CN102583406A - Purifying method for high-purity silica sol - Google Patents
Purifying method for high-purity silica sol Download PDFInfo
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- CN102583406A CN102583406A CN2012100181455A CN201210018145A CN102583406A CN 102583406 A CN102583406 A CN 102583406A CN 2012100181455 A CN2012100181455 A CN 2012100181455A CN 201210018145 A CN201210018145 A CN 201210018145A CN 102583406 A CN102583406 A CN 102583406A
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Abstract
The invention discloses a purifying method of a high-purity silica gel, belonging to the technical field of chemical-mechanical polishing. The purifying method is suitable for purifying silica sol in the chemical-mechanical polishing of a super-large-scale integrated circuit. The purifying method comprises the following steps: uniformly mixing regenerated strong acid cation exchange resin with strong base type anion exchange resin; adding silica sol to be purified in a container filled with strong acid and strong base mixed resin and controlling the temperature, stirring to enable the silica sol to be purified and the strong acid and strong base mixed resin to be mixed uniformly and realizing dynamic purification; and adding a composite chelating agent and a flocculating agent in the dynamic purifying process of the silica sol and controlling the pH value to 1-5 to obtain the purified silica sol. The content of metal ions in the purified silica sol is reduced to ppb level; and the obtained high-purity silica sol can meet the requirement of a substrate or a chip polishing solution for new generation of line width on the purity of the silica sol.
Description
Technical field
The invention belongs to the chemical Mechanical Polishing Technique field, particularly a kind of purification process of high-purity silicasol.
Background technology
Development along with large-scale integrated circuit; Novel micro-fabrication technology and equipment continue to bring out and perfect; Semicon industry is developing rapidly according to " Moore's Law " always, and promptly on the IC wafer of a slice same size, the number of transistors of being held can every two years double; In recent years; Development of integrated circuits mainly contains three characteristics: 1. characteristic dimension granular, characteristic dimension are being challenged the limit of silicon-base plane technology along 0.25um, 0.18um, 0.13um, 0.09um, 0.045um development; 2. silicon single crystal flake ever-larger diameters, the main IC major company in the whole world has all got into the Φ 300um stage, and Φ 450 is also in the middle of continuous development; 3. along with the continuous granular of characteristic dimension, single chip integration has reached 10
8-10
9, developed into the System on Chip/SoC stage now.
Along with the progress of integrated circuit technique, large-scale integrated circuit is constantly to more fine rule is wide, and more highdensity direction develops.Pollutent is outstanding further to the influence of device; Mainly comprise microparticle, chemical substance and bacterium; These pollutents are present in device surface with the form of atom, ion, molecule, particle or the film mode through chemistry or physical adsorption usually; Influence the electroconductibility of device surface, the integrity and the stability parameter of oxide compound, cause device performance to descend, yield rate reduces.These pollutents mainly come from the used silicon sol of configuration polishing fluid, and silicon sol is the suspension dispersion liquid of silica dioxide granule in water, is the staple in the polished semiconductor liquid, is consumptive material indispensable in the microelectronics industry.Because the pollution to silicon chip mainly comes from silicon sol in polishing process, reduce then that the content of metals ion seems most important in the silicon sol, the existing many pieces of patent reports of the method for the silicon sol of preparation low metal ion level.
Patent CN100586851C with organosilane that can rectification and purification as raw material; It is dissolved in mineral acid (alkali) or organic acid (alkali) makes acidic silicic acid (alkalescence siliceous (or not siliceous)) solution; With siliceous or not siliceous solution the thermotonus 105 degree below of acidic silicate solution, be prepared into silicon sol with alkalescence.Discharge sub product and a part of water such as methanol at last through the mode of heating.Have ultra-pure (metal ion content is less than 1ppm), alkali resistance and can be concentrated into the characteristics of high density.But this method raw material is more expensive, cost higher (raw material availability is less than 30%), and the ethanol or the methyl alcohol that add thermogenesis have pollution to environment.In addition, though the silicon sol purity of this method preparation is higher, silicon sol interior also residual have part ammonia and alcohol have a negative impact in chip polishing of new generation.
