CN106590442A - Preparation method of cerium dioxide polishing powder liquid - Google Patents
Preparation method of cerium dioxide polishing powder liquid Download PDFInfo
- Publication number
- CN106590442A CN106590442A CN201710062616.5A CN201710062616A CN106590442A CN 106590442 A CN106590442 A CN 106590442A CN 201710062616 A CN201710062616 A CN 201710062616A CN 106590442 A CN106590442 A CN 106590442A
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- CN
- China
- Prior art keywords
- preparation
- powder
- solution
- cerium dioxide
- polishing
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Abstract
The invention relates to a preparation method of a cerium dioxide polishing powder liquid. The preparation method comprises the steps: adding cerium dioxide powder into a mixed solution of a silane coupling agent compound and an organic solution, wherein the silane coupling agent compound contains alkoxyl at one end and a polar functional group at the other end, and an organic solvent in the organic solution is an alcohol; and dehydrating and drying the mixed solution to obtain polishing powder and then dissolving the polishing powder in an aqueous solution to obtain the polishing liquid. The cerium dioxide powder generated by the method provided by the invention can be stably and uniformly dispersed in the aqueous solution, is relatively long in suspending time, is unlikely to generate precipitates, can be applied to manufacturing various cerium dioxide related polishing powder slurry and liquid slurry, and has certain industrial application value.
Description
Technical field
The present invention relates to rare earth grinding-material field.For the polishing of optical glass, the polishing of semiconductor wafer.Especially relate to
And a kind of preparation method of ceria polishing powder liquid.
Background technology
Cerio grinding-material is widely used as the grinding of glass material with material.Particularly in recent years mobile phone glass and
Liquid crystal display (LCD), photomask etc. are electric, the Fast Growth of electronic device field, used as the grinding material of their glass substrates
Material increase in demand.With the continuous development of industry manufacturing technology, for the grinding of the glass such as substrate requires there is higher grinding
Mill speed and more preferable surface accuracy.Require that grinding-material has higher recycling performance simultaneously.
In addition particularly during manufacture of semiconductor, the grinding milk that cerium dioxide powder is formed in aqueous is easily
Generation coacervation, is agglomerated into larger granule and rapid subsidence, causes the effectively reduction of grinding matter in grinding milk, concentrates body
The time that now grinding sizing material is floated in aqueous solution is short, and stability is bad, thus reduces grinding efficiency, and grinds batch
Between unstability it is fairly obvious.
So developing a kind of stable performance, grinding efficiency is high, and the grinding milk that can be floated for a long time in aqueous becomes
One problem extremely protruded.
The content of the invention
The technical problem to be solved is to provide a kind of preparation method of ceria polishing powder liquid, prepares gained
The cerium oxide powder for arriving, can in aqueous stablize and be uniformly dispersed, and with longer suspension time, be not likely to produce
Precipitation.
For achieving the above object, the present invention employs the following technical solutions realization：
A kind of preparation method of ceria polishing fluid, cerium dioxide powder is added silane based coupling agents compound and is had
In the mixed solution of machine solution, the silane based coupling agents compound contains alkoxyl for one end, and one end contains polar functional group；Institute
It is alcohols to state organic solvent in organic solution；Cerium oxide powder is 1 with the mixing ratio of silane based coupling agents compound：1～1.0
Polishing powder is obtained after mixed solution dehydrate, then polishing powder is dissolved in aqueous solution, that is, obtain polishing fluid.
Described silane based coupling agents compound is N-3- trimethoxy silicon propyl group ethylenediamines.
Described organic solvent is ethanol.
The volume of described ethanol is the 50%-99% of organic solution cumulative volume.
Contain salt, inorganic matters, You Jijin in described silane based coupling agents compound and the mixed solution of organic solution
Category compound.
Ceria surface is modified using silane based coupling agents compound, makes ceria and coupling agent generation table
Face is bonded, and increases stability.Amido functional group is polarity, can be the functional group dissolved in aqueous, is very easy to and water
With reference to.In addition alkoxyl is contained in one end in the amino compound containing silicon, thus can with cerium dioxide powder surface bond,
Therefore the polishing powder from rare earth liquid for thus constituting can be uniformly swum in water.
Compared with prior art, the invention has the beneficial effects as follows：
Cerium oxide powder obtained by the method according to the invention, can in aqueous stablize and be uniformly dispersed,
And with longer suspension time, precipitation is not likely to produce, can be applicable to make various cerias related polishing slurry, liquid
Slurry, with certain industry using value.
