CN1872682A - Method for purifying Nano silica sol dedicated for super large scale integration - Google Patents
Method for purifying Nano silica sol dedicated for super large scale integration Download PDFInfo
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- CN1872682A CN1872682A CN 200610013970 CN200610013970A CN1872682A CN 1872682 A CN1872682 A CN 1872682A CN 200610013970 CN200610013970 CN 200610013970 CN 200610013970 A CN200610013970 A CN 200610013970A CN 1872682 A CN1872682 A CN 1872682A
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Abstract
This invention discloses a method for purifying silica nanosol used for large-scale integrated circuit. The method comprises: (1) adding hydrochloric acid to a cation exchange resin, and stirring to obtain acidic cation exchange resin; (2) adding basic silica nanosol with a high content of metal ions to the acidic cation exchange resin, and ion-exchanging to obtain acidic silica nanosol; (3) adding NaOH solution to an anion exchange resin, and stirring to obtain basic anion exchange resin; (4) adding acidic silica nanosol to the basic anion exchange resin, and ion-exchanging to obtain basic silica nanosol; (5) adding the basic silica nanosol to the acidic cation exchange resin, and ion-exchanging to obtain acidic silica nanosol with a low content of metal ions. The method has such advantages as high product purity, low equipment cost, and short purification time.
Description
Technical field
The invention belongs to the purification process of nanometer abrasive, especially relate to a kind of purification process that is used for the silicon sol of the special-purpose grinding and polishing of microelectronics manufacture field CMP.
Background technology
Along with the development of large-scale integrated circuit, the improving constantly of integrated level, constantly the reducing of live width, high-density, hachure, the shallow junction of integrated circuit technology development have become main flow.If the silicon substrate film surface is by the harmful heavy metal impurity contamination in the course of processing, then can influence the interfacial state of device, make device quiescent dissipation electric current increase SiO
2Dielectric breakdown strength reduces, and antistatic effect weakens, threshold voltage shift, early failure appears in the device power aging, especially outstanding in susceptible device susceptores such as CMOS, CCD, also can cause the anti-nuclear radiation ability of military device to weaken, product performance, reliability index and device yield descend.Metal contamination also can destroy integrity, increase leakage current density, the minimizing minority carrier life time of thin oxide layer; Movable ion such as sodium can cause dislocation charge in zone of oxidation, influence the stability of MOS device; Heavy metal ion can increase dark current; Fast diffusion ion as copper, nickel, easily is deposited on silicon face, forms microstructural defects; The iron precipitation can make the gate oxide attenuation.Copper can form rich copper precipitation at silicon silicon-dioxide interface in addition, high temperature (1200 ℃/supersaturation copper silicide can make the zone of oxidation bending, break 20s) time, until penetrating, low temperature (900 ℃/form the lensing precipitation 20s) time make the zone of oxidation attenuation.When metal contamination is serious, also can form vaporific defective (Haze).Alkalimetal ion (Na especially
+) be mobile ion very harmful in the present microelectronics, in the CMP process, can enter in substrate or the medium layer, cause the effects such as local break-through, leakage current increase of device, make that the chip operation reliability reduces, shorten device lifetime.Therefore, microelectronic industry must be controlled harmful metal impurity content etc.Current, be the 64000000 DRAM devices of 0.35 μ m for live width, the critical particle size that influences circuit is 0.06 μ m, the metallic contaminants from surface of polished section stains should be all less than 5 * 10
15At/cm
2, general ULSI processing requirement on the substrate slice that provides metallic pollution less than 10
10Atom/cm
2
In silicon chip processing and device manufacturing processes, all external mediums that contact with silicon chip all may make silicon chip be stain by poisonous metal, glossing be final in the wafer process process, also be most important one manufacturing procedure, and SiO
2Colloidal sol is maximum, the best nanometer abrasive of effect that CMP uses in the ULSI processing procedure, the various impurity of the wafer spontaneous absorption of meeting of new polishing, absorption to metal ion is particularly serious, if the content of metal ion is higher in the polishing fluid, metal ions a large amount of after polishing remain in wafer surface, have not only increased the burden of matting, simultaneously, in polishing process, strengthen the metal ion that enters into wafer inside, these metal ions that enter into wafer inside then are difficult to wash down again.Along with the development of IC technology, to CMP special-purpose nanometer SiO
2Purifying requires will be more and more stricter.The production of silicon sol at present mainly adopts water glass as raw material, causes to contain a large amount of metal ions (Na especially in the silicon sol product
+).Therefore, remove the impurity in the silicon sol, it is very necessary that silicon sol is carried out purifying.
