CN101121520A - Acidic silicon dioxide sol and its preparation method and use - Google Patents
Acidic silicon dioxide sol and its preparation method and use Download PDFInfo
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- CN101121520A CN101121520A CNA2007101195789A CN200710119578A CN101121520A CN 101121520 A CN101121520 A CN 101121520A CN A2007101195789 A CNA2007101195789 A CN A2007101195789A CN 200710119578 A CN200710119578 A CN 200710119578A CN 101121520 A CN101121520 A CN 101121520A
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Abstract
The present invention provides an acid silica sol, which is characterized in that the present invention comprises water and a silicon dioxide colloid with the particle size of nanometer and submicron, produced from a silicon powder and dispersed in the water. The pH value of the sol is between 1.5 and 3.5 and the content of a copper ion is less than or equal to 50 ppb. The sol has the advantages of high stability and high purity quotient, applicable to the chemical mechanical polishing (CMP) of the electronic industry, the semiconductor, the hard disk, the compound crystal and the precise optical device. Because of the low copper content, the present invention has an obvious predominance in the semiconductor polishing field. The present invention also provides the preparation method and use of the acid silica sol.
Description
Technical field
The present invention relates to silicon sol is polishing material, particularly a kind of acid silicon dioxide sol and its production and use.
Background technology
Fast development along with information industry, the integrated degree of electron device is more and more higher, it is very important that the planarization process of device surface just seems, chemically machinery polished (CMP) technology of being developed jointly by IBM and Microtechnology company is a kind of preferred method of making unicircuit, this method can obtain integral planarization on wafer, silicon sol is (as patent TW245789B, CN1359997, CN1822325, JP2002284516, KR20040056167, JP2005159351, US6048789, CN1727431, CN1359997, CN1194288, TW544336B) or silicon sol oxide coated (as patent JP2003193038, CA2382724, US2004211337, WO2005035688, CN1543492) polishing fluid be the most representative at present CMP technology rumbling compound.
Silicon sol is the amorphous silica aggregated particles colloidal solution that homodisperse forms in water.Can be divided into two kinds of acidic silicasol and alkaline silica sols according to pH value of solution value scope.The alkalescence silicon dioxide gel is a kind of stabilising system, and is more about the patent of its preparation and application facet both at home and abroad, as KR920005405B, and JP2006036605, GB1211483, CN1352673, CN1084490, CN1155514 have report in this respect.
Relative alkaline silica sol, acidic silicasol is in metastable state, and the gel trend of acidic silicasol that pectisation, especially high density can take place in put procedure gradually is more obvious, becomes the major influence factors of its application of restriction.The preparation technology commonly used of acidic silicasol is as follows: the commercial water glass is exchanged by dilution and with Zeo-karb, obtain active silicic acid; Silicic acid is handled to alkalescence with alkali lye; Silicate solution that again should alkalescence heats condensation reaction and concentrates, and makes alkaline silica sol; At last alkaline silica sol is carried out cationic exchange through resin cation (R.C.) again, add an amount of acid simultaneously and regulate, obtain the acidic silicasol under the corresponding acid number.By the acidic silicasol poor stability that above-mentioned technology makes, be raw material as patent US2244325 with water glass, the shelf-time of the acidic silica gel that makes is only for several hours, and its peak concentration is 15%, brings great inconvenience for storage and transportation; Patent US3867304 is raw material with water glass, can improve the stability of gained acidic silica gel greatly by repeatedly positively charged ion and anionresin.Other method discloses a kind of silicon-dioxide lapping liquid that contains the pH of methyl alcohol at 1-6 as patent TW234579B, and this lapping liquid can be used for the polishing of silicon substrate; CN1587041 discloses a kind of preparation method of acid silicon dioxide sol, and promptly sulfuric acid and the above dispersion agent silicon-dioxide of 200 orders with 50-65% mixes, and regulates the pH value through sodium hydroxide then, imposes 100 volts of voltage commutations at last and handles and get; The colloidal sol that this method makes is mainly as people, fowl and animal excrement and garbage treating process.Patent JP6199515 and JP63123807 obtain more stable acid silicon dioxide sol through ion exchange treatment then by small amounts aluminium is joined in the silicon dioxide gel.
