CN1817997A - Nanometer silicon nitride polishing composition and production thereof - Google Patents
Nanometer silicon nitride polishing composition and production thereof Download PDFInfo
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- CN1817997A CN1817997A CN 200610033127 CN200610033127A CN1817997A CN 1817997 A CN1817997 A CN 1817997A CN 200610033127 CN200610033127 CN 200610033127 CN 200610033127 A CN200610033127 A CN 200610033127A CN 1817997 A CN1817997 A CN 1817997A
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Abstract
A nanometer silicon nitride polishing composition and its production are disclosed. The composition consists of surface modified nanometer silicon nitride 1~8wt%, coupling agent of organic titanate 0.1~1.0wt%, pentaerythritol ester stearate 0.1~2wt%, glycerin monomer ester palmitate 0.1~1wt% and base oil residue. It is simple, has better finish degree and no impurity.
Description
Technical field
The present invention relates to a kind of nanometer silicon nitride polishing composition that is used to polish high hardness material, the invention still further relates to the preparation method of this nanometer silicon nitride polishing composition.
Background technology
Nano-silicon nitride has characteristics such as high strength, wear-resisting, heat-resisting, heat shock resistance and self-lubricating, is one of best abrasive material of various high hardness materials, and it is applicable to the grinding and the polishing of high hardness material.
Chinese patent application number is 02117756.2, publication number is CN1384166A, denomination of invention is " polishing composition and the finishing method thereof that are used for the memory, hard disk and magnetic head surface finish ", a kind of polishing composition that is used for the memory, hard disk and magnetic head polishing is disclosed, it is characterized in that, this polishing composition comprises following component at least: (1) is selected from a kind of abrasive material in diamond, silicon-dioxide, aluminum oxide, cerium oxide, zirconium white, titanium oxide, silicon nitride and the Manganse Dioxide of nanometer scale or the combination of multiple abrasive material, accounts for the 0.01-50% of gross weight; (2) mineral oil of alkane or synthetic oil account for the 50-99.99% of gross weight; (3) buffer components accounts for the 0-50% of gross weight, and the pH value that makes described polishing composition is 6-8.The polishing composition of this invention can be used for the rough polishing or the finishing polish of memory, hard disk and magnetic head, or is similar to the metal or the nonmetallic surface of head surface.Because the buffering component of one of main component of this invention uses some alkalescence or acidic substance, become salt in the polishing fluid neutralization, and become impurity or pollutent, thereby polluted the surface of polished material.
Summary of the invention
The objective of the invention is shortcoming at prior art, a kind of super finishing polish nanometer silicon nitride polishing composition that is used to polish high hardness material is provided, make polished material surface reach the smooth finish of super minute surface, and in polishing process, do not have impurity or the polished material surface of contaminants.
Another object of the present invention provides the preparation method of above-mentioned nanometer silicon nitride polishing composition.
The present invention seeks to realize like this:
A kind of nanometer silicon nitride polishing composition, its component and weight percent content be,
The nano-silicon nitride 1%～8% of surface modification
Titanate coupling agent 0.1%～1.0%
Pentaerythritol stearate 0.1%～2%
Glycerine list n-Hexadecane acid esters 0.1%～1%
Base oil 88%～98.7%.
The nano-silicon nitride of described surface modification is the nano-silicon nitride through the polyoxyethylene surface modification.
The particle diameter of described nano-silicon nitride is 20～40nm.
Described base oil is the mineral oil of C4～C8 alkane.
Another object of the present invention is achieved in that a kind of preparation method of above-mentioned nanometer silicon nitride polishing composition, and it comprises the steps:
(1) be 1 by weight: the nano-silicon nitride of 10-15 and deionized water are put into the ball mill ball milling; Be that 1: 0.12～0.15 weight ratio adds polyoxyethylene, ball milling again by nano-silicon nitride and polyoxyethylene then; Will the nano-silicon nitride slurry behind ball milling emit and dewater, the nano-silicon nitride drying after will dewatering be again used the pulverizer high speed pulverization at last, promptly gets the nano-silicon nitride of surface modification;
(2) with total polishing composition weight percent meter, the base oil with 88%～98.7% is divided into three parts;
In first part's base oil, with total polishing composition weight percent meter, add 0.1～1.0% titanate coupling agent, allow it fully dissolve;
In the second section base oil, add additive,, wherein add 0.1%～2% pentaerythritol stearate, add 0.1%～1% glycerine list n-Hexadecane acid esters with total polishing composition weight percent meter;
(3) two kinds of solution with step (2) mix, and then, with total polishing composition weight percent meter, the nano silicon nitride silicon powder of the surface modification of adding 1%～8% is placed on the ultra-sonic dispersion machine again and is dispersed into slurry;
(4) third part base oil in the slurry of step (3) gained is mixed with mixed solution in container, stirs, promptly get nanometer silicon nitride polishing composition.
Advantage of the present invention:
1. nano-silicon nitride of the present invention mixes polishing, and to be combined as the polishing Vickers' hardness be 2500～9000 high hardness material, makes its material surface reach the smooth finish of super minute surface, and promptly polished thing surface roughness Ra is≤5nm.Its detection method is " a super scanning electron microscope of emission " scanning, and its equipment is HITACHI/S-5200 ultrahigh resolution scanning electronic microscope.
2. among the preparation method of the present invention the purpose of nano silicon nitride silicon face by the polyoxyethylene modification be on the source of material be nano-silicon nitride under dry powder, make it to become the powder of high dispersing, thereby lay a good foundation for post-order process.
