CN102659111B - Method for recovering silicon and silicon carbide from silicon wafer cutting waste mortar - Google Patents
Method for recovering silicon and silicon carbide from silicon wafer cutting waste mortar Download PDFInfo
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- CN102659111B CN102659111B CN201210129869.7A CN201210129869A CN102659111B CN 102659111 B CN102659111 B CN 102659111B CN 201210129869 A CN201210129869 A CN 201210129869A CN 102659111 B CN102659111 B CN 102659111B
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Abstract
The invention discloses a method for recovering silicon and silicon carbide from silicon wafer cutting waste mortar. The method is an energy-saving and environment-friendly process for separating and recovering silicon powder and the silicon carbide from the silicon wafer cutting waste mortar by a method of combining electrophoretic separation and ultrasonic dispersion. The method is low in cost, environment-friendly, energy-saving and good in separation effect. According to the method, electric potentials of the silicon powder and the silicon carbide powder in a suspension are changed by regulating a pH value of the suspension, so that electric potentials of the silicon powder and the silicon carbide powder are in the positive state and negative state respectively; and mutual action among granules is weakened by ultrasonic dispersion to achieve the optimal separation effect. Recovered high-purity micro powder can be used as raw materials for preparing monocrystalline silicon or polycrystalline silicon bars further, and the silicon carbide powder can be prepared into grinding materials which are used for the cutting or other purposes of the silicon bars again.
Description
Technical field
In the waste mortar that the present invention relates to produce a kind of cutting from silicon single crystal or polycrystalline silicon rod or Grinding Process, reclaim the method for silica flour and carborundum powder.
Background technology
In sun power, electron trade, the cutting of silicon chip or ground finish adopt multi-wire saw principle.Machine guide wheel is at the middle drive steel wire that runs up, and the mortar of cutting liquid and silicon carbide abrasive composition is delivered to cutting area, mortar in the running up of steel wire be pressed in silicon single crystal on gauze or polycrystalline silicon rod and recur friction and cut.After cutting, cutting liquid can be taken the silicon carbide abrasive after using out of, simultaneously due to cutting action, can produce a small amount of silica flour and metal fragment, and these a small amount of impurity are also cut liquid simultaneously and take out of, form old sand slurry.Although this mortar can recycle, along with the carrying out of cutting process, silicon bits and the metal-powder of in mortar, sneaking into are more and more, and the diameter of silicon carbide abrasive is more and more less, thereby causes the cutting efficiency of mortar to reduce inefficacy, becomes waste mortar.Waste mortar the inside is generally mixed with 32%～35% polyoxyethylene glycol, 7%～9% silicon powder and 30%～33% silicon carbide micro-powder.If directly enter Sewage treatment systems not only too high being difficult to of COD value process, simultaneously wherein contained a large amount of solid particulates can produce a large amount of mud, cause processing a large amount of waste residues.And silicon is as important photoelectric material, semiconductor material, almost account for 50% of cost.Therefore the silica flour in waste mortar and carborundum powder are reclaimed, be further used for preparing the raw material of silicon single crystal or polysilicon.Not only reduce cost, improved economic benefit; To economizing on resources, protection of the environment has great importance simultaneously.
To the recovery of silicon chip dicing waste mortar, researchist has done a few thing, but still exists a lot of problems not yet to solve.Subject matter is wherein how energy-conservation and environmental protection.Chinese patent 201010140008.X discloses the recovery method of a silicon and silicon carbide.The technique adopting is by after waste mortar pickling, adds distilled water and dispersion agent gum arabic to form suspension, regulates the pH value of suspension to 3-3.5, put into horizontal strip electrophoresis device electrophoretic separation 5-15min, repeatedly, positive pole obtains silica flour in repetitive operation, and negative pole obtains carborundum powder.The electrophoretic separation technique adopting in technique, the dispersiveness of particle in suspension plays an important role to the effect separating, and only adds dispersion agent particle cannot be disperseed completely, and many tiny silicon particles are also attached to silicon-carbide particles surface.When particle moves in horizontal component of electric field, interaction force is large, sterically hindered large, is subject to influence of gravity simultaneously, separates unintelligiblely, and sample classification is collected difficulty, obtains product purity low, need to increase repeated isolation work many times.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the object of the present invention is to provide the recovery method of silicon and silicon carbide in a kind of silicon chip dicing waste mortar of energy-saving and environmental protection.By electrophoretic separation and ultrasonic disperse phase combination, silica flour in silicon chip dicing waste mortar and silicon carbide are carried out to the energy-conserving and environment-protective technique of Separation and Recovery.
