CN107010631A - A kind of aspherical cataloid nanometer grain preparation method - Google Patents
A kind of aspherical cataloid nanometer grain preparation method Download PDFInfo
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- CN107010631A CN107010631A CN201610060268.3A CN201610060268A CN107010631A CN 107010631 A CN107010631 A CN 107010631A CN 201610060268 A CN201610060268 A CN 201610060268A CN 107010631 A CN107010631 A CN 107010631A
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- aspherical
- cataloid
- water glass
- preparation
- nanometer grain
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/142—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates
- C01B33/143—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates of aqueous solutions of silicates
- C01B33/1435—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates of aqueous solutions of silicates using ion exchangers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention provides a kind of aspherical cataloid nanometer grain preparation method, this method is based on modified ion-exchange, the time being slowly added into cationic ion-exchange resin within the temperature range of 40 to 70 degrees Celsius when preparing silicic acid in the dilution water glass solution being sufficiently stirred for is more than half an hour, reach that its pH value is less than 3, according still further to the growth of normal ion-exchange, i.e. comprising forming mother liquor and growing the process based on amplifying step by step, a kind of colloidal silica nano silicon particles of aspherical are ultimately formed.A kind of aspherical colloidal silica nano silicon particles prepared by the present invention, be particularly suitable for use in polishing field superhard material, such as sapphire CMP process.
Description
Technical field
The present invention relates to a kind of aspherical colloidal silica silicon preparation method, more particularly to a kind of aspherical colloidal silica
Nano silicon particles preparation method, belongs to CMP process field, especially belongs to superhard material polishing field.
Background technology
Colloidal silica nano silicon particles are widely used in printing, papermaking, photograph, coating, hot investment casting, chemical machinery throwing
The all trades and professions such as light.At present, main flow preparation method mainly has ion-exchange, organosilicon hydrolyzation method, elemental silicon Hydrolyze method, electric osmose
Analysis method etc..Commercially available prod particle diameter 5-200nm, solid content≤50%, pattern is in perfect spherical.
The big application of the one of colloidal silica nano silicon particles is the nanometer in chemically mechanical polishing (CMP) technique polishing fluid
Abrasive material.CMP is under a certain pressure, using the chemical action of chemical analysis in polishing fluid, to be carried out first with polishing material surface
Chemical reaction, forms the matter soft formation easily removed, then rub by being contacted between the abrasive material and polishing material in polishing pad, polishing fluid
Wiping is acted on, and removes the matter soft formation of early stage formation.Finally, through rolling action of the porous polishing pad by polishing fluid, polishing is gone
The material removed takes away polishing material surface, exposes fresh surface, further reacts and removes again again, preferential again and again to remove
Surface convex portion, so as to reach polishing effect.
Cataloid is played most important as most widely used nanometer abrasive in CMP planarization liquid to CMP performances
Effect.Particularly with needing easily, the matter of a few hours or even dozens of hour processing is hard, (such as indigo plant is precious for chemical inertness superhard material
Stone), the effect of nanometer abrasive is particularly important.To lift the processing efficiency to superhard material, the developing direction of nanometer abrasive is main
There are two：1. increase abrasive hardness.2. increase the frictional behaviour of abrasive material in the case of not changing abrasive hardness.By adopting in direction 1
Superhard material processing efficiency generally can be significantly lifted very much with the bigger nanometer abrasive of hardness (such as diamond, aluminum oxide),
But often significantly sacrifice the surface quality after processing.Therefore popularization of the method in precise polished is limited always, and only
Some popularizations are obtained in coarse polishing.Abrasive material is used as by using the cataloid of aspherical so that polishing in direction 2
During occur sliding friction rather than rolling friction, can more efficiently complete the processing to superhard material.To obtain aspherical
Colloidal silica particles, existing trial is induced and growth technique when being concentrated mainly on growth crystal seed using ion
Shi Caiyong gradient processes condition (such as local temperature, pressure be not equal).Ion induction method is difficult to be formed the colloid two more than 50nm
Silicon oxide particle, and there is injury effect in stability of the ionic strength to cataloid in itself；Gradient processes conditioned growth
Then more it is difficult to be controlled technique.Therefore, both approaches are difficult to obtain large-scale application.
In terms of silicon dioxide gel preparation, patent CN 1974385B, it is entitled that " a kind of monodispersive silica is molten
The patent of the preparation method of glue ", mainly protects and goes to prepare single dispersing Ludox using silica flour method, and its parent material is silicon
Powder, is grown to monodisperse spherical Ludox by base catalysis in a heated condition；Patent CN 1183379A use reverse micelle solvent
Method prepares nanometer silicon dioxide particle, and the core of this method is organic for the reverse micelle and polarity of mating surface activating agent formation
Phase control forms porous, spherical nano-silicon dioxide.This two patents are to submit spherical and porous silica silica sol granule,
Belong to traditional preparation methods.