The purifying process of silicon sol does not form the technology of oneself at present, and considerable document is only mentioned once with " aftertreatment ", has only the minute quantity document to mention the method that adopts resin cation exchange to handle.The micelle structure of silicon sol and synoptic diagram thereof as shown in Figure 1, the double electrical layers of silicon sol as shown in Figure 2, the micelle of silicon sol is by a unbodied mSiO
2Be core, surface adsorption silicic acid and silicic acid negative ion (H
2SiO
4, H
3SiO
4 -), a part of zNa of gegenion
+Be adsorbed in the fixed layer another part (y-z) Na
+Be distributed in the diffusion layer, constitute double electrical layers.Electric charge y is called combined potential, and electric charge (y-z) is called electro kinetic potential or claims Zeta potential, zeta-potential.Owing to there is solvation, the ion around the micelle all exists with the solvation form, so that forms one deck high viscosity aquation film, and the thickness of its thickness and diffusion double layer is suitable.Adopt the cationic exchange initial stage, the metal ion of the outer aqueous phase of micelle is the free ion of unbound state, and the metal ion of micelle diffusion layer periphery and the electrostatic force between the micelle are very weak, very easily being adsorbed the stronger material of power catches, so storng-acid cation exchange resin can adsorb and exchange this two-part metal ion rapidly, and the H of electric charge such as release simultaneously
+, and then in and the whole OH of aqueous phase
-, because H
+Amount much larger than OH
-, excessive H
+Make the pH value of solution cross the neutral zone rapidly and enter acidic region, thereby make exchange back silicon sol be acid, metal ion content reduces, and the Zeta potential absolute value increases.
After silicon sol carries out cationic exchange, the Na of silicon sol diffusion layer periphery
+And other metallic cation is removed remaining Na
+With other metallic cation mainly be present in enclose in the diffusion layer and fixed layer in, it is strong that ion is subjected to glue nuclear sucking action in this scope, and the micelle surface is with the hydration shell of one deck viscosity higher, this layer hydration shell slowed down H
+Diffuse into and replace Na in the fixed layer
+Speed with other metallic cation.H
+Slowly enter fixed layer, the micelle surface pH value is changed slowly, a large amount of Na in the silicon sol
+With other metallic cation by H
+Replace H
+Hydratability compare Na
+Strong with other metallic cation, these H
+Cause micelle hydration shell on every side to thicken, seriously hindered Na
+With other metallic cation and H
+Mutual metathetical speed.Therefore, the simple Zeo-karb that adopts comes purified silicon colloidal sol, though can remove the metal ion of part silicon sol, its inside still has the existence of a large amount of metal ions, purification effect is not good, and does not have too big change with the metal ion content that increases of Zeo-karb number of processes.
Summary of the invention
The present invention is in order to overcome weak point of the prior art, a kind of content that effectively reduces the silicon sol metal ion neutralization product to be provided, with the purification process of the silicon sol that improves the wafer quality.