Technical scheme: in order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: the recovery method of silicon and silicon carbide in a kind of silicon chip dicing waste mortar, it comprises the following steps:
(1) in silicon chip dicing waste mortar, add viscosity-depression agent, after stirring, carry out solid-liquid separation, obtain mixed solution take polyoxyethylene glycol as main component and the solid particulate take silicon carbide, silicon as main component;
(2) obtained solid particulate is carried out to pickling and remove metal-powder, then repeatedly clean until pH value is 6.5～7 the solid particulate after being washed with distilled water;
(3) in the solid particulate after washing, add distilled water, and add dispersion agent, obtain waste mortar suspension; Wherein the consumption of distilled water is 60%～80% of solid particulate weight after washing, and the consumption of dispersion agent is 0. 10%～0. 40 % of solid particulate weight after washing;
(4) pH value to 2～4 of suspension in regulating step (3), then put into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator, carry out ultrasonic dispersion and electrophoretic separation simultaneously, obtain black anode silicon throw out and light green cathode carbonization siliceous deposits thing;
(5) settling anode and negative electrode being obtained is collected respectively filtration, cleans, dry, obtains respectively silica flour product and carborundum powder product.
The described viscosity-depression agent of step (1) is any in methyl alcohol, ethanol, water.It is whizzer that described solid-liquid separation adopts filtering centrifuge or sedimentation, and the rotating speed of whizzer is 3000～4000r/min, and centrifugation time is 0.5～1h.
Repeatedly until the viscosity of the mixed solution obtaining approaches the viscosity of viscosity-depression agent, polyoxyethylene glycol is fully separated according to the operation of step (1) with silicon, silicon carbide.
Pickling process described in step (2) refers to: adding mass concentration is that 20%～30% acid solution stirs, and solid-to-liquid ratio is 1:0.5～1:3(g/mL), leave standstill 3～5 hours.Described acid solution is any in sulfuric acid, hydrochloric acid, nitric acid, oxalic acid, citric acid.Metal-powder in solid particulate can be removed substantially by step (2), thereby be prevented that metal ion from affecting electrophoresis process, in the final solid reclaiming, heavy metal content can reach quality product requirement simultaneously.Wherein solid-to-liquid ratio refers to the ratio of solid masses and liquid volume, and the unit of solid masses is gram (g), and the unit of liquid volume is milliliter (ml).
Cleaning described in step (2) refers in the solid particulate after pickling and adds distilled water, then carries out sedimentation, finally supernatant liquid is discharged.
Dispersion agent described in step (3) is Xylo-Mucine, one or more in Tetramethylammonium hydroxide, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, triethyl hexyl phosphoric acid, sodium lauryl sulphate, polypropylene phthalein amine.Adopt dispersion agent can reduce the viscosity of suspension, the resistance that particle is subject in electrophoresis process is reduced, separation degree is more abundant.
In step (4), the pH value of the suspension in described regulating step (3) is that the hydrochloric acid that the molar fraction of employing is 0.1mol/L carries out.
Ultrasonic dispersion and electrophoretic separation described in step (4), wherein electrode materials can be any in titanium or graphite, top crown is that anode, bottom crown are negative electrode, the voltage control of D.C. regulated power supply is at 3～10V, ultrasonic power is controlled at 200W～500W, and ultrasonic electrophoresis time is controlled at 10～20min.With this understanding, the electronegative migration of anode upward of silicon particle, the positively charged cathodic migration downwards of carborundum particle; After ultrasonic electrophoresis finishes, observe obvious layering in electrophoresis apparatus, anode deposits color is black, and cathode deposit color is light green.
Beneficial effect: compared with prior art, advantage of the present invention is that cost is low, environmental friendliness, energy efficient, good separating effect.By regulating the pH value of suspension, in change suspension, the electro kinetic potential of silicon and silicon carbide powder makes the electro kinetic potential of two powders in a positive negative state; Carry out ultrasonic dispersion simultaneously and weaken the interaction between particle, to reach best separating effect.The high purity silica powder reclaiming can be further as the raw material of preparing silicon single crystal or polysilicon bar, and silicon carbide powder can be prepared into abrasive material and is reused for the cutting of silicon rod or is used as other purposes.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that reclaims silicon carbide and silicon in a kind of silicon chip dicing waste mortar of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail.
