commercially available.
The present invention is cleaned using weak acid and weak base, reduces cost, the danger of high degree reduced to environment and people
Evil, has achieved the effect that environmental protection, and simple for process easy to operate.By optimizing cleaning, pollution is not used
Acid, caustic corrosion silicon material are tested and promote that cleaning agent component is biodegradable, good environmental protection, chemistry does not occur in cleaning process
Corrosion reaction, the SEH cleanings of no silicon material loss (loss of colliding with is disregarded).
SEH cleanings are suitable for semi-automatic cleaning machine and clean normal silicon material, which mainly (removes including bulk polycrystal material
Loose material), material, edge skin material end to end, be not suitable for pot bottom material, pier crucible material, the dirtier silicon material of the exceptions such as loose polycrystal material or surface.
SEH cleanings, main component is weak acid and weak base, in terms of literal meaning, indicates safety (Safety), environmental protection
(Environment), a kind of cleaning of healthy (health).Behind SEH cleaning silicon materials surface, silicon material smooth surface, section
Bright foreign, non-variegation, section brightness is low, a little shades but very uniformly, non-variegation, cleaning yield rate can reach
99.8%;Crystal forming rate can be promoted to 5%.
Metallic atom or ion are acted on the ligand for containing there are two or connecting more than two coordination atoms, and generation has cyclic annular
The complex compound of structure, the complex compound are called chelate.This ligand substance of chelate can be generated chelating agent, also become complexing
Agent, also known as cheland, chelation group (or multidentate ligand).The present invention use be chelating agent mixture, including at least two
The chelating agent of kind, used chelating agent are the chelating agent of routine.
After having understood above-mentioned raw materials and method etc., below in conjunction with specific embodiment to a kind of the clear of silicon material of the present invention
Technique is washed to be further described in detail:
Embodiment 1.
Concrete operation step is as follows:
(1) pickling:Quantitative (flooding silicon material) acid blistering examination is added in ready 1# slots (specified volume) in advance
(the acid blistering reagent includes for agent:Hydrochloric acid, compound oil displacement agent and water;Wherein, the mass fraction of hydrochloric acid is 4%, compound to deoil
The mass fraction of agent is 10%), silicon material to be immersed in 35min in 25 DEG C of acid blistering reagent, obtains the silicon material after pickling;
The silicon material includes mainly bulk polycrystal material (removing loose material), end to end material, edge skin material.
(2) spray rinsing:Silicon material after pickling is fitted into Special tooling clamp (being no more than total volume 2/3rds), it will
It is put into 2# slots, and sprays, arranges soon, rinsing, repeats spray, the fast operation arranged, rinsed 3 times, obtains the silicon material after spray rinsing.
(3) alkali cleaning:Silicon material after spray rinsing is immersed in the 3# for the alkaline cleaner solution for being 2% equipped with mass fraction
In slot, at 60 DEG C, 45Hz, it is cleaned by ultrasonic 6min, obtains the silicon material after alkali cleaning;The alkaline cleaner includes:Potassium hydroxide and
The mass fraction of water, potassium hydroxide is 4%;
(4) it neutralizes:Silicon material after alkali cleaning is immersed in the 4# slots for the acid acceptor solution for being 4% equipped with mass fraction
It is interior, at 60 DEG C, 45Hz, it is cleaned by ultrasonic 6min, the silicon material after must neutralizing;The acid acceptor includes:Acetic acid, calcium oxide,
The mass fraction of magnesia, sodium pyrophosphate, oil base hydroxypropyl sulfonic acid ester, acetic acid and water, acetic acid is less than 10%.
(5) it is cleaned by ultrasonic:Silicon material immersion after neutralization is transferred to the 5# slots equipped with ultra-pure water, in 6# slots successively, 30 DEG C,
Under 45Hz, it is cleaned by ultrasonic 10min, the silicon material after must being cleaned by ultrasonic.