Aforesaid method; because the restriction of method itself or the influence of raw material; the normal acidic silica gel that makes that makes exists poor stability or the high shortcoming of metal ion content; perhaps need to add the stability that other auxiliary agents increase acidic silicasol, regular meeting produced bigger pollution when this was used for electronics or semiconductor applications CMP polishing to silicon dioxide gel.
Summary of the invention
The present invention is directed to the defective or the deficiency that exist in the prior art, a kind of acid silicon dioxide sol is provided, this colloidal sol has high stability and highly purified characteristics, can be applicable to the chemically machinery polished (CMP) of electron trade, semi-conductor, hard disk, compound crystal, precision optics etc., because of its low copper content has superiority in the polished semiconductor field especially.
The present invention also provides the preparation method of above-mentioned acid silicon dioxide sol.
The present invention also provides the purposes of above-mentioned acid silicon dioxide sol.
Technical scheme of the present invention is as follows:
A kind of acid silicon dioxide sol is characterized in that: comprising water and being scattered in the water is that the particle diameter that raw material makes is the silicon dioxide colloid of nano level or submicron order with the silica flour, and the pH value of colloidal sol is 1.5～3.5, content of copper ion≤50ppb.
The particle diameter of described silicon dioxide colloid is 5～200nm.
The mass percent concentration of described silicon dioxide colloid is 5～50%.
Described water is the high purity water of resistivity 〉=14M Ω cm.
Kinematic viscosity≤the 5mm of described colloidal sol
2/ s.
The shelf time of described colloidal sol 〉=12 month.
Described silica flour is 100～800 purpose silica flours, and its chemical ingredients is Si 〉=99%, Cu≤0.005%.
The preparation method of above-mentioned acid silicon dioxide sol is characterized in that may further comprise the steps:
(1) is raw material with the silica flour, under the katalysis of alkali, makes alkaline silicon dioxide gel by the thermal hydrolysis reaction;
(2) the alkaline silicon dioxide gel that will make carries out filtration treatment;
(3) the alkaline silicon dioxide gel after will filtering is handled by the strong acidic ion resin exchange and is obtained the pH value at 2.5～4 acid silicon dioxide sol;
(4) acid silicon dioxide sol after the exchange can be regulated pH value to 1.5～3.5 as required.
The particle diameter of described silicon dioxide colloid and concentration are controlled by the feed rate of reaction times and silica flour.
The purposes of above-mentioned acid silicon dioxide sol is characterized in that: be used for the chemically machinery polished of electron trade, semi-conductor, hard disk, compound crystal or precision optics.
Technique effect of the present invention is as follows:
Acid silicon dioxide sol of the present invention, long shelf time and low content of copper ion are arranged, be applicable to the chemically machinery polished (CMP) of electron trade, semi-conductor, hard disk, compound crystal, precision optics etc., because of its low copper content has superiority in the polished semiconductor field especially.Utilize acid silicon dioxide sol of the present invention as polishing fluid the GaAs wafer to be carried out the final step polished finish, the quality product that result's proof makes by the present invention occupy advanced international standard.
Description of drawings
Fig. 1 is the technological process of production figure of preparation acid silicon dioxide sol.
Fig. 2 is that the particle diameter that the present invention obtains is transmission electron microscope (TEM) photo of the silicon dioxide gel about 60nm.
Embodiment
The invention provides a kind of acid silicon dioxide sol and preparation technology thereof, the colloidal sol particle diameter is 5-200nm, and kinematic viscosity is less than 5mm
2/ s, the pH value is 1.5-3.5, and mass percent concentration is 5-50%, and content of copper ion is less than 50ppb.This colloidal sol is to be raw material with the silica flour, under the katalysis of alkali, by the thermal hydrolysis reaction, filters after strong acidic ion resin exchanges preparation.The invention still further relates to acid silicon dioxide sol that can pass through this method acquisition and uses thereof.The present invention has following characteristics: (a) a kind of acid silicon dioxide sol, its particle diameter are 5-200nm, and its kinematic viscosity is less than 5mm
2/ s, its pH value is 1.5-3.5, and its mass percent concentration is 5-50%, and its content of copper ion is less than 50ppb, and its shelf time was greater than 12 months.(b) this colloidal sol is to be raw material with the silica flour, under the katalysis of alkali, goes out alkaline silicon dioxide colloid with the high purity water prepared in reaction; This process can obtain the silicon dioxide colloid of particle diameter at 5-200nm by the add-on of control silica flour, the conditions such as speed and reaction times that add; With storng-acid cation exchange resin alkaline silicon dioxide colloid is exchanged, obtain the acid silicon dioxide colloid of pH value at 2.5-4, exchange process also is simultaneously the process that a secondary is purified; By suitable pH regulator agent, can obtain the acid silicon dioxide sol of pH value in the 1.5-3.5 scope.(c) acid silicon dioxide sol in this invention, long shelf time and low content of copper ion are arranged, be applicable to the chemically machinery polished (CMP) of electron trade, semi-conductor, hard disk, compound crystal, precision optics etc., because of its low copper content has superiority in the polished semiconductor field especially.