Embodiment 1: utilize the present invention to process silicon chip dicing waste mortar, wherein waste mortar component polyethyleneglycol content 42%, SiC content is that 45%, Si content is 9%, other impurity are 4%.Specifically comprise the following steps, as shown in Figure 1:
(1) in silicon chip dicing waste mortar, add distilled water, after stirring, use filtering centrifuge to carry out centrifugation 0.5 hour, the rotating speed of whizzer is 3000r/min, repetitive operation four times, obtains mixed solution take polyoxyethylene glycol as main component and the solid particulate take silicon carbide, silicon as main component; Wherein mixed solution is on upper strata, and solid particulate is in lower floor;
(2) in obtained solid particulate, adding mass concentration is that 20% salpeter solution is removed metal-powder, and solid-to-liquid ratio is 1:0.5(g/mL), leave standstill 3 hours, then repeatedly clean until pH value is 6.5 the particle after being washed with distilled water;
(3) in the particle after washing, add distilled water, and add Tetramethylammonium hydroxide as dispersion agent, obtain waste mortar suspension; Wherein the consumption of distilled water be washing after solid particulate weight 60%, the consumption of dispersion agent be washing after solid particulate weight 0. 10%;
(4) with the hydrochloric acid of 0.1mol/L, the pH value of the suspension configuring is adjusted to 2.5, puts into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator and carry out electrophoretic separation.Wherein electrode materials is selected graphite.Electrophoresis apparatus top crown is anode, and bottom crown is negative electrode.Regulating the voltage of D.C. regulated power supply is 3V, and ultrasonic power is 400W, and ultrasonic time is 15min.Obtain anode and cathode deposit; With this understanding, the electronegative migration of anode upward of silicon particle, the positively charged cathodic migration downwards of carborundum particle; After ultrasonic electrophoresis finishes, observe obvious layering in electrophoresis apparatus, anode deposits color is black, and cathode deposit color is light green; Wherein anodic deposition thing is silica flour, and cathode deposit is silicon carbide;
(5) anode obtaining and cathode deposit are collected respectively to filtration, anodic deposition thing (silica flour) is cleaned, the dry silica flour product that obtains.Cathode deposit (silicon carbide) cleans, is dried, classification obtains qualified carborundum powder product.Detect through GB 3045-89, the purity of silicon is 98.9%, and silicon carbide purity is 99.3%.
Embodiment 2: utilize the present invention to process silicon chip dicing waste mortar, wherein waste mortar component polyethyleneglycol content 42%, SiC content is that 45%, Si content is 9%, other impurity are 4%.Specifically comprise the following steps:
(1) in silicon chip dicing waste mortar, add methyl alcohol, after stirring, use settling centrifuge to carry out centrifugation 1 hour, the rotating speed of whizzer is 3500r/min, repetitive operation three times, obtains mixed solution take polyoxyethylene glycol as main component and the solid particulate take silicon carbide, silicon as main component.
(2) in obtained solid particulate, adding massfraction is 25% sulphuric acid soln, and solid-to-liquid ratio is 1:1(g/mL), leave standstill 3 hours, then repeatedly clean until pH value is 6.7 the particle after being washed with distilled water.
(3) in the particle after washing, add distilled water, and add Xylo-Mucine as dispersion agent, obtain waste mortar suspension; Wherein the consumption of distilled water be washing after solid particulate weight 60%, the consumption of dispersion agent be washing after solid particulate weight 0. 20%;
(4) with the hydrochloric acid of 0.1mol/L, the pH value of the suspension configuring is adjusted to 3.5, puts into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator and carry out electrophoretic separation.Wherein electrode materials is selected titanium.Electrophoresis apparatus top crown is anode, and bottom crown is negative electrode.Regulating the voltage of D.C. regulated power supply is 5V, and ultrasonic power is 300W, and ultrasonic time is 15min.Obtain anode and cathode deposit;
(5) anode obtaining and cathode deposit are collected respectively to filtration, anodic deposition thing (silica flour) is cleaned, the dry silica flour product that obtains.Cathode deposit (silicon carbide) cleans, is dried, classification obtains qualified carborundum powder product.Detect through GB 3045-89, the purity of silicon is 98.7%, and silicon carbide purity is 99.0%.
Embodiment 3: utilize the present invention to process silicon chip dicing waste mortar, wherein waste mortar component polyethyleneglycol content 42%, SiC content is that 45%, Si content is 9%, other impurity are 4%.Specifically comprise the following steps:
(1) in silicon chip dicing waste mortar, add ethanol, after stirring, use settling centrifuge to carry out centrifugation 0.6 hour, the rotating speed of whizzer is 3500r/min, repetitive operation three times, obtains mixed solution take polyoxyethylene glycol as main component and the solid particulate take silicon carbide, silicon as main component.