Patent CN101585541B is raw material with the silica flour; Preparation high-purity silicasol under catalytic condition; Select particle diameter through the particle diameter selector switch then, spent ion exchange resin, remove impurity, add stablizer at last and make electronic-grade silica sol through control exchange flow velocity.Because this method only adopts simple ion exchange resin that silicon sol is carried out purifying, it removes the limited in one's ability of metals ion, and efficient is not high.
Patent CN101070161B discloses that a kind of particle is tiny, the preparation method of the high reactivity silicon sol of narrow diameter distribution.It is characterized in that with the sodium silicate solution being raw material; Make active silicic acid solution after adopting improved ion exchange method to remove sodium ion; Through control active silicic acid solution proportion, pH value in reaction and Heating temperature; Prepare silicon sol, through the ultra-filtration membrane osmosis, prepare the high reactivity silicon sol at last by the superfine silicon dioxide granulometric composition.Have that particle is little, even particle size distribution, dehydration and purifying carries out synchronously, advantage of low energy consumption.But this method complex steps, preparation efficiency are not high, are not suitable for the industriallization continuous production.
Patent CN101475180 discloses a kind of purification process of ultra-pure silicon dioxide sol; Make silicon sol to be purified successively adverse current process strong-acid type cation exchange bed and strong base anion exchange bed; After adding sequestrant; Another mistake stream obtains ultra-pure silicasol through strong acid and strong base type ion exchange resin mixed bed.This method efficient is higher, and the content of some metals ions can be reduced to the ppb level in the silicon sol behind the purifying, but for Au
+, Ag
+, Pd
2+, Cu
2+And Pb
2+Also can't reduce and cause the ppb level.
In addition, the disclosed silicon sol purification process of patent CN101475180 must load into ion exchange column with ion exchange resin earlier, makes the silicon sol adverse current through ion exchange column then, under static state, realizes the purifying of silicon sol.Though the existing very quantum jump of this method, technology is simpler, and industrialization efficient is higher, needs to optimize.
In order to make the silicon sol behind the purifying be applicable to that more the IC industry to the raw material requirement of high purity, makes Au
+, Ag
+, Pd
2+, Cu
2+, Pb
2+Cause the ppb level Deng the metals ion reduction, more adapt to the continuous production of industrialization simultaneously, make industrialization process simple, operation efficiency is high, and this patent has proposed better purifying process route.
Summary of the invention
The invention discloses a kind of purification process that is applicable to the high-purity silicasol of VLSI chemically machinery polished, the method for metal ion content in a kind of effective reduction high-purity silicasol is provided.
The purification process of a kind of high-purity silicasol provided by the invention is characterized in that, this method steps is following:
(1) strongly acidic cation-exchange and strong basic type anion-exchange resin are carried out manipulation of regeneration respectively;
(2) will regenerate good strongly acidic cation-exchange and strong basic type anion-exchange resin proportional mixing gets the strong acid and strong base hybrid resin, and packs into and have in the container of cooling, heating and stirring;
(3) join in the container that the strong acid and strong base hybrid resin is housed silicon sol to be purified and controlled temperature, the weight ratio of strong acid and strong base hybrid resin and silicon sol is 1: (1～100);
(4) open whipping appts in the container, stir, silicon sol to be purified and strong acid and strong base hybrid resin are mixed;
(5) carry out in the process adding composite chelate agent and flocculation agent at step (4) dynamic purification, control pH is 1～5, obtains the silicon sol behind the purifying;
Said composite chelate agent comprises main sequestering agent and auxiliary sequestrant;
Said main sequestering agent is for containing the sequestrant of dithiocarbamic acid (DTC) group;
Said auxiliary sequestrant is polyethylene imine based xanthogenic acid, starch xanthate, epoxy polyamine chloropropane multipolymer xanthogenate, SEPIGEL 305 xanthogenate, trithio tricyanic acid, YD 30; Nitrilotriacetic acid (claiming NTA again), one or more in diethylene triaminepentaacetic acid(DTPA) and salt thereof, Hydrocerol A, tartrate and glucono-, hydroxyethylethylene diamine tri-acetic acid, bicine N-, polymethyl acrylic acid, HPMA, fumaric acid (FUMARIC ACID TECH GRADE)-propene sulfonic acid interpolymer, ethylenediamine tetraacetic ethylidene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, Diethylenetriamine five ethylidene phosphonic acids, Diethylenetriamine pentamethylene phosphonic acids, three second tetramines, six ethylidene phosphonic acids, tn four ethylidene phosphonic acids, the tn tetramethylene phosphonic acid;
Said flocculation agent is a kind of in SEPIGEL 305, ROHM, Vinylpyrrolidone polymer, Z 150PH, the polyoxyethylene.