(6) it rinses:Silicon material after ultrasonic cleaning is transferred in Washing basin and impregnates, rinse, and repeats the operation impregnated, rinsed
3 times, it is neutral, water quality resistivity >=8M Ω cm to detect last one of rinsing process pure water with PH meters, confirms that cleaning performance closes
Lattice, the silicon material after must rinsing.
(7) silicon material after flushing is dried by high-temperature blast, drying temperature is more than 110 DEG C, is packed after drying.
(8) discharging of waste liquid:The waste liquid of step (1), step (3) and step (4) is neutralized, it is 6- to make its pH value
It, can direct emission after 8.
Silicon material surface smooth surface, section, section light, evenness, nothing after rather sour etching technique cleans in conventional
Foreign matter, non-variegation, cleaning yield rate reach 98.61%, and average crystal forming rate has reached 81.64%, and cleaning cost is 4.75 yuan/
kg,。
Silicon material surface smooth surface, section light foreign after the present embodiment cleaning, non-variegation, section brightness is low, shades a little
But very uniformly, non-variegation, cleaning yield rate reach 99.4%, improve 1.08%;Average crystal forming rate has reached 83.79%,
Improve 2.15%;Cleaning cost is 1.86 yuan/kg, reduce 2.89 yuan/kg, cost reduction 60.84%.
A kind of cleaning of silicon material described in the embodiment of the present invention has not used pollution by optimizing cleaning
Acid, caustic corrosion silicon material, reduce cost, the exhaust gas such as nitrogenfree oxide discharge, high degree is reduced to environment and people
Harm, has achieved the effect that environmental protection;And the cleaning agent component used is biodegradable, good environmental protection, cleaning process
In chemical attack reaction does not occur, (loss of colliding with is disregarded) is lost in no silicon material;Also the technique is SEH cleanings, simple easy
Operation, cleaning yield rate reach 99.4%;Crystal forming rate improves 2.15%, cost reduction 60.84%.
Embodiment 2.
Concrete operation step is as follows:
(1) pickling:It is (described that quantitative (flooding silicon material) acid blistering reagent is added in ready cleaning PP boxes in advance
Acidity blistering reagent include:Hydrochloric acid, compound oil displacement agent and water;Wherein, the mass fraction of hydrochloric acid is 4%, the matter of compound degreaser
It is 10%), silicon material to be immersed in 25min in 35 DEG C of acid blistering reagent, obtains the silicon material after pickling to measure score;
The silicon material includes mainly bulk polycrystal material (removing loose material), end to end material, edge skin material.
(2) spray rinsing:Silicon material after pickling is fitted into Special tooling clamp (being no more than total volume 2/3rds), it will
It is put into 2# slots, and sprays, arranges soon, rinsing, repeats spray, the fast operation arranged, rinsed 2 times, obtains the silicon material after spray rinsing.
(3) alkali cleaning:Silicon material after spray rinsing is immersed in the 3# for the alkaline cleaner solution for being 4% equipped with mass fraction
In slot, at 30 DEG C, 35Hz, it is cleaned by ultrasonic 10min, obtains the silicon material after alkali cleaning;The alkaline cleaner includes:Potassium hydroxide and
The mass fraction of water, potassium hydroxide is 4%;
(4) it neutralizes:Silicon material after alkali cleaning is immersed in the 4# slots for the acid acceptor solution for being 6% equipped with mass fraction
It is interior, at 30 DEG C, 35Hz, it is cleaned by ultrasonic 10min, the silicon material after must neutralizing;The acid acceptor includes:Succinic acid, oxidation
The mass fraction of calcium, magnesia, the mixture of chelating agent, acetic acid and water, acetic acid is 9%.
(5) it is cleaned by ultrasonic:Silicon material immersion after neutralization is transferred to the 5# slots equipped with ultra-pure water, in 6# slots successively, 60 DEG C,
Under 35Hz, it is cleaned by ultrasonic 6min, the silicon material after must being cleaned by ultrasonic.