(2) in obtained solid particulate, adding massfraction is 30% oxalic acid solution, and solid-to-liquid ratio is 1:2(g/mL), leave standstill 4 hours, then repeatedly clean until pH value is 7 the particle after being washed with distilled water.
(3) in the particle after washing, add distilled water, and add triethyl hexyl phosphoric acid as dispersion agent, obtain waste mortar suspension; Wherein the consumption of distilled water is 70% of solid particulate weight after washing, and the consumption of dispersion agent is 0. 30 % of solid particulate weight after washing;
(4) with the hydrochloric acid of 0.1mol/L, the pH value of the suspension configuring is adjusted to 3, puts into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator and carry out electrophoretic separation.Wherein electrode materials is selected graphite.Electrophoresis apparatus top crown is anode, and bottom crown is negative electrode.Regulating the voltage of D.C. regulated power supply is 6V, and ultrasonic power is 450W, and ultrasonic time is 20min.Obtain anode and cathode deposit;
(5) anode just obtaining and cathode deposit are collected respectively filtration, and anodic deposition thing (silica flour) is cleaned, the dry silica flour product that obtains.Cathode deposit (silicon carbide) cleans, is dried, classification obtains qualified carborundum powder product.Detect through GB 3045-89, the purity of silicon is 99.7%, and silicon carbide purity is 99.5%.
Embodiment 4: utilize the present invention to process silicon chip dicing waste mortar, wherein waste mortar component polyethyleneglycol content 42%, SiC content is that 45%, Si content is 9%, other impurity are 4%.Specifically comprise the following steps:
(1) in silicon chip dicing waste mortar, add distilled water, after stirring, use settling centrifuge to carry out centrifugation 1 hour, the rotating speed of whizzer is 4000r/min, repetitive operation three times, obtains mixed solution take polyoxyethylene glycol as main component and the solid particulate take silicon carbide, silicon as main component.
(2) in obtained solid particulate, adding massfraction is 30% hydrochloric acid soln, and solid-to-liquid ratio is 1:3(g/mL), leave standstill 5 hours, then repeatedly clean until pH value is 7 the particle after being washed with distilled water.
(3) in the particle after washing, add distilled water, and add Tetramethylammonium hydroxide and sodium lauryl sulphate as dispersion agent, obtain waste mortar suspension; Wherein the consumption of distilled water be washing after solid particulate weight 80%, the consumption of dispersion agent be washing after solid particulate weight 0. 30%;
(4) with the hydrochloric acid of 0.1mol/L, the pH value of the suspension configuring is adjusted to 3, puts into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator and carry out electrophoretic separation.Wherein electrode materials is selected titanium.Electrophoresis apparatus top crown is anode, and bottom crown is negative electrode.Regulating the voltage of D.C. regulated power supply is 10V, and ultrasonic power is 500W, and ultrasonic time is 20min.Obtain anode and cathode deposit;
(5) anode obtaining and cathode deposit are collected respectively to filtration, anodic deposition thing (silica flour) is cleaned, the dry silica flour product that obtains.Cathode deposit (silicon carbide) cleans, is dried, classification obtains qualified carborundum powder product.Detect through GB 3045-89, the purity of silicon is 99.9%, and silicon carbide purity is 99.9%.
Embodiment 5: substantially the same manner as Example 1, difference is kind and the consumption of dispersion agent: dispersion agent is any in tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, its consumption is 0. 40 % of the solid particulate weight after washing.
Embodiment 6: substantially the same manner as Example 1, difference is the kind and consumption of dispersion agent: dispersion agent is the mixture that polypropylene phthalein amine, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99 become with any combination, and dispersant dosage is 0. 40 % of the solid particulate weight after washing.
Embodiment 7: substantially the same manner as Example 1, difference is the sour kind in step (2), and acid used is citric acid.
Embodiment 8: substantially the same manner as Example 2, difference is step (4), be specially: the pH value of the suspension configuring is adjusted to 2 with the hydrochloric acid of 0.1mol/L, puts into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator and carry out electrophoretic separation.Wherein electrode materials is selected titanium.Electrophoresis apparatus top crown is anode, and bottom crown is negative electrode.Regulating the voltage of D.C. regulated power supply is 5V, and ultrasonic power is 200W, and ultrasonic time is 10min.Obtain anode and cathode deposit.
Embodiment 9: substantially the same manner as Example 3, difference is step (4), be specially: the pH value of the suspension configuring is adjusted to 4 with the hydrochloric acid of 0.1mol/L, puts into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator and carry out electrophoretic separation.Wherein electrode materials is selected graphite; Electrophoresis apparatus top crown is anode, and bottom crown is negative electrode; Regulating the voltage of D.C. regulated power supply is 8V, and ultrasonic power is 250W, and ultrasonic time is 15min.Obtain anode and cathode deposit.