Dithiocarbamic acid (DTC) unit structure formula is:
Said main sequestering agent is for containing in ammonium, sodium or the sylvite of dithiocarbamic acid (DTC) group one or more.
The said sequestrant that contains dithiocarbamic acid (DTC) group is dimethyl dithiocarbamate, N,N-Diethyldithiocarbamic Acid, dibutyl dithiocaarbamate salt, dibenzyl aminodithioformic acid salt, dioctyl MGD, double hydroxyethyl MGD, the two dithio formates of triethylene tetramine, polyamines dithio formate, 1; 3, one or more in the 5-Hexahydrotriazine dithio formate.
In the said high-purity silicasol, silica concentration is 1～50wt%, and particle diameter is 1～300nm, and the positively charged ion total amount is 200～5000ppm.
Strongly acidic cation-exchange and strong basic type anion-exchange resin volume ratio are (0.1～10) in the said strong acid and strong base hybrid resin: 1.
Said composite chelate agent addition be in the silicon sol silicon-dioxide quality 0.01～5%.Wherein, the main sequestering agent addition is preferably 0.3%～2% of silicon-dioxide quality, and auxiliary sequestrant addition is preferably 0.1%～1.5% of silicon-dioxide quality.
Said flocculation agent addition be in the silicon sol silicon-dioxide quality 0.02%～0.08%.
In the step (3), controlled temperature is at 0～60 ℃.
In the step (4), can stir 10～30min.
The technique effect that the present invention reaches is:
The present invention is according to the double electrical layers principle of the exchange mechanism and the silicon dioxide gel itself of ion exchange resin; Used sun-the moon to mix the method for dynamic exchange; Be equivalent to form the process of numerous sun-anionresin; Ion in feasible " fixed layer " forms so continuous round-robin process, thereby the metals ion in the silicon sol is effectively removed constantly to external migration, exchange.
The composite chelate agent that the present invention adopts; The single sequestrant that its sequestering power is superior to using always (YD 30, nitrilotriacetic acid); The sequestrant through containing the DTC group and the acting in conjunction of auxiliary sequestrant; Make the water soluble characteristic of composite chelate agent better, the deposition flco that generates when reacting with metal-chelating is big, settling property good, and metals ion is effectively separated from matrix; Though and like sequestrant commonly used such can with metal ion-chelant, the inner complex that forms is because water soluble and can not make metals ion in the matrix obtain essence to reduce.Metal ion content through in the back silicon sol of purifying has been reduced to the ppb level, the gained high-purity silicasol applicable to live width substrate for use of new generation or chip polishing fluid for the silicon sol purity requirement.
The present invention develops on the CN101475180 basis, has adopted positive negatively charged ion hybrid resin and has combined the composite chelate agent and flocculation agent carries out dynamic exchange, has simplified purifying process, on its purification effect basis, further makes Au
+, Ag
+, Pd
2+, Cu
2+, Pb
2+Cause the ppb level Deng the metals ion reduction, cost is low, and the purifying time is short, is fit to industrialization production.
The present invention is optimized the silicon sol purification process that proposes among the patent CN101475180; Purge process is carried out in the container that has cooling, heating and stir; Under the acting in conjunction of composite chelate agent and flocculation agent, only use positive negatively charged ion hybrid resin, realize the dynamic purification of silicon sol.The present invention makes the needed step of purifying silicon colloidal sol still less under the prerequisite that guarantees purification effect, the time is shorter.Metal ion content is all in the ppb level in the silicon sol behind the purifying, and the metals ion total amount is lower than 10ppm.