It is 5-200nm that the present invention can provide a kind of particle diameter, and kinematic viscosity is less than 5mm
2/ s, the pH value is 1.5-3.5, and mass percent concentration is 5-50%, and its content of copper ion is less than 50ppb, and shelf time is more than 12 months and do not contain acid silicon dioxide sol of any additives and preparation method thereof.In conjunction with shown in Figure 1, its technological process is as follows:
(1) is raw material with the silica flour, under the katalysis of alkali, makes alkaline silicon dioxide gel, under this reaction conditions, can avoid introducing metal ion effectively by the thermal hydrolysis reaction;
(2) the alkaline silicon dioxide gel that will make is handled after filtration, removes unreacted silica flour and impurity completely;
(3) the alkaline silicon dioxide gel after will filtering is handled by the strong acidic ion resin exchange and is obtained the acid silicon dioxide sol of pH value at 2.5-4, and this process is equivalent to the process of a secondary purification through ion-exchange;
(4) acid silicon dioxide sol after the exchange can be regulated the pH value as required to 1.5-3.5.
Related content is explained as follows in the above-mentioned technology:
1. described silica flour is 100～800 purpose silica flours, and its chemical ingredients is Si 〉=99%, Cu≤0.005%;
2. described alkali is the pure alkali metal hydroxide of top grade, is preferably sodium hydroxide and potassium hydroxide;
3. described water is high purity water, and resistivity is greater than 14M Ω cm;
4. described resin is a kind of storng-acid cation exchange resin with sulfonic group;
5. described pH regulator agent is diluted acid (the inorganic or organic acid) aqueous solution, is preferably dilute hydrochloric acid;
6. described filtration unit is plate-and-frame filter press and micro-filter;
7. described temperature of reaction is 70-95 ℃, is preferably 85 ℃;
8. the described reaction times is 6-80h;
9. described exchange number of times is 2-3 time;
10. described feed rate is 0.01-30Kg/30mim;
11. in the above-mentioned technology, to the manipulation of regeneration employing strong acid aqueous solution immersion of Zeo-karb, such as 1: 2-1: 4 hydrochloric acid.
The acid silicon dioxide polishing fluid that adopts the present invention to make carries out the final step polished finish to the GaAs wafer, and the quality product that result's proof makes by the present invention occupy advanced international standard.
Accompanying drawing 1 has provided the technological process of production figure of preparation acid silicon dioxide sol.
It is transmission electron microscope (TEM) photo of the silicon dioxide gel about 60nm that accompanying drawing 2 has provided the gained particle diameter.
Describe several specific embodiments of the present invention below in detail.