The present invention is achieved through the following technical solutions:
A kind of purification process of Nano silica sol dedicated for super large scale integration is characterized in that may further comprise the steps:
(1) at first the hydrochloric acid soln of 3%-10% being injected Zeo-karb stirs, make Zeo-karb regeneration fully, hydrochloric acid wherein: wet Zeo-karb is 1.4-1.8 milligramequivalent/milliliter, behind the standing demix upper solution is removed, with the remaining Zeo-karb of deionized water rinsing to its pH value in the 2-4 scope, acidic cation-exchange resin;
(2) alkaline silica sol that then metal ion content is higher than 100ppm joins under the situation of continuously stirring in the acidic cation-exchange resin that makes in the above-mentioned steps (1), wherein, alkaline silica sol is 1 with the ratio of the amount of substance of acidic cation-exchange resin: 2-1: 5, under condition of stirring, exchange 10-60min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir behind 30mv-60mv, discharging must show the tart silicon sol behind the standing demix;
(3) the sodium hydroxide solution injection anionite-exchange resin with 3%-10% stirs, make anionite-exchange resin regeneration fully, sodium hydroxide wherein: wet anionite-exchange resin is 1.2-1.6 milligramequivalent/milliliter, behind the standing demix upper solution is removed, with the remaining anionite-exchange resin of deionized water rinsing to its pH value between 9-10, obtain basic anion exchange resin;
(4) then the acidic silicasol that makes in the above-mentioned steps (2) is joined in the basic anion exchange resin that makes in the above-mentioned steps (3), wherein, acidic silicasol is 1 with the ratio of the amount of substance of basic anion exchange resin: 2-1: 5, under condition of stirring, exchange 10-60min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir behind 30mv-60mv, discharging obtains showing the silicon sol of alkalescence behind the standing demix;
(5) again the alkaline silica sol after the exchange that makes in the step (4) is joined under condition of stirring in the acidic cation-exchange resin that makes in the step (1), wherein, alkaline silica sol is 1 with the ratio of the amount of substance of acidic cation-exchange resin: 2-1: 5, under condition of stirring, exchange 10-60min, measure the Zeta potential of exchange solution simultaneously, make its absolute value behind 30mv-60mv, stop to stir, discharging behind the standing demix obtains the apparent tart silicon sol that metal ion reaches several ppm.
In order to make main component is polishing fluid better metal ion of removing in polishing process of silicon sol, make acidic silicasol be converted into alkaline silica sol simultaneously, after sun-male-female ion-exchange, to under condition of stirring, join the acidic silicasol that makes after above-mentioned sun-male-female ion-exchange in the FA/O sequestrant, make final alkaline silica sol product, wherein the volume ratio of acidic silicasol and sequestrant is 1000: 2-10.
Used Zeo-karb is strongly acidic styrene's type Zeo-karb, and used anionite-exchange resin is strong alkaline quaternary ammonium anionite-exchange resin.
The particle diameter of the silicon sol of described purifying is 20nm-60nm.
Action principle of the present invention is as follows:
At first, adopt the metal ion of the outer aqueous phase of Zeo-karb exchange silicon sol micelle and the metal ion of micelle diffusion layer periphery.After silicon sol carries out cationic exchange, the Na of silicon sol diffusion layer periphery
+And other metallic cation is removed remaining Na
+With other metallic cation mainly be present in enclose in the diffusion layer and fixed layer in, this moment since hydration shell thicken, seriously hindered Na
+With other metallic cation and H
+Mutual metathetical speed.Therefore, adopt anionite-exchange resin to exchange, anionite-exchange resin exchange water middle reaches from negatively charged ion (Cl
-, the silicic acid negative ion), discharge OH
-And with the original H of water
+Neutralization generates water, and pH value is risen gradually, makes the silicon sol after the exchange be alkaline, and after the ion-exchange equilibrium, mainly there is the H that is not neutralized in aqueous phase
+, electrolyte concentration descends greatly in the solution.And colloidal electrostatic double layer thickness and electrolytical concentration are inverse ratio, so after the resin anion(R.A) exchange, colloidal electrostatic double layer thickness becomes original tens of times, constitutes the positively charged ion (Na of double electrical layers in a large number
+, H
+) be pushed to position away from glue nuclear, and the magnetism between the glue nuclear weakens greatly, and the viscosity of hydration shell is also corresponding to be reduced, Na in diffusion layer and the fixed layer
+Diffuse into water in a large number with other metallic cation, and then adopt cationic exchange, the Na of absorption aqueous phase
+With other metallic cation, continue to reduce the metal ion content in the silicon sol.So circulation, hydration shell is effectively removed the control of ion diffusion effect, can obtain the few silicon sol of foreign matter content.But because repeatedly repeat to increase cost, reduce production efficiency, take all factors into consideration every factor, select sun-male-female three secondary ions to exchange purifying silicon colloidal sol.