Description of the drawings
Fig. 1 is embodiment, and comparative example ceria Floating Height changes over figure.
Fig. 2 is embodiment, and comparative example ceria Zeta potential is with PH variation relations.
Specific embodiment
With reference to embodiment, the present invention is further described：
Following examples describe the present invention.These embodiments are only that preferred embodiment of the invention is entered
Row description, does not limit the scope of the present invention.
The preparation method of ceria polishing fluid, by cerium dioxide powder silane based coupling agents compound (N-3- tri- is added
Methoxyl group silicon propyl group ethylenediamine) with the mixed solution of ethanol solution in, cerium oxide powder and N-3- trimethoxy silicon propyl group second
The mixing ratio of diamidogen is 1：1～1.0, the volume of ethanol is the 50%-99% of cumulative volume in ethanol solution.Contain in mixed solution
Salt, inorganic matters, organo-metallic compound.This mixed liquor is placed in into ultrasound 10min in ultrasound wave pond, then 70 DEG C of water-baths again
Middle stirring 120min, then dewatering and filtering, with sewage washing with alcohol three times, is placed in 80 DEG C of baking oven and is dried to obtain polishing powder,
Then polishing powder is dissolved in aqueous solution, that is, obtains polishing fluid.
Embodiment 1
100ml is added to contain 99% volume ratio 2g cerium oxide powders and 0.8gN-3- trimethoxy silicon propyl group ethylenediamine
Ethanol solution in mix, and this mixed liquor is placed in into ultrasound 10min in ultrasound wave pond, then in 70 DEG C of stirred in water bath
120min, then dewatering and filtering, with sewage washing with alcohol three times, is placed in 80 DEG C of baking oven and is dried to obtain powder sample.
Embodiment 2
100ml is added to contain 95% volume ratio 2g cerium oxide powders and 1.0gN-3- trimethoxy silicon propyl group ethylenediamine
Ethanol solution in mix, and this mixed liquor is placed in into ultrasound 10min in ultrasound wave pond, then in 70 DEG C of stirred in water bath
120min, then dewatering and filtering, with sewage washing with alcohol three times, is placed in 80 DEG C of baking oven and is dried to obtain powder sample.
Embodiment 3
100ml is added to contain 50% volume ratio 2g cerium oxide powders and 2gN-3- trimethoxy silicon propyl group ethylenediamine
Mix in ethanol solution, and this mixed liquor is placed in into ultrasound 10min in ultrasound wave pond, then in 70 DEG C of stirred in water bath
120min, then dewatering and filtering, with sewage washing with alcohol three times, is placed in 80 DEG C of baking oven and is dried to obtain powder sample.
Comparative example 1
2g cerium oxide powders and 0.8gN-3- trimethoxy silicon propyl group ethylenediamine are added in 100ml aqueous solutions and are mixed,
And this mixed liquor is placed in into ultrasound 10min in ultrasound wave pond, it is then dehydrated then in 70 DEG C of stirred in water bath 120min
Filter, with sewage washing with alcohol three times, is placed in 80 DEG C of baking oven and is dried to obtain powder sample.
Comparative example 2
2g cerium oxide powders addition 100ml is also had in the ethanol solution of 95% volume ratio and is mixed, and by this mixed liquor
Ultrasound 10min in ultrasound wave pond is placed in, then in 70 DEG C of stirred in water bath 120min, then dewatering and filtering, uses sewage ethanol
Washing three times, is placed in 80 DEG C of baking oven and is dried to obtain powder sample.
Embodiment and comparative example method of testing：
Take sample each two grams, be placed in the graduated cylinder containing 100ml pure water, use Glass rod mix homogeneously, stand, measure area's keyed
The height of time change floating thing, acquired results Floating Height is changed over as shown in Figure 1：Embodiment after 200 hours
The only a little sedimentations of 1-3, and comparative example 1 then has after 25 hours half or so to settle, and settles completely later within 50 hours.Comparative example
2 settle quickly within 10min.The more explanation solidss of bottom precipitum suspension in the solution is poor, therefore can be with table
Ceria polishing powder liquid suspension obtained by bright this patent method is good.
The mixed aqueous solution of the sample preparation of 1-3 examples and comparative example 1 into 5% will be implemented stir in tabular order wherein to mix homogeneously
Afterwards, pH value is adjusted by 3-11, measure the Zeta potential situation of change of solution, such as accompanying drawing 2 and shown with HCl and NaOH：From on figure
It can be seen that the current potential of embodiment 1-3 is almost unchanged before 8, and slightly reduce between 8-11, but be all positive potential, and it is right
Ratio 1 was positive potential before 8, was nagative potential after 8, and this detection shows that the inventive method can change ceria surface
Current potential, and resulting polishing powder liquid has the wider PH scope of applications.