Embodiment one:
The 2L high purity water is heated to 50 ℃ in four-hole boiling flask, adds the pure NaOH5.0g of top grade then, continue to be heated to 70 ℃, whipped state adds silica flour 30.0g down, adds silica flour 30.0g later per half an hour, stops heating behind the reaction 7h.In entire reaction course, maintain the temperature at about 85 ℃.After reaction solution is chilled to room temperature, filter.Colloidal sol after filtering is carried out cationic exchange, and the mass ratio of used resin and silica gel is 1: 1, behind the exchange 2h, leach silica gel, resin cation (R.C.) is carried out manipulation of regeneration, and regenerated liquid is 1: 2 a dilute hydrochloric acid, after the regeneration, be washed till neutrality with high purity water, carry out the exchange second time, behind the exchange 4h, leach silica gel, silica obtained parameter is tested, and the result is as follows:
| Test event | Test result | Testing method |
| PH value concentration kinematic viscosity particle diameter content of copper ion | 3.04 32％ 3.63mm 2/s 24nm 32ppb | Acidometer specific gravity hydrometer capillary viscosimeter laser particle analyzer ICP-MS |
Embodiment two:
The 500L high purity water is heated to 50 ℃ by electrically heated mode in reactor, add the pure NaOH2.5Kg of top grade then, continue to be heated to 60 ℃, add silica flour 2Kg, open and stir, close heating, add silica flour 2Kg in the time of 75 ℃, add silica flour 4.0Kg later per half an hour, stop to feed in raw material behind the reaction 6h, continue reaction 4h.In reaction process, the regular replenishment high purity water to maintain the temperature at below 95 ℃.After reaction solution is chilled to room temperature, filter.Colloidal sol after filtering is carried out cationic exchange, behind the exchange 4h, leach silica gel, resin cation (R.C.) is carried out manipulation of regeneration, after the regeneration, be washed till neutrality, carry out the exchange second time, behind the exchange 4h with high purity water, leach silica gel, regulate the pH value with dilute hydrochloric acid, each parameter is tested, the result is as follows:
| Test event | Test result | Testing method |
| PH value concentration kinematic viscosity particle diameter content of copper ion | 2.42 22％ 2.1mm 2/s 39nm 36.0ppb | Acidometer specific gravity hydrometer capillary viscosimeter laser particle analyzer ICP-MS |
Embodiment three:
The 500L high purity water is heated to 60 ℃ by electrically heated mode in reactor, add the pure NaOH2Kg of top grade then, continue to be heated to 70 ℃, add silica flour 2Kg, open and stir, close heating, add silica flour 2Kg in the time of 75 ℃, add silica flour 2.5Kg later per half an hour, stop to feed in raw material behind the reaction 10h, continue reaction 2h.After reaction solution is chilled to room temperature, filter.Colloidal sol after filtering is carried out cationic exchange, behind the exchange 4h, leach silica gel, resin cation (R.C.) is carried out manipulation of regeneration, after the regeneration, be washed till neutrality with high purity water, carry out the exchange second time, behind the exchange 4h, leach silica gel, regulate the pH value with dilute hydrochloric acid, each parameter is tested and with this silica gel the GaAS wafer carried out polishing experiments, the result is as follows:
| Test event | Test result | Testing method |
| Content of copper ion on the wafer of pH value concentration kinematic viscosity particle diameter content of copper ion polishing back | 2.34 24％ 2.9mm 2/s 18nm 43.2ppb 39.9*E10atoms/cm 2 | Acidometer specific gravity hydrometer capillary viscosimeter laser particle analyzer ICP-MS TXRF |
Annotate: ICP-MS is the inductively coupled plasma mass spectrometry test.
TXRF is a total-reflection type X-ray fluorescence spectrum.
Contrast that content of copper ion is 246*E10atoms/cm on the wafer of used external product polishing back
2
Embodiment four:
The 500L high purity water is heated to 55 ℃ by electrically heated mode in reactor, add the pure NaOH2.8Kg of top grade then, continue to be heated to 60 ℃, add silica flour 2.5Kg, open and stir, close heating, add silica flour 5.0Kg in the time of 75 ℃, add silica flour 2.0Kg later per half an hour, stop to feed in raw material behind the reaction 12h, continue reaction 8h.After reaction solution is chilled to room temperature, filter.Colloidal sol after filtering is carried out the highly acidic cation exchange, behind the exchange 4h, leach silica gel, resin cation (R.C.) is carried out manipulation of regeneration, after the regeneration, be washed till neutrality, carry out the exchange second time, behind the exchange 4h with high purity water, leach silica gel, regulate the pH value with dilute hydrochloric acid, each parameter is tested, the result is as follows:
| Test event | Test result | Testing method |
| PH value concentration kinematic viscosity particle diameter content of copper ion | 2.6 24％ 2.6mm 2/s 87nm 39.2ppb | Acidometer specific gravity hydrometer capillary viscosimeter laser particle analyzer ICP-MS |
Should be pointed out that the above embodiment can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.Therefore, although this specification sheets has been described in detail to the present invention,, it will be appreciated by those skilled in the art that still and can make amendment or be equal to replacement the present invention; And all do not break away from the technical scheme and the improvement thereof of spirit of the present invention, and it all should be encompassed in the middle of the protection domain of patent of the present invention.
Claims (10)
1. acid silicon dioxide sol is characterized in that: comprising water and being scattered in the water is that the particle diameter that raw material makes is the silicon dioxide colloid of nano level or submicron order with the silica flour, and the pH value of colloidal sol is 1.5～3.5, content of copper ion≤50ppb.
