CN101077946A - Preparing method of silicon dioxide abrasive material - Google Patents
Preparing method of silicon dioxide abrasive material Download PDFInfo
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Abstract
The process of preparing silica abradant with water glass as material includes the following four steps: 1. primary purifying through diluting water glass to SiO2 content below 15 %, filtering and cationic ion resin exchanging; 2. preparing crystal seed through regulating pH value of the purified liquid to 8.0-11.0, heating to 60-135 deg.c while stirring, and cooling; 3. increasing grain size through heating the liquid from the step 2 to 60-135 deg.c, and adding liquid from the step 1 in the temperature below 50 deg.c to obtain coarse abradant; and 4. purification through ion exchange with cation resin and anion resin to obtain the silica abradant product. The silica abradant thus prepared has homogeneous grain size and high purity, and can meet the requirement for polishing in electronic industry.
Description
Technical field
The present invention relates to a kind of preparation method of abrasive material, the preparation method of the abrasive material of a kind of silicon-dioxide of more specifically saying so.
Background technology
Abrasive silica is the main component of the polishing thing of used in electronic industry, as State Intellectual Property Office's on July 27th, 2005 disclosed " the silicon dioxide base CMP composition that contains methyl alcohol " (publication number CN1646651), the polishing composition on February 1st, 2006 disclosed " composition of chemically machinery polished silicon-dioxide and silicon nitride and the method " patent documentations such as (publication number CN1727431) all is main raw material with the abrasive silica.
Usually, silicon dioxide CMP liquid has abrasive silica and a small amount of chemical reagent configuration to form, silica dioxide granule in the abrasive material plays the mechanical grinding effect to polished object, chemical reagent plays corrosive nature to polished object, and the synergy of these two effects makes polished object reach the effect of global planarization.
For improving the polishing speed of polishing fluid, increase particle diameter and improve the mechanical effect that the particulate dispersity can obviously improve polishing fluid, increase the chemical action that chemical agent concentration can improve polishing fluid at an easy rate.Metal ion in the polishing fluid can optionally be adsorbed and enter into the film the inside by some functional film in polishing process, thereby leakage current is increased, and causes the instability of made device.Therefore, make high-quality and efficient polishing fluid key is will be based on the hyperpure abrasive silica of the big particle diameter of high evenness.
Because the abrasive silica particle diameter that is used for the electronic industry polishing is at 20-500nm, and the requirement of silicon-dioxide particle diameter is more even, be that the content of the metal ion of representative is not higher than 2ppm with sodium.And ordinary silicon to hold the silicon-dioxide median size of glue be 5-20nm, and it contains a large amount of metal ions, can not satisfy the requirement of abrasive material.It is the report that raw material is produced silicon sol that domestic literature had with water glass, also once reported the manufacture method of excessive particle diameter silicon sol, as " Tianjin light industry " 1992.1 29-30 pages or leaves disclosed " preparation of volume particle size silicon sol ", but do not see the concrete report of the particles dispersed degree being implemented control.And for example State Intellectual Property Office's on March 16th, 2005, disclosed " preparation method of big particle diameter silicon sol " (publication number CN1594080) document was introduced a kind of preparation method of big particle diameter silicon sol: the water glass after (1) will dilute carries out permutoid reaction by resin cation (R.C.), remove sodium ion and other cation impurity, obtaining concentration is the active silicic acid solution of 4-30%.(2) be 8-11 at pH value, be heated in the alkaline media under the boiling state, add active silicic acid solution, the pH value in the reaction process is controlled in the 8-11 scope, reaction back ageing 1-3h gets 5-10nmSiO2 crystal seed mother liquor, concentration is 4-30%.(3) the crystal seed mother liquor heats under normal pressure and keeps the explosive evaporatoin state, the heating and temperature control scope is 90-110 ℃, stirring and dropping into concentration down is the active silicic acid solution of 4-30%, reaction solution pH value setting range is 8.5-10.5, the concentration of controlling reaction solution by the branch water conservancy project skill of evaporation water outlet is 20-50%, the Zata current potential absolute value that grain is produced in the growth process remains in the 28-30mv scope, and it is 50-70mv that Zata current potential absolute value is finished in reaction, ageing 1-5 hour big particle diameter silicon sol.(4) silicon sol after the ageing is removed the purification process of impurity, obtains the silicon sol finished product.The problem that this kind method exists is: the particle diameter of silicon-dioxide is inhomogeneous, and easy in process of production gel, the also difficult requirement that reaches abrasive material of purity.