Refining effect of the present invention is good, can be met the high-purity silicasol of chemically machinery polished requirement, and purification step is simple, and the time is short, and efficient is high, can be used for the industriallization continuous production.
Embodiment
Following embodiment can make those skilled in the art more comprehensively understand the present invention, but does not limit the present invention in any way.
The manipulation of regeneration of strongly acidic cation-exchange and strong basic type anion-exchange resin adopts following method respectively among the embodiment:
(1) manipulation of regeneration of strongly acidic cation-exchange: adopting concentration is the H of 1～8wt%
2SO
4Or concentration is the HCl of 4～8wt%, and strongly acidic cation-exchange is carried out manipulation of regeneration, and the regenerated liquid volume is 2～5 times of strong acid type cationic resin volume; The regenerated liquid flow rate is 1～10m/h; Advance the acid back water forward drip washing that finishes, wash to resin pH be 3～7, after the drip washing; It is 3～5kg/cm that inflation makes resin mixing, air pressure
2, the time is 10～30min;
(2) manipulation of regeneration of strong basic type anion-exchange resin: employing concentration is that the NaOH of 2～5wt% carries out manipulation of regeneration to strong basic type anion-exchange resin; The regenerated liquid volume is 2～6 times of strong base resin anion(R.A) volume, and the regenerated liquid flow rate is 1～10m/h, advances the alkali back water reverse drip washing that finishes; It is 7～9 that water is washed till resin pH; After the drip washing, it is 3～5kg/cm that inflation makes resin mixing, air pressure
2, the time is 10～30min;
Regeneration treating method with Shangyang anionite-exchange resin is a kind of method in common, under the prerequisite that does not break away from know-why of the present invention, can also make corresponding adjustment and improvement, and these adjustment and improvement also should be regarded as protection scope of the present invention.
Embodiment 1
Strongly acidic cation-exchange is for having cation exchange groups-SO on resin matrix
3The Zeo-karb of H is selected Dowex 50W for use; Strong basic type anion-exchange resin is for having cation exchange groups-N on resin matrix
+(CH
3)
3Cl
-Or-N
+(CH
3)
3C
2H
4OHCl
-Anionite-exchange resin, select Dowex 1 for use.
Dioxide-containing silica is 20% in the silicon sol to be purified, and particle diameter is 40nm, the about 3000ppm of metal ion content, the about 300ppm of anion-content.The purification process step of high-purity silicon dioxide colloidal sol is following:
(1) strongly acidic cation-exchange and strong basic type anion-exchange resin are carried out manipulation of regeneration respectively;
(2) will regenerate good strongly acidic cation-exchange and strong basic type anion-exchange resin mixed in 10: 1 by volume the strong acid and strong base hybrid resin, and pack into and have in the container of cooling, heating and stirring;
(3) silicon sol to be purified is joined in the container that the strong acid and strong base hybrid resin is housed, control silicon sol temperature is 10 ℃, and the weight ratio of strong acid and strong base hybrid resin and silicon sol is 1: 30;
(4) open whipping appts in the container, stir 15min, silicon sol to be purified and strong acid and strong base hybrid resin are mixed;
(5) carry out adding composite chelate agent and flocculation agent in the process at step (4) dynamic purification, wherein main sequestering agent is selected ammonium diethyldithiocarbamate for use, and addition is 0.3% of a silicon-dioxide quality; Auxiliary sequestrant is selected the trithio tricyanic acid for use; Addition is 0.1% of a silicon-dioxide quality, and flocculation agent is selected SEPIGEL 305 for use, and addition is 0.02% of a silicon-dioxide quality; Control pH is 1.5～2.5, obtains the silicon sol behind the purifying.
Silicon sol behind the purifying is that pH is 2.0 high-purity silicasol, and its metal ion content is all in the ppb level, and the metals ion total amount is lower than 10ppm.