The present invention has following technique effect:
1. the present invention is according to the electric double layer structure of the exchange mechanism and the silicon sol itself of ion exchange resin, and utilization sun-male-female ion exchange resin is the method purifying silicon colloidal sol of exchange alternately.The selectivity order of some common ions of storng-acid cation exchange resin is: Fe
3+Al
3+Ca
2+Mg
2+K
+Na
+H
+, the selectivity order of some common ions of strongly basic anion exchange resin is: SO
4 2-NO
3 -Cl
-OH
-F
-HCO
3 -HSiO
3 -Cationic exchange has been removed the metal ion of the outer aqueous phase of silicon sol micelle and the metal ion of micelle diffusion layer periphery for the first time.Introduce anionite-exchange resin then and exchange, effectively remove the control of hydration shell, make Na in diffusion layer and the fixed layer the ion diffusion effect
+Diffuse into water in a large number with other metallic cation, and then adopt cationic exchange, the Na of absorption aqueous phase
+With other metallic cation, greatly improved the exchange effect of Zeo-karb, greatly reduce the content of silicon sol metal ion neutralization product, purification effect is remarkable, has improved the quality of wafer.The silicon sol metal ion content that present method obtains can reach the ppb level, can satisfy the purity requirement of super large-scale integration complete processing CMP to abrasive, makes the chip operation reliability height of production, the long service life of device.
2. the present invention adopts the FA/O sequestrant to regulate the pH value, the FA/O sequestrant has special construction, its structural representation as shown in Figure 3, this material chelate ring is many, does not contain metal ion, soluble in water, have sequestering power, when regulating pH value, can also be in CMP (Chemical Mechanical Polishing) process the metal ion of effective chelating remnants, further reduce the content of metal ion, reduce the pollution of metal ion polished section.
3.Zeta current potential is greater than 30mv, solution is stable more.Swap time is long more, and metal ion content is more little.The present invention controls swap time by Zeta potential monitoring and ion-exchange time two aspects, both guaranteed the requirement of metal ion content, consider the influence of metal ion content again to Zeta potential, guaranteed the stability of silicon sol, provide necessary monitoring condition for carrying out industrialization, guarantee the repeatability of the stable and product of silicon sol quality in the actual production, make production can realize automatization.Take all factors into consideration the requirement and the production efficiency of quality, the selection Zeta potential is 30-60mv, and be 10-60min swap time.
4. adopt that method equipment cost of the present invention is low, the purifying time is short, energy consumption is low.
Description of drawings
The micelle structure and the synoptic diagram thereof of accompanying drawing 1 silicon sol;
The double electrical layers of accompanying drawing 2 silicon sol;
The structural representation of accompanying drawing 3 sequestrants;
Accompanying drawing 4Zeta potential test result.
Embodiment
Below in conjunction with specific embodiment to the detailed description of the invention.
Used Zeo-karb is strongly acidic styrene's type Zeo-karb among the present invention, as Nankai's board 001 * 7 type, U.S. Amberjet 1200Na, German Lewatit-100, Japanese DiaionSK-1 etc., used anionite-exchange resin is strong alkaline quaternary ammonium anionite-exchange resin, as Nankai's board 201 * 7 types, U.S. AmberliteIRA-400, German Lewatit M500, Britain Eerolite FF etc., ion-exchange time will be considered the Zeta potential factor of silicon sol.When regulating silicon sol pH value, adopted both to have the pH of adjusting value function, had chelated metal ions function FA/O sequestrant again.
Embodiment 1
1752ml, 3% hydrochloric acid soln are injected the ion exchange column that 800ml Nankai board 001 * 7 type Zeo-karb is housed to be stirred, standing demix behind the stirring 3min, upper solution is removed, with the remaining Zeo-karb of deionized water rinsing to its pH value between 2-2.5, acidic cation-exchange resin.
Be 30% with concentration then, particle diameter is 22nm, the alkaline silica sol 536g that metal ion content is higher than 100ppm joins under the situation of continuously stirring in the above-mentioned acidic cation-exchange resin of 400ml, under condition of stirring, exchange 15min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir after more than the 30mv, discharging must show the tart silicon sol behind the standing demix.