Claims (4)
1. a kind of preparation method of ceria polishing fluid, it is characterised in that cerium dioxide powder is added into silane based coupling agents
In the mixed solution of compound and organic solution, the silane based coupling agents compound contains alkoxyl for one end, and one end contains pole
Property functional group；Organic solvent is alcohols in the organic solution；Polishing powder is obtained after mixed solution dehydrate, then will
Polishing powder is dissolved in aqueous solution, that is, obtain polishing fluid.
2. a kind of preparation method of ceria polishing fluid according to claim 1, it is characterised in that described silylation
Coupler compound is N-3- trimethoxy silicon propyl group ethylenediamines.
3. the preparation method of a kind of ceria polishing fluid according to claim 1, it is characterised in that described is organic molten
Agent is ethanol.
4. the preparation method of a kind of ceria polishing fluid according to claim 3, it is characterised in that described ethanol
Volume is the 50%-99% of organic solution cumulative volume.
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| CN201710062616.5A CN106590442A (en) | 2017-01-22 | 2017-01-22 | Preparation method of cerium dioxide polishing powder liquid |
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| CN201710062616.5A CN106590442A (en) | 2017-01-22 | 2017-01-22 | Preparation method of cerium dioxide polishing powder liquid |
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Citations (8)
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| TW539741B (en) * | 2002-04-26 | 2003-07-01 | Everlight Chem Ind Corp | Method for manufacturing cerium dioxide powder |
| CN1480503A (en) * | 1997-12-18 | 2004-03-10 | 日立化成工业株式会社 | Abradant, grinding method for substrate, and mfg. method for semiconductor device |
| CN1699282A (en) * | 2005-06-09 | 2005-11-23 | 江苏工业学院 | Preparation of monodisperse spherical cerium oxide and its application in high precision polishing |
| CN101224397A (en) * | 2007-10-12 | 2008-07-23 | 南京航空航天大学 | Nanometer ceria sizing agent and preparing method thereof |
| CN101659850A (en) * | 2009-09-22 | 2010-03-03 | 中国科学院上海微系统与信息技术研究所 | Modified nanometer cerium oxide and preparation and application thereof |
| CN102775958A (en) * | 2012-08-16 | 2012-11-14 | 上海华明高纳稀土新材料有限公司 | Cerium oxide polishing material for stone grinding tool and preparation method thereof |
| US20150184027A1 (en) * | 2012-11-07 | 2015-07-02 | Grirem Advanced Materials Co., Ltd. | Cerium oxide based composite polishing powder and preparation method thereof |
| CN106277020A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of bigger serface micron cerium oxide preparation method |
-
2017
- 2017-01-22 CN CN201710062616.5A patent/CN106590442A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480503A (en) * | 1997-12-18 | 2004-03-10 | 日立化成工业株式会社 | Abradant, grinding method for substrate, and mfg. method for semiconductor device |
| TW539741B (en) * | 2002-04-26 | 2003-07-01 | Everlight Chem Ind Corp | Method for manufacturing cerium dioxide powder |
| CN1699282A (en) * | 2005-06-09 | 2005-11-23 | 江苏工业学院 | Preparation of monodisperse spherical cerium oxide and its application in high precision polishing |
| CN100351179C (en) * | 2005-06-09 | 2007-11-28 | 江苏工业学院 | Preparation of monodisperse spherical cerium oxide and its application in high precision polishing |
| CN101224397A (en) * | 2007-10-12 | 2008-07-23 | 南京航空航天大学 | Nanometer ceria sizing agent and preparing method thereof |
| CN101659850A (en) * | 2009-09-22 | 2010-03-03 | 中国科学院上海微系统与信息技术研究所 | Modified nanometer cerium oxide and preparation and application thereof |
| CN102775958A (en) * | 2012-08-16 | 2012-11-14 | 上海华明高纳稀土新材料有限公司 | Cerium oxide polishing material for stone grinding tool and preparation method thereof |
| US20150184027A1 (en) * | 2012-11-07 | 2015-07-02 | Grirem Advanced Materials Co., Ltd. | Cerium oxide based composite polishing powder and preparation method thereof |
| CN106277020A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of bigger serface micron cerium oxide preparation method |
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Application publication date: 20170426 |