And inventor herein is directed to preparing the colloidal silica particles of aspherical, for the key technology of the present invention
Point, has carried out deep document and patent retrieval, and the higher document of the degree of correlation is as follows：
(1) number of patent application is 200610155112.X, a kind of entitled " preparation side of monodispersive silica sol
The method that a kind of silica flour of patent protection of method " prepares monodisperse silica colloidal sol；Its technological deficiency is：1. silica flour is difficult to react
Completely, the Ludox prepared in this approach can engender black floating object residue with standing time, both influenceed outward appearance or limited
It is many high-end such as the application of polishing fields；2. the Ludox that prepared by this method is in monodisperse spherical, and can not accomplish this
The aspherical particle of patent application.
(2) number of patent application is 97125800.7, entitled " to prepare nanometer silicon dioxide particle from the silicate of alkali metal
Method " a kind of reverse micelle solvent method for preparing nanometer silicon dioxide particle of patent protection；Its technological deficiency is：1. this method
The Ludox organic residue of preparation is difficult to complete removal, there is mortal injury for the polishing field that this patent is applied；2. the party
Ludox prepared by method is porous, not fine and close, and friction efficiency is low in polishing application；3. the Ludox that prepared by this method is in single point
Dissipate spherical, and the aspherical particle of present patent application can not be accomplished.
Inventor herein has found through widely studied, delays cationic ion-exchange resin under certain temperature when preparing silicic acid
Slow be added in the dilution water glass solution being sufficiently stirred for pH value is less than 3, and this silicic acid is carried out into ion-exchange normal growth
After can obtain on pattern be in aspherical colloidal silica nano silicon particles.The aspherical cataloid prepared by the present invention is received
Rice grain, the CMP process for polishing field superhard material (such as sapphire) that be particularly suitable for use in.
The content of the invention
The purpose of the present invention is to improve the existing cataloid for using aspherical as the polishing process of abrasive material to roll
Dynamic friction rather than sliding friction, it is difficult to be formed colloidal silica particles and ionic strength more than 50nm in itself to colloid two
There is the technological deficiency based on injury in the stability of silica, using improved ion-exchange, there is provided a kind of aspherical colloid
Nano SiO 2 particle preparation method.
A kind of aspherical cataloid nanometer grain preparation method of the present invention, including two steps：
Step 1: the preparation of silicic acid：In cationic ion-exchange resin to be slowly added into be sufficiently stirred for dilute under certain temperature
Release in water glass solution to pH value less than 3；
Step 2: using the silicic acid prepared in step one, carry out normal ion-exchange growth, i.e., it is main to include being formed
Mother liquor and step by step growth amplification, ultimately form a kind of aspherical colloidal silica nano silicon particles.
Silicic acid preparation temperature model in a kind of aspherical cataloid nanometer grain preparation method that the present invention is provided
Enclose for 40-70 DEG C, preferably 40-50 DEG C.
Temperature it is too high (>70 DEG C), because of silicic acid and the fragile stability of small-grain-diametersilica silica sol, easily occur gel in preparation process
Phenomenon.And temperature it is too low (<40 DEG C), waterglass is converted to the unsteady state (pH value undergone during acidic silicic acid by alkalescence
4-7), sufficient heat energy induction is not obtained, it is impossible to form aspherical crystal seed.
It is used for the dilute of silicic acid preparation in a kind of aspherical cataloid nanometer grain preparation method that the present invention is provided
Modulus of water glass scope is released for 2-4, preferably 2-3.
Modulus of water glass it is too low (<2), the silicic acid concentration of preparation is too low, low yield；Modulus of water glass it is too high (>4), easily
Generation stability problem.
In a kind of aspherical cataloid nanometer grain preparation method that the present invention is provided in the preparation process of silicic acid,
Resin cation adds the water glass solution time more than 0.5 hour, preferably greater than 1 hour.
In conventional ion exchange process, silicic acid preparation technology flows through cation exchange column to dilute under water glass solution normal temperature.
General cation exchange column exchangeable sodium ion concentration is far above sodium content in dilution water glass solution, therefore dilution waterglass is molten
The moment sodium ion that liquid flows through cation exchange column is exchanged for hydrogen ion, pH value and is changed into acidity by alkalescence；And this hair
Resin cation is is slowly added to water glass solution by bright silicic acid preparation method, and early stage, water glass solution content was relative to cation
Exchanger resin is excessive, therefore there is a pH value by the alkaline gradual change for being changed into acidity from water glass solution to silicate solution
Journey.By controlling addition speed of the cationic ion-exchange resin into dilution water glass solution, it is ensured that whole solution system is crossed over
The time of (pH value 4-7) is to be sufficiently formed aspherical colloidal silica silicon seed between pH value unstable region.