2. acid silicon dioxide sol according to claim 1 is characterized in that: the particle diameter of described silicon dioxide colloid is 5～200nm.
3. acid silicon dioxide sol according to claim 1 is characterized in that: the mass percent concentration of described silicon dioxide colloid is 5～50%.
4. acid silicon dioxide sol according to claim 1 is characterized in that: described water is the high purity water of resistivity 〉=14M Ω cm.
5. acid silicon dioxide sol according to claim 1 is characterized in that: the kinematic viscosity≤5mm of described colloidal sol
2/ s.
6. acid silicon dioxide sol according to claim 1 is characterized in that: the shelf time of described colloidal sol 〉=12 month.
7. acid silicon dioxide sol according to claim 1 is characterized in that: described silica flour is 100～800 purpose silica flours, and its chemical ingredients is Si 〉=99%, Cu≤0.005%.
8. as the preparation method of one of claim 1-7 described acid silicon dioxide sol, it is characterized in that may further comprise the steps:
(1) is raw material with the silica flour, under the katalysis of alkali, makes alkaline silicon dioxide gel by the thermal hydrolysis reaction;
(2) the alkaline silicon dioxide gel that will make carries out filtration treatment;
(3) the alkaline silicon dioxide gel after will filtering is handled by the strong acidic ion resin exchange and is obtained the pH value at 2.5～4 acid silicon dioxide sol;
(4) acid silicon dioxide sol after the exchange can be regulated pH value to 1.5～3.5 as required.
9. the preparation method of acid silicon dioxide sol according to claim 8, it is characterized in that: the particle diameter of described silicon dioxide colloid and concentration can be controlled by the feed rate of reaction times and silica flour.
10. as the purposes of one of claim 1-7 described acid silicon dioxide sol, it is characterized in that: be used for the chemically machinery polished of electron trade, semi-conductor, hard disk, compound crystal or precision optics.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102187402A (en) * | 2008-10-16 | 2011-09-14 | 奥利安科技研究所 | Treatment of liquid wastes containing heavy metals |
| CN102432027A (en) * | 2011-08-31 | 2012-05-02 | 湖北大学 | Monodisperse large-grain-diameter and high-stability acid silica sol and preparation method thereof |
| CN102825561A (en) * | 2012-09-07 | 2012-12-19 | 北京国瑞升科技有限公司 | Water-base polishing film and preparation method thereof |
| CN106395836A (en) * | 2016-08-26 | 2017-02-15 | 强新正品（苏州）环保材料科技有限公司 | High stable silica sol, and preparation method thereof |
| CN109455724A (en) * | 2018-12-26 | 2019-03-12 | 江苏德鑫新材料科技有限公司 | A kind of preparation method of ultra-pure silicasol |
| CN109824274A (en) * | 2019-03-27 | 2019-05-31 | 台玻安徽玻璃有限公司 | A kind of wear-resisting type high light transmission float glass and preparation method thereof |
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2007
- 2007-07-26 CN CN2007101195789A patent/CN101121520B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102187402A (en) * | 2008-10-16 | 2011-09-14 | 奥利安科技研究所 | Treatment of liquid wastes containing heavy metals |
| CN102187402B (en) * | 2008-10-16 | 2015-07-29 | 奥利安科技研究所 | The process of the liquid wastes containing heavy metal |
| CN102432027A (en) * | 2011-08-31 | 2012-05-02 | 湖北大学 | Monodisperse large-grain-diameter and high-stability acid silica sol and preparation method thereof |
| CN102825561A (en) * | 2012-09-07 | 2012-12-19 | 北京国瑞升科技有限公司 | Water-base polishing film and preparation method thereof |
| CN102825561B (en) * | 2012-09-07 | 2015-10-28 | 北京国瑞升科技股份有限公司 | Water-based polished film and preparation method thereof |
| CN106395836A (en) * | 2016-08-26 | 2017-02-15 | 强新正品（苏州）环保材料科技有限公司 | High stable silica sol, and preparation method thereof |
| CN109455724A (en) * | 2018-12-26 | 2019-03-12 | 江苏德鑫新材料科技有限公司 | A kind of preparation method of ultra-pure silicasol |
| CN109824274A (en) * | 2019-03-27 | 2019-05-31 | 台玻安徽玻璃有限公司 | A kind of wear-resisting type high light transmission float glass and preparation method thereof |
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