Embodiment 2
Strongly acidic cation-exchange is for having cation exchange groups-SO on resin matrix
3The Zeo-karb of H is selected Amberlite IR-120 for use; Strong basic type anion-exchange resin is for having cation exchange groups-N on resin matrix
+(CH
3)
3Cl
-Or-N
+(CH
3)
3C
2H
4OHCl
-Anionite-exchange resin, select AmberliteIRA-400 for use.
Dioxide-containing silica is 40% in the silicon sol to be purified, and particle diameter is 30nm, the about 2000ppm of metal ion content, the about 650ppm of anion-content.The purification process step of high-purity silicon dioxide colloidal sol is following:
(1) strongly acidic cation-exchange and strong basic type anion-exchange resin are carried out manipulation of regeneration respectively;
(2) will regenerate good strongly acidic cation-exchange and strong basic type anion-exchange resin mixed in 3: 1 by volume the strong acid and strong base hybrid resin, and pack into and have in the container of cooling, heating and stirring;
(3) silicon sol to be purified is joined in the container that the strong acid and strong base hybrid resin is housed, control silicon sol temperature is 25 ℃, and the mass ratio of strong acid and strong base hybrid resin and silicon sol is 1: 38;
(4) open whipping appts in the container, stir 20min, silicon sol to be purified and strong acid and strong base hybrid resin are mixed;
(5) carry out adding in the process composite chelate agent and flocculation agent at step (4) dynamic purification, wherein main sequestering agent is selected the two dithio sodium formiates of triethylene tetramine for use, and addition is 1% of a silicon-dioxide quality; Auxiliary sequestrant is selected YD 30 (EDTA) for use; Addition is 0.3% of a silicon-dioxide quality, and flocculation agent is selected SEPIGEL 305 for use, and addition is 0.04% of a silicon-dioxide quality; Control pH is 2.0～3.0, obtains the silicon sol behind the purifying.
Silicon sol behind the purifying is that pH is 2.6 high-purity silicasol, and its metal ion content is all in the ppb level, and the metals ion total amount is lower than 10ppm.
Embodiment 3
Strongly acidic cation-exchange is for having cation exchange groups-SO on resin matrix
3The Zeo-karb of H is selected Amberlyst 15 for use; Strong basic type anion-exchange resin is for having cation exchange groups-N on resin matrix
+(CH
3)
3Cl
-Or-N
+(CH
3)
3C
2H
4OHCl
-Anionite-exchange resin, select Amberlite IRA-410 for use.
Dioxide-containing silica is 30% in the silicon sol to be purified, and particle diameter is 10nm, the about 3000ppm of metal ion content, the about 600ppm of anion-content.The purification process step of high-purity silicon dioxide colloidal sol is following:
(1) strongly acidic cation-exchange and strong basic type anion-exchange resin are carried out manipulation of regeneration respectively;
(2) will regenerate good strongly acidic cation-exchange and strong basic type anion-exchange resin mixed in 5: 1 by volume the strong acid and strong base hybrid resin, and pack into and have in the container of cooling, heating and stirring;
(3) silicon sol to be purified is joined in the container that the strong acid and strong base hybrid resin is housed, control silicon sol temperature is 30 ℃, and the weight ratio of strong acid and strong base hybrid resin and silicon sol is 1: 28;
(4) open whipping appts in the container, stir 25min, silicon sol to be purified and strong acid and strong base hybrid resin are mixed;
(5) carry out adding composite chelate agent and flocculation agent in the process at step (4) dynamic purification, wherein main sequestering agent is selected DDD dimethylammonium dimethyl dithiocarbamate for use, and addition is 1.5% of a silicon-dioxide quality; Auxiliary sequestrant is selected ethylenediamine tetraacetic ethylidene phosphonic acids for use; Addition is 1% of a silicon-dioxide quality, and flocculation agent is selected ROHM for use, and addition is 0.06% of a silicon-dioxide quality; Control pH is 3.0～3.5, obtains the silicon sol behind the purifying.