Summary of the invention
At the problems referred to above, it is even that the problem that quasi-solution of the present invention is determined provides a kind of grain diameter, the abrasive silica that purity is high.
For achieving the above object, the present invention has adopted following technical scheme: a kind of preparation method of abrasive silica, and it is raw material with water glass, comprises that first pure, crystal seed prepares, increases particle diameter and four steps of purifying:
Pure at the beginning of described is that water glass is diluted to SiO
2Weight content is not higher than 15%, filters, and filtrate is exchanged by resin cation (R.C.), removes sodium ion and other cation impurity;
Described crystal seed preparation is that the liquid after just pure is adjusted to PH8.0-11.0, and heat temperature raising carries out the polymerization of crystal seed to 60-135 ℃ gradually under agitation condition, gets the silicon sol of high evenness after the cooling;
Described increase particle diameter is that the silicon sol of high degree of dispersion that crystal seed is prepared is warming up to 60-135 ℃ under agitation condition, add temperature and be not higher than the pure liquid that obtains at the beginning of 50 ℃, add the just pure liquid control that obtains: reinforced flow be not higher than the silicon sol volume of the high evenness that 4 times of crystal seeds prepare/hour, reinforced flow velocity obtains the silicon-dioxide coarse abrasive at 30-40m/s;
Described purifying is that the silicon-dioxide coarse abrasive is exchanged through resin cation (R.C.) and resin anion(R.A), obtains the finished product abrasive silica.
As improvement, for obtaining the abrasive material that particle diameter more arrives, described increase particle diameter step repeats, being about to increase the silicon-dioxide coarse abrasive that the particle diameter step obtains repeats to be warming up to 60-135 ℃ under agitation condition, add temperature and be not higher than the pure liquid that obtains at the beginning of 50 ℃, add the just pure liquid control that obtains: reinforced flow be not higher than the silicon sol volume of the high evenness that four times of crystal seeds prepare/hour, reinforced flow velocity is at 30-40m/s, increased the silicon-dioxide coarse abrasive of particle diameter once more, this step can repeat repeatedly, reach necessary requirement to the particle diameter of silicon-dioxide till.
Filtration in the described pure step just is ultrafiltration or micro-filtration, and described ultrafiltration or microfiltration membrane are hollow-fibre membrane or shell-and-tube film.After the resin cation (R.C.) of described first pure step exchanges, also carried out resin anion(R.A) and exchanged.In the described pure step just, filter back, the preceding SiO of adjustment of cationic exchange
2Weight content is not higher than 7%.
In the described crystal seed preparation process, pH value is adjusted by liquid is joined in the alkali lye.In the described crystal seed preparation process, heat temperature raising is after 60-135 ℃, and the insulation of also carrying out 0.2-2 hour is aging.
In the described increase particle diameter step, the silicon sol of the high evenness that crystal seed is prepared is after being warming up to 60-135 ℃ under the agitation condition, and the insulation of also carrying out 0.2-2 hour is aging.
The resin cation (R.C.) of described purification step is the positively charged ion that allows existence on exchange zone in the solution, resin anion(R.A) OH
-OH on the exchange zone
-, and mix the dress post, the silicon-dioxide coarse abrasive is passed through to mix exchange column.