(6) it rinses:Silicon material after ultrasonic cleaning is transferred in Washing basin and impregnates, rinse, and repeats the operation impregnated, rinsed
3 times, it is neutral, water quality resistivity >=8M Ω cm to detect last one of rinsing process pure water with PH meters, confirms that cleaning performance closes
Lattice, the silicon material after must rinsing.
(7) silicon material after flushing is dried by high-temperature blast, drying temperature is 120 DEG C, then is packed.
(8) discharging of waste liquid:The waste liquid of step (1), step (3) and step (4) is neutralized, it is 6- to make its pH value
It, can direct emission after 8.
Silicon material surface smooth surface, section, section light, evenness, nothing after rather sour etching technique cleans in conventional
Foreign matter, non-variegation, cleaning yield rate reach 98.61%, and average crystal forming rate has reached 81.64%, and cleaning cost is 4.75 yuan/
kg,。
Silicon material surface smooth surface, section light foreign after the present embodiment cleaning, non-variegation, section brightness is low, shades a little
But very uniformly, non-variegation, cleaning yield rate reach 99.3%, improve 1.08%;Average crystal forming rate has reached 84.12%,
Improve 2.48%;Cleaning cost is 1.81 yuan/kg, reduce 2.94 yuan/kg, cost reduction 61.89%.
A kind of cleaning of silicon material described in the embodiment of the present invention has not used pollution by optimizing cleaning
Acid, caustic corrosion silicon material, reduce cost, the exhaust gas such as nitrogenfree oxide discharge, high degree is reduced to environment and people
Harm, has achieved the effect that environmental protection;And the cleaning agent component used is biodegradable, good environmental protection, cleaning process
In chemical attack reaction does not occur, (loss of colliding with is disregarded) is lost in no silicon material;Also the technique is SEH cleanings, simple easy
Operation, cleaning yield rate reach 99.3%;Crystal forming rate improves 2.48%, cost reduction 61.89%.
Embodiment 3.
Concrete operation step is as follows:
(1) pickling:Quantitative (flooding silicon material) acid blistering examination is added in ready 1# slots (specified volume) in advance
(the acid blistering reagent includes for agent:Hydrochloric acid, compound oil displacement agent and water;Wherein, the mass fraction of hydrochloric acid is 3%, compound to deoil
The mass fraction of agent is 10%), silicon material to be immersed in 30min in 30 DEG C of acid blistering reagent, obtains the silicon material after pickling;
The silicon material includes mainly bulk polycrystal material (removing loose material), end to end material, edge skin material.
(2) spray rinsing:Silicon material after pickling is fitted into Special tooling clamp (being no more than total volume 2/3rds), it will
It is put into 2# slots, and sprays, arranges soon, rinsing, repeats spray, the fast operation arranged, rinsed 3 times, obtains the silicon material after spray rinsing.
(3) alkali cleaning:Silicon material after spray rinsing is immersed in the 3# for the alkaline cleaner solution for being 3% equipped with mass fraction
In slot, at 50 DEG C, 40Hz, it is cleaned by ultrasonic 8min, obtains the silicon material after alkali cleaning;The alkaline cleaner includes:Potassium hydroxide and
The mass fraction of water, potassium hydroxide is 4%;
(4) it neutralizes:Silicon material after alkali cleaning is immersed in the 4# slots for the acid acceptor solution for being 5% equipped with mass fraction
It is interior, at 45 DEG C, 40Hz, it is cleaned by ultrasonic 8min, the silicon material after must neutralizing;The acid acceptor includes:Ethanedioic acid, oxidation
The mass fraction of calcium, magnesia, the mixture of chelating agent, acetic acid and water, acetic acid is 8%.
(5) it is cleaned by ultrasonic:Silicon material immersion after neutralization is transferred to the 5# slots equipped with ultra-pure water, in 6# slots successively, 50 DEG C,
Under 40Hz, it is cleaned by ultrasonic 8min, the silicon material after must being cleaned by ultrasonic.