A kind of aspherical cataloid nanometer grain preparation method that the present invention is provided, the aspherical glue finally prepared
Body nano SiO 2 particle scope is 5-180 nanometers.
Beneficial effect
The present invention proposes a kind of aspherical cataloid nanometer grain preparation method, has the advantages that：
1. aspherical cataloid nanometer grain preparation method proposed by the present invention is undergone by silicic acid preparation process
PH value unstable region (pH value 4-7), induced synthesis aspherical crystal seed, then to be finally grown to through ion-exchange aspherical silicon molten
Glue, and injury effect is not present to the stability of cataloid；
2. a kind of aspherical cataloid nanometer grain preparation method proposed by the present invention can than ion induction method
Realize the colloidal silica particles more than 50nm so that sliding friction rather than rolling friction occur in polishing process, can be more
The processing to superhard material is effectively completed, with higher polishing efficiency during for grinding hard materials；
3. a kind of aspherical cataloid nanometer grain preparation method proposed by the present invention can enter to processing technology
Row effectively control, specific controllable parameter is that temperature, dilution modulus of water glass scope and resin cation add water glass solution
Time；So that obtained nano SiO 2 particle, is particularly suitable for use in polishing field superhard material (such as sapphire)
CMP process.
Brief description of the drawings
Fig. 1 be with the embodiment of the present invention 1 with a kind of aspherical cataloid nanometer grain preparation method of the invention
Compared to a kind of design sketch for preparing of conventional colloidal silica nano silicon particles；
Fig. 2 be and a kind of aspherical cataloid nanometer grain preparation method of the invention in the embodiment of the present invention 2
Prepare design sketch.
Embodiment
The present invention will be further described in detail in by the following example, and the following example is only used for illustrating this hair
It is bright, without being imposed any restrictions to the scope of the present invention, modification and change that any one skilled in the art can realize easily
Change is included in the present invention and scope of the following claims.
Embodiment 1
It is prepared by a kind of conventional colloidal silica nano silicon particles：It is 2.2, silica by 8Kg moduluses under normal temperature condition
Content is 4wt% water glass solution, flows through the commercially available cationic ion-exchange resins of 1Kg.After 15min, gained silicic acid pH value is 2.87.
Above-mentioned gained silicic acid is taken, pH value is adjusted to heating stirring 1h under the conditions of 8.5,80 DEG C with ammoniacal liquor, conventional colloid can be obtained
Nano SiO 2 particle (see the SEM photograph in Fig. 1).The silica nanometer it can be seen from the SEM photograph in Fig. 1
Grain uniform particle sizes, in perfection it is spherical, particle diameter is about 25nm.
Embodiment 2
A kind of aspherical cataloid nanometer grain preparation method of the present embodiment：
Under the conditions of 40 DEG C, the modulus that the commercially available cationic ion-exchange resins of 1Kg are slowly added to be sufficiently stirred for is 2.2, dioxy
SiClx content is 4wt% 8Kg water glass solutions, and cationic ion-exchange resin is added completely after about 1.5h, and gained silicic acid pH value is
2.85。
Above-mentioned gained silicic acid is taken, pH value is adjusted to heating stirring 1h under the conditions of 8.5,80 DEG C with ammoniacal liquor, aspherical glue can be obtained
Body nano SiO 2 particle (See Figure SEM photograph).The nano SiO 2 particle pattern it can be seen from the SEM photograph
Different from comparative example 1, in obvious aspherical, the narrow region of particle is about 20-30nm, but length and cohesive size size are not
One.
Fig. 2 is a kind of design sketch of aspherical colloidal silica nano silicon particles obtained by the present embodiment.
Embodiment 3：Polish application examples
2 inches of C are polished to Sapphire Substrate and tested.
Instrument：Brook CP-4 polishing machines
Condition：Pressure (Down Force)：5psi
Polishing pad rotating speed (Pad Speed):100rpm
Rubbing head rotating speed (Carrier Speed):100rpm
Temperature：25℃
Polish flow velocity (Feed Rate)：50ml/ minutes
Polishing time：2 hours
Polishing fluid：Comparative example 1 and the Ludox of embodiment 1 are taken, SiO2 solid contents are diluted to for 20wt%, it is molten with NaOH
Liquid adjusts pH value to 10.0.