Silicon sol behind the purifying is that pH is 3.2 high-purity silicasol, and its metal ion content is all in the ppb level, and the metals ion total amount is lower than 10ppm.
Embodiment 4
Strongly acidic cation-exchange is for having cation exchange groups-SO on resin matrix
3The Zeo-karb of H is selected the D113 of Nankai for use, and strong basic type anion-exchange resin is for having cation exchange groups-N on resin matrix
+(CH
3)
3Cl
-Or-N
+(CH
3)
3C
2H
4OHCl
-Anionite-exchange resin select Lewati MP-M500 for use.
Dioxide-containing silica is 35% in the silicon sol to be purified, and particle diameter is 40nm, the about 1000ppm of metal ion content, the about 500ppm of anion-content.The purification process step of high-purity silicon dioxide colloidal sol is following:
(1) strongly acidic cation-exchange and strong basic type anion-exchange resin are carried out manipulation of regeneration respectively;
(2) will regenerate good strongly acidic cation-exchange and strong basic type anion-exchange resin mixed in 2: 1 by volume the strong acid and strong base hybrid resin, and pack into and have in the container of cooling, heating and stirring;
(3) silicon sol to be purified is joined in the container that the strong acid and strong base hybrid resin is housed, control silicon sol temperature is 5 ℃, and the weight ratio of strong acid and strong base hybrid resin and silicon sol is 1: 67;
(4) open whipping appts in the container, stir 30min, silicon sol to be purified and strong acid and strong base hybrid resin are mixed;
(5) carry out adding composite chelate agent and flocculation agent in the process at step (4) dynamic purification, wherein main sequestering agent selects 1,3 for use; 5-Hexahydrotriazine dithio sodium formiate, addition is 2% of a silicon-dioxide quality, auxiliary sequestrant is selected Hydrocerol A (CA) for use; Addition is 1.5% of a silicon-dioxide quality, and flocculation agent is selected polyoxyethylene for use, and addition is 0.08% of a silicon-dioxide quality; Control pH is 3.5～4.5, obtains the silicon sol behind the purifying.
Silicon sol behind the purifying is that pH is 4.0 high-purity silicasol, and its metal ion content is all in the ppb level, and the metals ion total amount is lower than 10ppm.
The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (10)
1. the purification process of a high-purity silicasol is characterized in that, this method steps is following:
(1) strongly acidic cation-exchange and strong basic type anion-exchange resin are carried out manipulation of regeneration respectively;
(2) will regenerate good strongly acidic cation-exchange and strong basic type anion-exchange resin proportional mixing gets the strong acid and strong base hybrid resin, and packs into and have in the container of cooling, heating and stirring;
(3) join in the container that the strong acid and strong base hybrid resin is housed silicon sol to be purified and controlled temperature, the weight ratio of strong acid and strong base hybrid resin and silicon sol is 1: (1～100);
(4) open whipping appts in the container, stir, silicon sol to be purified and strong acid and strong base hybrid resin are mixed;
(5) carry out in the process adding composite chelate agent and flocculation agent at step (4) dynamic purification, control pH is 1～5, obtains the silicon sol behind the purifying;
Said composite chelate agent comprises main sequestering agent and auxiliary sequestrant; Said main sequestering agent is the sequestrant that contains dithiocarbamate-based group;
Said auxiliary sequestrant is polyethylene imine based xanthogenic acid, starch xanthate, epoxy polyamine chloropropane multipolymer xanthogenate, SEPIGEL 305 xanthogenate, trithio tricyanic acid, YD 30; Nitrilotriacetic acid, one or more in diethylene triaminepentaacetic acid(DTPA) and salt thereof, Hydrocerol A, tartrate and glucono-, hydroxyethylethylene diamine tri-acetic acid, bicine N-, polymethyl acrylic acid, HPMA, fumaric acid (FUMARIC ACID TECH GRADE)-propene sulfonic acid interpolymer, ethylenediamine tetraacetic ethylidene phosphonic acids, ethylenediamine tetramethylene phosphonic acid, Diethylenetriamine five ethylidene phosphonic acids, Diethylenetriamine pentamethylene phosphonic acids, three second tetramines, six ethylidene phosphonic acids, tn four ethylidene phosphonic acids, the tn tetramethylene phosphonic acid;
Said flocculation agent is a kind of in SEPIGEL 305, ROHM, Vinylpyrrolidone polymer, Z 150PH, the polyoxyethylene.