The present invention is than prior art, because water glass (NaO
2.NSiO
2..XH
2O) contain a large amount of impurity in, in first pure step, adopted ultrafiltration or micro-filtration, removed a large amount of insoluble impuritiess in the water glass, not only improve the purity of end product, and make reaction process more stable; In increasing the particle diameter step, by controlling the temperature of reinforced flow, flow velocity and material, guarantee to add the silicon dioxide microparticle in the pan feeding and the join probability of seed particles, seed particles is further grown up, and uniform particles.The abrasive material quality index that inventor's test of many times obtains exists: dispersity: PDI＜2.0), particle diameter: 20-500nm, purity: with Na content is representative＜0.5ppm.Satisfy the requirement of electron trade polish abrasive fully.
In the last paragraph, can consult " electron device " that in December, 2004, electron device editorial office published about PDI, the 27th volume, the 4th phase, the 558th page, " the synthetic and applied research of the big particle diameter silicon sol of ULSI CMP of Dielectric nanometer abrasive " literary composition, the dispersity PDI formula of document introduction is: PDI=volume average particle size/quantity median size, PDI is low dispersion system near 1.
Embodiment
1, first pure step:
Selecting modulus for use is the water glass of 2.0-4.0, is diluted with water to SiO
2The % weight content is not higher than 15%.As 15%, 13%, 10%, 8%, 7%, 6%, use ultrafiltration membrance filter, filtrate reaches clarification, transparent, no Tyndall phenomenon, gets filtrate.Described ultra-filtration membrane can be to be 3000 hollow-fibre membrane or shell-and-tube film through molecular weight cut off, and the aperture is＜2um.
Certainly also can adopt the microfiltration membrane of same material according to practical situation.Here need to prove, too high and influence filtration velocity as the too high then viscosity of SiO2 concentration, therefore select suitable filtration concentration according to the situation of raw material.
SiO when filtering as the front
2The % weight content is higher than under 7% the situation, needs water to adjust filter liquor concentration, makes the SiO2 weight content not be higher than 7%, uses resins exchange after treated cation then in exchange column, as uses NH
4 +Resin cation (R.C.) is removed sodium ion and impurity cationic in the water glass, obtains the silicic acid (small-particle acidic silicasol, particle is at 3-5nm) of high-polymerization degree.Owing to resins exchange after the treated cation in the exchange column is being widely used in the art, therefore here be not described in detail, as improvement, after resins exchange after the treated cation, also carry out in the exchange column resins exchange after the anionic treatments, further improved purity.
Now the material that first pure step is obtained is called " A solution ".
2, crystal seed preparation process:
In the solution that is placed with small amount of alkali (soluble metal oxyhydroxide or ammoniacal liquor or organic bases etc.), its alkali is generally less than 0.1 volumetric molar concentration, as 0.8,0.9,0.7.Under abundant agitation condition, add A solution gradually, control PH8.0-11.0.
Then under abundant agitation condition gradually heat temperature raising surpass 100 ℃ to the 60-135 ℃ of polymerization of carrying out crystal seed if heat up, then need in pressurized vessel, carry out.Preferably insulation is aging after the heating, and the insulation aged time is 0.2-2 hour, and it is relevant with heat temperature raising, and the insulation digestion time that needs under the lower situation that general temperature rises is then longer, and as heat temperature raising to 60 ℃, then insulation was worn out 2 hours; Heat temperature raising to 80 ℃, then insulation is aging 1 hour; Heat temperature raising to 100 ℃, then insulation is aging 0.5 hour.Get the silicon sol of high evenness after the cooling.
Now the material that this step is obtained is called " B solution ".
3, increase the particle diameter step
B solution is warming up to 60-135 ℃ under agitation condition, add temperature and be not higher than 50 ℃ A solution, the liquid control that adds A solution: reinforced flow be not higher than 4 times of B liquor capacity amounts/hour, reinforced flow velocity is at 30-40m/s, be preferably in 60-135 ℃ of insulation 0.2-2 hour then, its insulation aging method is aging identical with the insulation in the crystal seed preparation process.Now the material that this step is obtained is called C1 solution.