The front and rear Sapphire Substrate tablet quality of polishing is weighed using assay balance (precision 0.1mg), it is close to sapphire according to C
Degree, area, thickness change and polishing time change into corresponding polishing speed.
Polish test result as shown in table 1 below.
The polishing test result contrast of the embodiment of table 1 and comparative example
As can be seen from Table 1, under similarity condition, thrown using obtained by the aspherical colloidal silica nano silicon particles of embodiment 2
Light liquid, sapphire polishing speed is 5.0um/h；And use and thrown obtained by the conventional ball colloidal silica nano silicon particles of embodiment 1
Light liquid, sapphire polishing speed is 2.3um/h.And after both have thrown, surface quality of sapphire is suitable.It can thus be seen that making
The aspherical colloidal silica particles prepared with this patent provider method, compared to conventional ball colloidal silica particles,
Can in the case where not influenceing surface quality, greatly improve the sapphire polishing efficiency of superhard material.
Embodiment described above is preferable for a kind of aspherical cataloid nanometer grain preparation method of the invention
Embodiment, the present invention should not be limited to the embodiment and accompanying drawing disclosure of that.It is every not depart from institute's public affairs of the invention
The equivalent or modification completed under the spirit opened, both falls within the scope of protection of the invention.
Claims (5)
1. a kind of aspherical cataloid nanometer grain preparation method, it is characterised in that：
Including following two steps：Step 1: the preparation of silicic acid：Cationic ion-exchange resin is slowly added at a certain temperature
So far the pH value that water glass solution is diluted in the dilution water glass solution being sufficiently stirred for is less than 3；
Step 2: the silicic acid prepared using step one, carries out normal ion-exchange growth, i.e., including forming mother liquor and step by step
Process based on growth amplification, until forming a kind of aspherical colloidal silica nano silicon particles.
2. a kind of aspherical cataloid nanometer grain preparation method according to claim 1, is further characterized in that：
Silicic acid preparation temperature scope in the step one is 40-70 DEG C；
Wherein, silicic acid preparation temperature scope preferably is 40-50 DEG C.
3. a kind of aspherical cataloid nanometer grain preparation method according to claim 1, is further characterized in that：
Dilution modulus of water glass scope in the step one is 2-4；
It is preferred that dilution modulus of water glass scope be 2-3.
4. a kind of aspherical cataloid nanometer grain preparation method according to claim 1, is further characterized in that：
Resin cation in the step one added the water glass solution time more than 0.5 hour；
It is preferred that resin cation add the water glass solution time be more than 1 hour.
5. a kind of aspherical cataloid nanometer grain preparation method according to claim 1, is further characterized in that：
A kind of aspherical cataloid nanoparticle range prepared in the step 2 is 5-180nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110217799A (en) * | 2018-03-02 | 2019-09-10 | 中国石油化工股份有限公司 | Silica solution and preparation method thereof |
| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
| CN111373006A (en) * | 2017-11-17 | 2020-07-03 | 信越化学工业株式会社 | Polishing agent for synthetic quartz glass substrate and polishing method for synthetic quartz glass substrate |
| CN114605923A (en) * | 2022-03-22 | 2022-06-10 | 深圳清华大学研究院 | Large-size silicon edge polishing solution and preparation method thereof |
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| TW201018644A (en) * | 2008-11-07 | 2010-05-16 | Jgc Catalysts & Chemicals Ltd | Non-orbicular silica sol, preparation method thereof and polishing composition using the same |
| CN102390837A (en) * | 2011-08-03 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Preparation method of nonspherical nanometer-scale silica sol |
| CN103896287A (en) * | 2012-12-28 | 2014-07-02 | 上海新安纳电子科技有限公司 | Non-spherical silicon dioxide sol and preparation method thereof |
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| US20080038996A1 (en) * | 2006-08-14 | 2008-02-14 | Nippon Chemical Industrial Co., Ltd. | Polishing composition for semiconductor wafer, production method thereof, and polishing method |
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| TW201018644A (en) * | 2008-11-07 | 2010-05-16 | Jgc Catalysts & Chemicals Ltd | Non-orbicular silica sol, preparation method thereof and polishing composition using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111373006A (en) * | 2017-11-17 | 2020-07-03 | 信越化学工业株式会社 | Polishing agent for synthetic quartz glass substrate and polishing method for synthetic quartz glass substrate |
| CN111373006B (en) * | 2017-11-17 | 2022-04-26 | 信越化学工业株式会社 | Polishing agent for synthetic quartz glass substrate and polishing method for synthetic quartz glass substrate |
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| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
| CN114605923A (en) * | 2022-03-22 | 2022-06-10 | 深圳清华大学研究院 | Large-size silicon edge polishing solution and preparation method thereof |
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