Get 834ml then, 3% sodium hydroxide solution injects the ion exchange column that the wet anionite-exchange resin of 400ml Nankai board 201 * 7 types is housed and stirs, standing demix behind the stirring 3min, upper solution is removed, with the remaining anionite-exchange resin of deionized water rinsing to its pH value between 9-9.5, obtain basic anion exchange resin.Then the acidic silicasol 536g after the above-mentioned resin cation exchange is joined in the above-mentioned 400ml basic anion exchange resin, under condition of stirring, exchange 15min, measure the Zeta potential of exchange solution simultaneously, its absolute value stops to stir after more than the 30mv, and discharging obtains showing the silicon sol of alkalescence behind the standing demix.
Again the alkaline silica sol 536g after the above-mentioned resin anion(R.A) exchange is joined under condition of stirring in the above-mentioned 400ml acidic cation-exchange resin, under condition of stirring, exchange 15min, measure the Zeta potential of exchange solution simultaneously, its absolute value stops to stir after more than the 30mv, discharging behind the standing demix obtains the apparent tart silicon sol that metal ion reaches several ppm.
For the user who adopts acid polishing slurry, above-mentioned acidic silicasol gets final product.
For adopting alkalescence and strict polishing fluid, the acidic silicasol through after sun-male-female ion-exchange with 536g joins under condition of stirring in the FA/O sequestrant of 0.8ml at last, makes final silicon sol product.
Embodiment 2
2102.2ml, 5% hydrochloric acid soln are injected the ion exchange column that 1600ml U.S. Amberjet 1200Na type Zeo-karb is housed to be stirred, standing demix behind the stirring 5min, upper solution is removed, with the remaining Zeo-karb of deionized water rinsing to its pH value between 2.5-3, acidic cation-exchange resin.
Be 32% with concentration then, particle diameter is 47nm, the alkaline silica sol 536g that metal ion content is higher than 100ppm joins under the situation of continuously stirring in the above-mentioned acidic cation-exchange resin of 800ml, under condition of stirring, exchange 30min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir after more than the 40mv, discharging must show the tart silicon sol behind the standing demix.
Get 1000ml then, 5% sodium hydroxide solution injects the ion exchange column that the wet anionite-exchange resin of 800ml U.S. AmberliteIRA-400 type is housed and stirs, standing demix behind the stirring 5min, upper solution is removed, with the remaining anionite-exchange resin of deionized water rinsing to its pH value between 9.5-10, obtain basic anion exchange resin.Then the acidic silicasol 536g after the above-mentioned resin cation exchange is joined in the above-mentioned 800ml basic anion exchange resin, under condition of stirring, exchange 30min, measure the Zeta potential of exchange solution simultaneously, its absolute value stops to stir after more than the 40mv, and discharging obtains showing the silicon sol of alkalescence behind the standing demix.
Again the alkaline silica sol 536g after the above-mentioned resin anion(R.A) exchange is joined under condition of stirring in the above-mentioned 800ml acidic cation-exchange resin, under condition of stirring, exchange 30min, measure the Zeta potential of exchange solution simultaneously, its absolute value stops to stir after more than the 40mv, discharging behind the standing demix obtains the apparent tart silicon sol that metal ion reaches several ppm.
The acidic silicasol through after sun-male-female ion-exchange with 536g joins under condition of stirring in the FA/O sequestrant of 2.4ml at last, makes final silicon sol product.
Embodiment 3
1325ml, 10% hydrochloric acid soln are injected the ion exchange column that 2000ml Germany Lewatit-100 type Zeo-karb is housed to be stirred, standing demix behind the stirring 10min, upper solution is removed, with the remaining Zeo-karb of deionized water rinsing to its pH value between 3-3.5, acidic cation-exchange resin.
Be 42% with concentration then, particle diameter is 60nm, the alkaline silica sol 536g that metal ion content is higher than 100ppm joins under the situation of continuously stirring in the above-mentioned acidic cation-exchange resin of 1000ml, under condition of stirring, exchange 60min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir after more than the 60mv, discharging must show the tart silicon sol behind the standing demix.