More stable for controlling this step, can be earlier with B solution with ultrafiltration or evaporation concentration, or thin up makes, and SiO2% regulates PH8.0-11.0 at 0.5-40 with alkali lye in the mother liquor.
As improvement, available C
1Solution substitutes the B solution of preceding step, and other method is the same, and the material that obtains is called C
2Solution.Can repeat repeatedly to obtain C like this
3Solution, C
4Solution C
5Solution ...Till reaching necessary requirement to the particle diameter of silicon-dioxide.
4, purification step
The silicon-dioxide coarse abrasive is exchanged through resin cation (R.C.) and resin anion(R.A), obtain the finished product abrasive silica, this method is being widely used in the art, therefore here is not described in detail.
It is emphasized that the present invention can be: the resin cation (R.C.) of purification step is the positively charged ion that allows existence on exchange zone in the solution, resin anion(R.A) OH
-OH on the exchange zone
-, and mix the dress post, the silicon-dioxide coarse abrasive is passed through to mix exchange column.Remove in the solution foreign ion and the abrasive silica of purifying.
Above-mentioned crystal seed preparation process, increase particle diameter step can be carried out in the 5000L reactor.
Following table be the applicant test each embodiment and abrasive material mass effect table:
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | |
| Just pure | SiO during filtration 2% content | 15 | 13 | 10 | 8 | 7 | 6 | 11 | 9 |
| Filtering membrane | Ultrafiltration | Micro-filtration | Ultrafiltration | Micro-filtration | Ultrafiltration | Micro-filtration | Ultrafiltration | Micro-filtration | |
| Whether use anionic treatments | Be | Not | Be | Not | Be | Not | Be | Not | |
| The crystal seed preparation | Heating temperature (℃) | 60 | 80 | 90 | 70 | 100 | 110 | 125 | 135 |
| Soaking time (hour) | 2 | 1.5 | 1.2 | 1.8 | 1.0 | 0.2 | 0 | 0 | |
| Increase particle diameter | Heating temperature | 60 | 80 | 90 | 70 | 100 | 110 | 125 | 135 |
| Soaking time | 2 | 1.5 | 1.2 | 1.8 | 1.0 | 0.2 | 0 | 0 | |
| Reinforced flow (times mother liquor volume/hour) | 4 | 3 | 2 | 1 | 4 | 3 | 2 | 1 | |
| Reinforced flow velocity (m/s) | 40 | 30 | 32 | 34 | 36 | 38 | 35 | 33 | |
| Increase the particle diameter number of times | 1 | 2 | 3 | 4 | 4 | 3 | 2 | 1 | |
| Purifying | Positively charged ion, anion exchange process | --- | --- | --- | --- | --- | --- | --- | --- |
| Mass effect | Uniformity coefficient (PDI＜) | 2.0 | 1.8 | 1.5 | 1.7 | 1.6 | 1.5 | 1.4 | 1.54 |
| Particle diameter (nm) | 20-30 | 60-80 | 80-120 | 120-160 | 160-180 | 80-120 | 60-80 | 30-50 | |
| (with Na content is representative＜ppm) to purity | 0.45 | 0.44 | 0.43 | 0.43 | 0.44 | 0.45 | 0.44 | 0.43 | |
In the last table, purification step does not change.