2. method according to claim 1 is characterized in that: said main sequestering agent is one or more in ammonium, sodium or the sylvite that contains dithiocarbamate-based group.
3. method according to claim 1; It is characterized in that: the said sequestrant that contains dithiocarbamate-based group is dimethyl dithiocarbamate, N,N-Diethyldithiocarbamic Acid, dibutyl dithiocaarbamate salt, dibenzyl aminodithioformic acid salt, dioctyl MGD, double hydroxyethyl MGD, the two dithio formates of triethylene tetramine, polyamines dithio formate, 1; 3, one or more in the 5-Hexahydrotriazine dithio formate.
4. method according to claim 1 is characterized in that: said composite chelate agent addition be in the silicon sol silicon-dioxide quality 0.01～5%.
5. method according to claim 4 is characterized in that: the main sequestering agent addition is 0.3%～2% of a silicon-dioxide quality, and auxiliary sequestrant addition is 0.1%～1.5% of a silicon-dioxide quality.
6. method according to claim 1 is characterized in that: said flocculation agent addition be in the silicon sol silicon-dioxide quality 0.02%～0.08%.
7. method according to claim 1 is characterized in that: in the said high-purity silicasol, silica concentration is 1～50wt%, and particle diameter is 1～300nm, and the positively charged ion total amount is 200～5000ppm.
8. method according to claim 1 is characterized in that: strongly acidic cation-exchange and strong basic type anion-exchange resin volume ratio are (0.1～10) in the said strong acid and strong base hybrid resin: 1.
9. method according to claim 1 is characterized in that: in the step (3), controlled temperature is at 0～60 ℃.
10. method according to claim 1 is characterized in that: in the step (4), stir 10～30min.
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| CN103145133A (en) * | 2013-03-17 | 2013-06-12 | 上虞市佳和化工有限公司 | Preparation method of silicon sol |
| CN104030300A (en) * | 2014-07-09 | 2014-09-10 | 中国海洋石油总公司 | Preparation method of silica sol for catalytic cracking catalyst binding agent |
| CN104263249A (en) * | 2014-09-26 | 2015-01-07 | 深圳市力合材料有限公司 | Treatment method of silica sol |
| CN104591192A (en) * | 2014-12-24 | 2015-05-06 | 上海新安纳电子科技有限公司 | Method for preparing high-purity silicic acid |
| CN105419645A (en) * | 2014-09-16 | 2016-03-23 | 旭硝子株式会社 | Method of regenerating polishing slurry and method of manufacturing substrate |
| CN108349741A (en) * | 2015-10-20 | 2018-07-31 | 日产化学工业株式会社 | The manufacturing method of purified silicate aqueous solution |
| CN113583038A (en) * | 2021-07-27 | 2021-11-02 | 合盛硅业(鄯善)有限公司 | Octamethylcyclotetrasiloxane purification method |
| CN113896204A (en) * | 2021-11-29 | 2022-01-07 | 苏州西丽卡电子材料有限公司 | Preparation method of ultra-high purity silica sol |
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| CN105419645A (en) * | 2014-09-16 | 2016-03-23 | 旭硝子株式会社 | Method of regenerating polishing slurry and method of manufacturing substrate |
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| CN104263249B (en) * | 2014-09-26 | 2016-06-29 | 深圳市力合材料有限公司 | A kind of processing method of Ludox |
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| CN108349741A (en) * | 2015-10-20 | 2018-07-31 | 日产化学工业株式会社 | The manufacturing method of purified silicate aqueous solution |
| CN113583038A (en) * | 2021-07-27 | 2021-11-02 | 合盛硅业(鄯善)有限公司 | Octamethylcyclotetrasiloxane purification method |
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