(6) it rinses:Silicon material after ultrasonic cleaning is transferred in Washing basin and impregnates, rinse, and repeats the operation impregnated, rinsed
3 times, it is neutral, water quality resistivity >=8M Ω cm to detect last one of rinsing process pure water with PH meters, confirms that cleaning performance closes
Lattice, the silicon material after must rinsing.
(7) silicon material after flushing is dried by high-temperature blast, drying temperature is 130 DEG C, packaging.
(8) discharging of waste liquid:The waste liquid of step (1), step (3) and step (4) is neutralized, it is 6- to make its pH value
It, can direct emission after 8.
Silicon material surface smooth surface, section, section light, evenness, nothing after rather sour etching technique cleans in conventional
Foreign matter, non-variegation, cleaning yield rate reach 98.61%, and average crystal forming rate has reached 81.64%, and cleaning cost is 4.75 yuan/
kg,。
Silicon material surface smooth surface, section light foreign after the present embodiment cleaning, non-variegation, section brightness is low, shades a little
But very uniformly, non-variegation, cleaning yield rate reach 99.8%, improve 1.08%;Average crystal forming rate has reached 86.72%,
Improve 5.08%;Cleaning cost is 1.61 yuan/kg, reduce 3.14 yuan/kg, cost reduction 66.11%.
A kind of cleaning of silicon material described in the embodiment of the present invention has not used pollution by optimizing cleaning
Acid, caustic corrosion silicon material, reduce cost, the exhaust gas such as nitrogenfree oxide discharge, high degree is reduced to environment and people
Harm, has achieved the effect that environmental protection;And the cleaning agent component used is biodegradable, good environmental protection, cleaning process
In chemical attack reaction does not occur, (loss of colliding with is disregarded) is lost in no silicon material;Also the technique is SEH cleanings, simple easy
Operation, cleaning yield rate reach 99.8%;Crystal forming rate improves 5.08%, cost reduction 66.11%.
Embodiment 4.
Concrete operation step is as follows:
(1) pickling:Quantitative (flooding silicon material) acid blistering examination is added in ready 1# slots (specified volume) in advance
(the acid blistering reagent includes for agent:Hydrochloric acid, compound oil displacement agent and water;Wherein, the mass fraction of hydrochloric acid is 3%, compound to deoil
The mass fraction of agent is 10%), silicon material to be immersed in 32min in 28 DEG C of acid blistering reagent, obtains the silicon material after pickling;
The silicon material includes mainly bulk polycrystal material (removing loose material), end to end material, edge skin material.
(2) spray rinsing:Silicon material after pickling is fitted into Special tooling clamp (being no more than total volume 2/3rds), it will
It is put into 2# slots, and sprays, arranges soon, rinsing, repeats spray, the fast operation arranged, rinsed 3 times, obtains the silicon material after spray rinsing.
(3) alkali cleaning:Silicon material after spray rinsing is immersed in the 3# for the alkaline cleaner solution for being 3% equipped with mass fraction
In slot, at 40 DEG C, 45Hz, it is cleaned by ultrasonic 7min, obtains the silicon material after alkali cleaning;The alkaline cleaner includes:Potassium hydroxide and
The mass fraction of water, potassium hydroxide is 3%;
(4) it neutralizes:Silicon material after alkali cleaning is immersed in the 4# slots for the acid acceptor solution for being 5% equipped with mass fraction
It is interior, at 50 DEG C, 45Hz, it is cleaned by ultrasonic 7min, the silicon material after must neutralizing;The acid acceptor includes:Formic acid, calcium oxide,
The mass fraction of magnesia, the mixture of chelating agent, acetic acid and water, acetic acid is 9%.
(5) it is cleaned by ultrasonic:Silicon material immersion after neutralization is transferred to the 5# slots equipped with ultra-pure water, in 6# slots successively, 40 DEG C,
Under 45Hz, it is cleaned by ultrasonic 10min, the silicon material after must being cleaned by ultrasonic.