Claims (9)
1, a kind of preparation method of abrasive silica, it is raw material with water glass, that its feature comprises is just pure, the crystal seed preparation, increase particle diameter and four steps of purifying:
Pure at the beginning of described is that water glass is diluted to SiO
2Weight content is not higher than 15%, filters, and filtrate is exchanged by resin cation (R.C.), removes sodium ion and other cation impurity;
Described crystal seed preparation is that the liquid after just pure is adjusted to PH8.0-11.0, and heat temperature raising carries out the polymerization of crystal seed to 60-135 ℃ gradually under agitation condition, gets the silicon sol of high evenness after the cooling;
Described increase particle diameter is that the silicon sol of high evenness that crystal seed is prepared is warming up to 60-135 ℃ under agitation condition, add temperature and be not higher than the pure liquid that obtains at the beginning of 50 ℃, add the just pure liquid control that obtains: reinforced flow be not higher than the silicon sol volume of the high evenness that 4 times of crystal seeds prepare/hour, reinforced flow velocity obtains the silicon-dioxide coarse abrasive at 30-40m/s;
Described purifying is that the silicon-dioxide coarse abrasive is exchanged through resin cation (R.C.) and resin anion(R.A), obtains the finished product abrasive silica.
2, the preparation method of abrasive silica according to claim 1 and 2, it is characterized in that described increase particle diameter step is to repeat, being about to increase the silicon-dioxide coarse abrasive that the particle diameter step obtains repeats to be warming up to 60-135 ℃ under agitation condition, add temperature and be not higher than the pure liquid that obtains at the beginning of 50 ℃, add the just pure liquid control that obtains: reinforced flow be not higher than the silicon sol volume of the high evenness that four times of crystal seeds prepare/hour, reinforced flow velocity is increased the silicon-dioxide coarse abrasive of particle diameter once more at 30-40m/s.
3, the preparation method of abrasive silica according to claim 1 and 2 is characterized in that the filtration in the described pure step just is ultrafiltration or micro-filtration, and described ultrafiltration or microfiltration membrane are hollow-fibre membrane or shell-and-tube film.
4, the preparation method of abrasive silica according to claim 1 and 2 after the resin cation (R.C.) that it is characterized in that described pure step just exchanges, has also carried out resin anion(R.A) and has exchanged.
5, the preparation method of abrasive silica according to claim 1 and 2 is characterized in that in the described pure step just, filters back, the preceding SiO of adjustment of cationic exchange
2Weight content is not higher than 7%.
6, the preparation method of abrasive silica according to claim 1 and 2 is characterized in that pH value is adjusted by liquid is joined in the alkali lye in the described crystal seed preparation process.
7, the preparation method of abrasive silica according to claim 1 and 2 is characterized in that in the described crystal seed preparation process, and heat temperature raising is after 60-135 ℃, and the insulation of also carrying out 0.2-2 hour is aging.
8, the preparation method of abrasive silica according to claim 1 and 2, it is characterized in that in the described increase particle diameter step, the silicon sol of the high evenness that crystal seed is prepared is after being warming up to 60-135 ℃ under the agitation condition, and the insulation of also carrying out 0.2-2 hour is aging.
9, the preparation method of abrasive silica according to claim 1 and 2, the resin cation (R.C.) that it is characterized in that described purification step is the positively charged ion that allows existence on exchange zone in the solution, resin anion(R.A) OH
-OH on the exchange zone
-, and mix the dress post, the silicon-dioxide coarse abrasive is passed through to mix exchange column.
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| US20130075651A1 (en) * | 2011-09-16 | 2013-03-28 | Nissan Chemical Industries, Ltd. | Method for producing purified active silicic acid solution and silica sol |
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| US20130075651A1 (en) * | 2011-09-16 | 2013-03-28 | Nissan Chemical Industries, Ltd. | Method for producing purified active silicic acid solution and silica sol |
| CN105800622B (en) * | 2011-09-16 | 2019-07-05 | 日产化学工业株式会社 | The manufacturing method of the activated silica acid solution and silica solution that are purified |
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| CN109135346A (en) * | 2018-09-05 | 2019-01-04 | 中建材蚌埠玻璃工业设计研究院有限公司 | Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof |
| CN112499633A (en) * | 2020-11-27 | 2021-03-16 | 上海都进新材料科技有限公司 | Colloidal silicon dioxide abrasive hardness control method suitable for integrated circuit chemical mechanical polishing |
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