Get 625ml then, 10% sodium hydroxide solution injects the ion exchange column that the wet anionite-exchange resin of 1000ml Germany LewatitM500 type is housed and stirs, standing demix behind the stirring 10min, upper solution is removed, with the remaining anionite-exchange resin of deionized water rinsing to its pH value between 9.5-10, obtain basic anion exchange resin.Then the acidic silicasol 536g after the above-mentioned resin cation exchange is joined in the above-mentioned 1000ml basic anion exchange resin, under condition of stirring, exchange 60min, measure the Zeta potential of exchange solution simultaneously, its absolute value stops to stir after more than the 60mv, and discharging obtains showing the silicon sol of alkalescence behind the standing demix.
Again the alkaline silica sol 536g after the above-mentioned resin anion(R.A) exchange is joined under condition of stirring in the above-mentioned 1000ml acidic cation-exchange resin, under condition of stirring, exchange 60min, measure the Zeta potential of exchange solution simultaneously, its absolute value stops to stir after more than the 60mv, discharging behind the standing demix obtains the apparent tart silicon sol that metal ion reaches several ppm.
The acidic silicasol through after sun-male-female ion-exchange with 536g joins under condition of stirring in the FA/O sequestrant of 4ml at last, makes final silicon sol product.
The detected result of silicon sol metal ion content is as shown in the table:
A: before the exchange:
| The metallic element kind | The self-control product | External product | Home products |
| Na(mg/L) Al(mg/L) K(mg/L) Cu(mg/L) Fe(mg/L) | 371535 321.2 60 80 90 | 3175 348.0 - - ＜0.01 | 2774 321.2 - - ＜0.01 |
B: exchange back metal ion content:
| The metallic element kind | Corresponding content/mg/L after the ion exchange treatment |
| Na Al K Cu Fe | 3.4＜0.01 do not detect＜0.01 do not detect 0.023＜0.01 and do not detect |
Accompanying drawing 4 is the Zeta potential test result, and X-coordinate is the Zeta potential value, and ordinate zou is %class.From test result, the absolute value of Zeta potential is all greater than 30mv, is in to make the stable potential range of depositing of silicon sol.
Although the disclosed purification process that relates to a kind of Nano silica sol dedicated for super large scale integration has been carried out special description with reference to embodiment, embodiment described above is illustrative and not restrictive, under the situation that does not break away from the spirit and scope of the present invention, all variations and modification are all within the scope of the present invention.
Claims (4)
1, a kind of purification process of Nano silica sol dedicated for super large scale integration is characterized in that may further comprise the steps:
(1) at first the hydrochloric acid soln of 3%-10% being injected Zeo-karb stirs, make Zeo-karb regeneration fully, hydrochloric acid wherein: wet Zeo-karb is 1.4-1.8 milligramequivalent/milliliter, behind the standing demix upper solution is removed, again with deionized water rinsing remaining Zeo-karb to its pH value in the 2-4 scope, must acidic cation-exchange resin;
(2) alkaline silica sol that then metal ion content is higher than 100ppm joins under the situation of continuously stirring in the acidic cation-exchange resin that makes in the above-mentioned steps (1), wherein, alkaline silica sol is 1 with the ratio of the amount of substance of acidic cation-exchange resin: 2-1: 5, under condition of stirring, exchange 10-60min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir behind 30mv-60mv, discharging must show the tart silicon sol behind the standing demix;
(3) the sodium hydroxide solution injection anionite-exchange resin with 3%-10% stirs, make anionite-exchange resin regeneration fully, sodium hydroxide wherein: wet anionite-exchange resin is 1.2-1.6 milligramequivalent/milliliter, behind the standing demix upper solution is removed, with the remaining anionite-exchange resin of deionized water rinsing to its pH value between 9-10, obtain basic anion exchange resin;
(4) then the acidic silicasol that makes in the above-mentioned steps (2) is joined in the basic anion exchange resin that makes in the above-mentioned steps (3), wherein, acidic silicasol is 1 with the ratio of the amount of substance of basic anion exchange resin: 2-1: 5, under condition of stirring, exchange 10-60min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir behind 30mv-60mv, discharging obtains showing the silicon sol of alkalescence behind the standing demix;
(5) again the alkaline silica sol after the exchange that makes in the step (4) is joined under condition of stirring in the acidic cation-exchange resin that makes in the step (1), wherein, alkaline silica sol is 1 with the ratio of the amount of substance of acidic cation-exchange resin: 2-1: 5, under condition of stirring, exchange 10-60min, measure the Zeta potential of exchange solution simultaneously, make its absolute value stop to stir behind 30mv-60mv, discharging behind the standing demix obtains the apparent tart silicon sol that metal ion reaches the ppb level.