(6) it rinses:Silicon material after ultrasonic cleaning is transferred in Washing basin and impregnates, rinse, and repeats the operation impregnated, rinsed
3 times, it is neutral, water quality resistivity >=8M Ω cm to detect last one of rinsing process pure water with PH meters, confirms that cleaning performance closes
Lattice, the silicon material after must rinsing.
(7) silicon material after flushing is dried by high-temperature blast, drying temperature is more than 110 DEG C, packaging.
(8) discharging of waste liquid:The waste liquid of step (1), step (3) and step (4) is neutralized, it is 6- to make its pH value
It, can direct emission after 8.
Silicon material surface smooth surface, section, section light, evenness, nothing after rather sour etching technique cleans in conventional
Foreign matter, non-variegation, cleaning yield rate reach 98.61%, and average crystal forming rate has reached 81.64%, and cleaning cost is 4.75 yuan/
kg,。
Silicon material surface smooth surface, section light foreign after the present embodiment cleaning, non-variegation, section brightness is low, shades a little
But very uniformly, non-variegation, cleaning yield rate reach 99.6%, improve 1.08%;Average crystal forming rate has reached 85.25%,
Improve 3.61%;Cleaning cost is 1.74 yuan/kg, reduce 3.01 yuan/kg, cost reduction 63.37%.
A kind of cleaning of silicon material described in the embodiment of the present invention has not used pollution by optimizing cleaning
Acid, caustic corrosion silicon material, reduce cost, the exhaust gas such as nitrogenfree oxide discharge, high degree is reduced to environment and people
Harm, has achieved the effect that environmental protection;And the cleaning agent component used is biodegradable, good environmental protection, cleaning process
In chemical attack reaction does not occur, (loss of colliding with is disregarded) is lost in no silicon material;Also the technique is SEH cleanings, simple easy
Operation, cleaning yield rate reach 99.6%;Crystal forming rate improves 3.61%, cost reduction 63.37%.
Embodiment 5.
Concrete operation step is as follows:
(1) pickling:Quantitative (flooding silicon material) acid blistering examination is added in ready 1# slots (specified volume) in advance
(the acid blistering reagent includes for agent:Hydrochloric acid, compound oil displacement agent and water;Wherein, the mass fraction of hydrochloric acid is 4%, compound to deoil
The mass fraction of agent is 10%), silicon material to be immersed in 30min in 35 DEG C of acid blistering reagent, obtains the silicon material after pickling;
The silicon material includes mainly bulk polycrystal material (removing loose material), end to end material, edge skin material.
(2) spray rinsing:Silicon material after pickling is fitted into Special tooling clamp (being no more than total volume 2/3rds), it will
It is put into 2# slots, and sprays, arranges soon, rinsing, repeats spray, the fast operation arranged, rinsed 2 times, obtains the silicon material after spray rinsing.
(3) alkali cleaning:Silicon material after spray rinsing is immersed in the 3# for the alkaline cleaner solution for being 3% equipped with mass fraction
In slot, at 50 DEG C, 45Hz, it is cleaned by ultrasonic 10min, obtains the silicon material after alkali cleaning;The alkaline cleaner includes:Potassium hydroxide and
The mass fraction of water, potassium hydroxide is 3%;
(4) it neutralizes:Silicon material after alkali cleaning is immersed in the 4# slots for the acid acceptor solution for being 5% equipped with mass fraction
It is interior, at 60 DEG C, 45Hz, it is cleaned by ultrasonic 10min, the silicon material after must neutralizing;The acid acceptor includes:Organic acid, oxidation
The mass fraction of calcium, magnesia, the mixture of chelating agent, acetic acid and water, acetic acid is 6%.