The above is only the preferred embodiment of the present invention; be noted 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 also should be considered as protection scope of the present invention.
Claims (2)
1. a recovery method for silicon and silicon carbide in silicon chip dicing waste mortar, is characterized in that, it comprises the following steps:
(1) in silicon chip dicing waste mortar, add viscosity-depression agent, described viscosity-depression agent is any in methyl alcohol, ethanol, water, after stirring, adopt filtering centrifuge or settling centrifuge to carry out solid-liquid separation, the rotating speed of whizzer is 3000～4000r/min, centrifugation time is 0.5～1h, obtains mixed solution take polyoxyethylene glycol as main component and the solid particulate take silicon carbide, silicon as main component;
(2) obtained solid particulate is carried out to pickling and remove metal-powder, described pickling process refers to: adding mass concentration is that 20%～30% acid solution stirs, take g/mL solid-to-liquid ratio as 1:0.5～1:3, leave standstill 3～5 hours, described acid solution is any in sulfuric acid, hydrochloric acid, nitric acid, oxalic acid, citric acid, then repeatedly clean with distilled water until pH value is 6.5～7, solid particulate after being washed, described cleaning refers in the solid particulate after pickling and adds distilled water, then carry out sedimentation, finally supernatant liquid is discharged;
(3) in the solid particulate after washing, add distilled water, and add dispersion agent, described dispersion agent is Xylo-Mucine, one or more in Tetramethylammonium hydroxide, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, triethyl hexyl phosphoric acid, sodium lauryl sulphate, polypropylene phthalein amine, obtain waste mortar suspension; Wherein the consumption of distilled water be washing after solid particulate weight 60%～80%, the consumption of dispersion agent be washing after solid particulate weight 0.10%～0.40%;
(4) pH value to 2～4 of suspension in regulating step (3), then put into electrophoresis apparatus until just do not have top crown, and this electrophoresis apparatus is put into ultrasonic decollator, carry out ultrasonic dispersion and electrophoretic separation simultaneously, obtain black anode silicon throw out and light green cathode carbonization siliceous deposits thing, the pH value of the suspension in described regulating step (3) is that the hydrochloric acid that the molar fraction of employing is 0.1mol/L carries out, described ultrasonic dispersion and electrophoretic separation, wherein electrode materials is any in titanium or graphite, top crown is anode, bottom crown is negative electrode, the voltage control of D.C. regulated power supply is at 3～10V, ultrasonic power is controlled at 200W～500W, ultrasonic electrophoresis time is controlled at 10～20min,
(5) settling anode and negative electrode being obtained is collected respectively filtration, cleans, dry, obtains respectively silica flour product and carborundum powder product.
2. according to the recovery method of silicon and silicon carbide in the silicon chip dicing waste mortar described in claims 1, it is characterized in that, according to the operation of step (1) repeatedly until the viscosity of the mixed solution obtaining approaches the viscosity of viscosity-depression agent.
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| CN103172066B (en) * | 2013-02-18 | 2015-05-20 | 江苏双净净化科技有限公司 | Rotational-flow purifying process for silicon carbide powder |
| CN103496831B (en) * | 2013-09-18 | 2015-04-29 | 河南新大新材料股份有限公司 | Recycling method of silicon wafer cutting edge material waste water treatment sludge |
| CN103528874A (en) * | 2013-09-26 | 2014-01-22 | 镇江耐丝新型材料有限公司 | Separating method of carborundum particles on surface of diamond wire |
| CN104437822A (en) * | 2014-11-27 | 2015-03-25 | 河南新大新材料股份有限公司 | C-SiC micro powder separating method |
| CN105084367B (en) * | 2015-08-18 | 2017-03-08 | 北京科技大学 | The method that current potential dispersion microwave acid wash removes polysilicon lines cutting waste material impurity |
| CN106430210A (en) * | 2016-08-31 | 2017-02-22 | 江西恩克新材料股份有限公司 | Method for removing iron and silicon impurities in silicon carbide micropowder for crystalline silicon wire cutting |
| CN109554620A (en) * | 2018-09-30 | 2019-04-02 | 北京金物科技发展有限公司 | A kind of high-carbon-chromium bearing steel and preparation method thereof |
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| CN102161486A (en) * | 2011-02-23 | 2011-08-24 | 天津大学 | Device and method for separating and recovering silicon and silicon carbide in cutting waste mortar of silicon wafers |
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