2, the purification process of Nano silica sol dedicated for super large scale integration according to claim 1, it is characterized in that, after sun-male-female ion-exchange, again the FA/O sequestrant is joined in the acidic silicasol after above-mentioned sun-male-female ion-exchange, make final silicon sol product, wherein the volume ratio of acidic silicasol and sequestrant is 1000: 2-10.
3, the purification process of Nano silica sol dedicated for super large scale integration according to claim 1 and 2, it is characterized in that: used Zeo-karb is strongly acidic styrene's type Zeo-karb, and used anionite-exchange resin is strong alkaline quaternary ammonium anionite-exchange resin.
4, the purification process of Nano silica sol dedicated for super large scale integration according to claim 1 is characterized in that: the particle diameter of the silicon sol of described purifying is 20nm-60nm.
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| CN101585541B (en) * | 2009-06-23 | 2011-06-01 | 济南银丰硅制品有限责任公司 | Method for preparing electronic-grade silica sol |
| CN102583406A (en) * | 2012-01-19 | 2012-07-18 | 深圳市力合材料有限公司 | Purifying method for high-purity silica sol |
| CN103043671A (en) * | 2012-12-27 | 2013-04-17 | 上海新安纳电子科技有限公司 | Production method for polysilicic acid |
| CN106115721A (en) * | 2016-06-27 | 2016-11-16 | 霍山县忠福硅溶胶有限公司 | A kind of preparation method of industry silicasol |
| CN114132935A (en) * | 2021-12-31 | 2022-03-04 | 山东百特新材料有限公司 | Purification method of silica sol |
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| JP3225549B2 (en) * | 1991-09-25 | 2001-11-05 | 日産化学工業株式会社 | Production method of high purity aqueous silica sol |
| DE69310950T2 (en) * | 1992-02-27 | 1997-10-23 | Nissan Chemical Ind Ltd | Process for the preparation of a high purity aqueous silica sol |
| CN1155514A (en) * | 1996-01-25 | 1997-07-30 | 天津市化学试剂一厂 | Manufacture of high purity, high concentration and high granularity large granular silicon dioxide gel |
| CN1260125C (en) * | 2004-04-09 | 2006-06-21 | 苏州天马医药集团精细化学品有限公司 | Method for fabricating nano sol of silicon dioxide in use for papermaking |
| CN1304288C (en) * | 2004-07-03 | 2007-03-14 | 河北工业大学 | Method for preparing silicasol with big grain diameter |
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| CN101585541B (en) * | 2009-06-23 | 2011-06-01 | 济南银丰硅制品有限责任公司 | Method for preparing electronic-grade silica sol |
| CN102583406A (en) * | 2012-01-19 | 2012-07-18 | 深圳市力合材料有限公司 | Purifying method for high-purity silica sol |
| CN102583406B (en) * | 2012-01-19 | 2014-03-19 | 深圳市力合材料有限公司 | Purifying method for high-purity silica sol |
| CN103043671A (en) * | 2012-12-27 | 2013-04-17 | 上海新安纳电子科技有限公司 | Production method for polysilicic acid |
| CN103043671B (en) * | 2012-12-27 | 2014-12-03 | 上海新安纳电子科技有限公司 | Production method for polysilicic acid |
| CN106115721A (en) * | 2016-06-27 | 2016-11-16 | 霍山县忠福硅溶胶有限公司 | A kind of preparation method of industry silicasol |
| CN114132935A (en) * | 2021-12-31 | 2022-03-04 | 山东百特新材料有限公司 | Purification method of silica sol |
| CN114292535A (en) * | 2021-12-31 | 2022-04-08 | 山东百特新材料有限公司 | Method for improving water resistance of nano ceramic coating |
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