(5) it is cleaned by ultrasonic:Silicon material immersion after neutralization is transferred to the 5# slots equipped with ultra-pure water, in 6# slots successively, 60 DEG C,
Under 45Hz, it is cleaned by ultrasonic 6min, the silicon material after must being cleaned by ultrasonic.
(6) it rinses:Silicon material after ultrasonic cleaning is transferred in Washing basin and impregnates, rinse, and repeats the operation impregnated, rinsed
3 times, it is neutral, water quality resistivity >=8M Ω cm to detect last one of rinsing process pure water with PH meters, confirms that cleaning performance closes
Lattice, the silicon material after must rinsing.
(7) silicon material after flushing is dried by high-temperature blast, drying temperature is more than 110 DEG C, packaging.
(8) discharging of waste liquid:The waste liquid of step (1), step (3) and step (4) is neutralized, it is 6- to make its pH value
It, can direct emission after 8.
Silicon material surface smooth surface, section, section light, evenness, nothing after rather sour etching technique cleans in conventional
Foreign matter, non-variegation, cleaning yield rate reach 98.61%, and average crystal forming rate has reached 81.64%, and cleaning cost is 4.75 yuan/
kg,。
Silicon material surface smooth surface, section light foreign after the present embodiment cleaning, non-variegation, section brightness is low, shades a little
But very uniformly, non-variegation, cleaning yield rate reach 99.8%, improve 1.08%;Average crystal forming rate has reached 83.63%,
Improve 1.99%;Cleaning cost is 1.88 yuan/kg, reduce 2.87 yuan/kg, cost reduction 60.42%.
A kind of cleaning of silicon material described in the embodiment of the present invention has not used pollution by optimizing cleaning
Acid, caustic corrosion silicon material, reduce cost, the exhaust gas such as nitrogenfree oxide discharge, high degree is reduced to environment and people
Harm, has achieved the effect that environmental protection;And the cleaning agent component used is biodegradable, good environmental protection, cleaning process
In chemical attack reaction does not occur, (loss of colliding with is disregarded) is lost in no silicon material;Also the technique is SEH cleanings, simple easy
Operation, cleaning yield rate reach 99.8%;Crystal forming rate improves 1.99%, cost reduction 60.42%.
The above is only the preferred embodiment of the embodiment of the present invention, not makees any shape to the embodiment of the present invention
Limitation in formula, the technical spirit of embodiment is to any simple modification, equivalent variations made by above example according to the present invention
With modification, in the range of still falling within technical solution of the embodiment of the present invention.
Claims (10)
1. a kind of cleaning of silicon material, which is characterized in that include the following steps:
(1) pickling:Silicon material is immersed in 25-35min in 25-35 DEG C of acid blistering reagent, obtains the silicon material after pickling;
(2) spray rinsing:Silicon material after pickling is taken out, and spray rinsing 2-3 times, obtains the silicon material after spray rinsing;The spray
Leaching rinsing is spray, fast row, rinsing;
(3) alkali cleaning:Silicon material after spray rinsing is immersed in the alkaline cleaner solution that mass fraction is 2-4%, in 30-60
At DEG C, it is cleaned by ultrasonic 6-10min, obtains the silicon material after alkali cleaning;
(4) it neutralizes:Silicon material after alkali cleaning is immersed in the acid acceptor solution that mass fraction is 4-6%, at 30-60 DEG C
Under, it is cleaned by ultrasonic 6-10min, the silicon material after must neutralizing;
(5) it is cleaned by ultrasonic:Silicon material after neutralization is immersed in ultra-pure water, at 30-60 DEG C, is cleaned by ultrasonic 6-10min, obtains super
Silicon material after sound cleaning;
(6) it rinses:Silicon material after ultrasonic cleaning is impregnated, is rinsed, and repeats the operation impregnated, rinsed, until the water after rinsing
Resistivity is not less than 8M Ω cm, the silicon material after must rinsing;
(7) by the silicon material drying after flushing, packaging.
2. cleaning according to claim 1, which is characterized in that wherein,
The acid blistering reagent includes:Hydrochloric acid, compound oil displacement agent and water.
3. cleaning according to claim 2, which is characterized in that wherein,
The mass fraction of the hydrochloric acid is less than 5%;
The mass fraction of the compound degreaser is less than 11%.
4. cleaning according to claim 1, which is characterized in that wherein,
In the step (1), the temperature of the acid blistering reagent is 30 DEG C, soaking time 30min;
In the step (3), the frequency of the ultrasonic cleaning is 35-45Hz;
In the step (4), the frequency of the ultrasonic cleaning is 35-45Hz;
In the step (5), the frequency of the ultrasonic cleaning is 35-45Hz;
In the step (6), immersion, the operation rinsed 3 times is repeated;
In the step (7), the drying temperature is more than 110 DEG C.
5. cleaning according to claim 4, which is characterized in that wherein,
In the step (7), the drying is that high-temperature blast is dried.
6. cleaning according to claim 1, which is characterized in that wherein,
In the step (1), the silicon material is bulk polycrystal material, end to end material and edge skin material.
7. cleaning according to claim 1, which is characterized in that wherein,
In the step (3), the mass fraction of the alkaline cleaner solution is 3%;
In the step (4), the mass fraction of the acid acceptor solution is 5%.
8. cleaning according to claim 1, which is characterized in that wherein,
In the step (3), the alkaline cleaner includes:The mass fraction of potassium hydroxide and water, the potassium hydroxide is less than
5%.
9. cleaning according to claim 1, which is characterized in that wherein,
In the step (4), the acid acceptor solution includes:The mixture of organic acid, calcium oxide, magnesia, chelating agent
And water;The organic acid includes:Acetic acid;
The mass fraction of the acetic acid is less than 10%.
10. cleaning according to claim 1, which is characterized in that wherein,
The cleaning further includes step (8) discharging of waste liquid:During the waste liquid of step (1), step (3) and step (4) is carried out
And processing can direct emission after making its pH value be 6-8.
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| CN109848122A (en) * | 2018-12-29 | 2019-06-07 | 晶能光电（江西）有限公司 | The cleaning method of SiC panel surface AlN film layer |
| CN109950137A (en) * | 2019-04-11 | 2019-06-28 | 江苏美科硅能源有限公司 | One kind is for handling cutting belt adhesive tape fragment material processing method |
| CN110773507A (en) * | 2019-11-06 | 2020-02-11 | 张旭松 | Crystal cleaning method for improving surface smoothness of crystal |
| CN111921945A (en) * | 2020-07-14 | 2020-11-13 | 海盐得胜化工设备有限公司 | Cleaning process for polycrystalline silicon structured packing |
| CN112620233A (en) * | 2020-12-23 | 2021-04-09 | 孟闯 | Cleaning method of sheet degumming agent |
| CN112725904A (en) * | 2020-12-09 | 2021-04-30 | 天通银厦新材料有限公司 | Method for recycling leftover material crystal shell material of sapphire crystal |
| CN113857140A (en) * | 2021-09-30 | 2021-12-31 | 安徽微芯长江半导体材料有限公司 | Method for cleaning silicon carbide wafer subjected to multi-wire cutting |
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| CN111921945A (en) * | 2020-07-14 | 2020-11-13 | 海盐得胜化工设备有限公司 | Cleaning process for polycrystalline silicon structured packing |
| CN112725904A (en) * | 2020-12-09 | 2021-04-30 | 天通银厦新材料有限公司 | Method for recycling leftover material crystal shell material of sapphire crystal |
| CN112620233A (en) * | 2020-12-23 | 2021-04-09 | 孟闯 | Cleaning method of sheet degumming agent |
| CN113857140A (en) * | 2021-09-30 | 2021-12-31 | 安徽微芯长江半导体材料有限公司 | Method for cleaning silicon carbide wafer subjected to multi-wire cutting |
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