3. the characteristic with self-lubricating of nano silicon nitride silicon powder among the preparation method of the present invention, nano-silicon nitride is wetting at the basal liquid medium easily, thus the nano silicon nitride silicon grain of surface modification can disperse in polishing composition well.
4. workpiece must place polished thing on the mill (polishing disk) in polishing process, and nano-silicon nitride is a kind of fully suspension after the process magnetic agitation, and the suspension of high dispersing is used for polishing so that be ejected on the polished thing fully; Simultaneously still when the nano-silicon nitride that need be pressed on mill in the composition, the precipitation from homogeneous solution on mill that it must fully highly loose in 24 hours is pressed into mill and uses for polishing so that will homogeneously precipitate in nano-silicon nitride on the mill.This should stirring suspension the characteristic of static precipitation from homogeneous solution again, requirement must be added various additives in base oil, as:
1. pentaerythritol stearate: play precipitation, lubrication.
2. glycerine list n-Hexadecane acid esters: play stable dispersion, the froth breaking effect.
5. it is strong and be easy to improve the characteristics that focus on the ability of concentrating that ultrasonic wave has beam, consequently produce effects such as machinery, heat, light, electrochemistry, the localized hyperthermia that produces when particularly utilizing ultrasonic cavitation, high pressure or strong shock wave and microjet etc., the intergranular interaction energy of nano-silicon nitride that greatly weakened, thereby dispersing nanometer silicon nitride effectively.
6. because basic oil viscosity is slightly high, can not more ground abundant solubilising additive, thereby influence the addition of additive and cause influencing polishing efficiency.Need add titanate coupling agent for this reason.Titanate coupling agent is the both sexes structural materials, its polar group can react with base oil molecules, form and strongly close by force, and non-polar group and additive organic polymer generation chemical reaction or physics twine, thereby base oil and additive are combined securely.
Specific embodiments:
Embodiment 1
A kind of manufacture method of nanometer silicon nitride polishing composition, it comprises the steps:
(1) 1Kg α-Dan Huagui and 10Kg deionized water are put into ball mill, ball milling under the slow speed of revolution; Add 120g surface-modifying agent polyoxyethylene then, again ball milling; Will the nano-silicon nitride slurry behind ball milling emit and dewater, the pulverizer high speed pulverization be used in the nano-silicon nitride lyophilize after will dewatering again at last, promptly gets surperficial modified Nano silicon nitride powder;
(2) with adding the 100g titanate coupling agent in the 19.9Kg base oil, allow it fully dissolve;
To add additive in the 19.8Kg base oil, wherein add the 100g pentaerythritol stearate, add 100g glycerine list n-Hexadecane acid esters;
(3) two kinds of solution with step (2) mix, and the nano silicon nitride silicon powder with step (1) preparation 1Kg surface modification mixes with it then, is placed on the ultra-sonic dispersion machine again and is dispersed into slurry.
(4) slurry of step (3) gained is poured in the container that fills the 59Kg base oil while stirring, stirred, promptly get the nano silicon nitride silicon composition.
The base oil of present embodiment is the mineral oil of C4 alkane.
Embodiment 2-5
Embodiment 2-6 prepares nanometer silicon nitride polishing composition by step of manufacturing of the present invention, wherein component among each embodiment and content and parameter such as following table:
| Embodiment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | ||
| Nano-silicon nitride | Weight (Kg) | 8 | 6 | 4 | 2 | |
| Particle diameter (nm) | 40 | 33 | 26 | 20 | ||
| Deionized water (Kg) | 80 | 66 | 50 | 30 | ||
| (Kg) polyoxyethylene | 0.96 | 0.78 | 0.56 | 0.30 | ||
| Nanometer silicon nitride polishing composition | The nano-silicon nitride of surface modification (Kg) | 8 | 6 | 4 | 2 | |
| Titanate coupling agent (Kg) | 1 | 0.7 | 0.5 | 0.3 | ||
| Pentaerythritol stearate (Kg) | 2 | 1.5 | 0.8 | 0.2 | ||
| Glycerine list n-Hexadecane acid esters (Kg) | 1 | 0.8 | 0.4 | 0.1 | ||
| Base oil | Weight (Kg) | 88 | 91 | 94.3 | 97.4 | |
| Mineral oil | C8 alkane | C7 alkane | C6 alkane | C5 alkane | ||
| Surface roughness Ra (nm) | 5.0 | 4.2 | 3.2 | 1.6 | ||
Annotate: the measuring method that goes up surface roughness Ra in the table: nano-silicon nitride is thrown composition be sprayed on equably on the happiness Pepsi HY series correct grinding type tin mill that U.S. ENGIS Corp. produces, treat the silicon nitride powder post precipitation, its sedimentary silicon nitride is pressed in the tin mill, be placed on then on the happiness Pepsi 36LMH polisher lapper, put into the magnetic head bar again and carry out the magnetic head polishing.Then polished magnetic head is placed under the HITACH1/S-5200 superelevation resolution scanning electronic microscope that HIT produces and tests.
Claims (5)
1. nanometer silicon nitride polishing composition is characterized in that: its component and weight percent content be,
The nano-silicon nitride 1%～8% of surface modification
Titanate coupling agent 0.1%～1.0%
Pentaerythritol stearate 0.1%～2%
Glycerine list n-Hexadecane acid esters 0.1%～1%
Base oil 88%～98.7%.
2. nanometer silicon nitride polishing composition according to claim 1 is characterized in that: the nano-silicon nitride of described surface modification is the nano-silicon nitride through the polyoxyethylene surface modification.
3, nanometer silicon nitride polishing composition according to claim 1 and 2 is characterized in that: the particle diameter of described nano-silicon nitride is 20～40nm.
4, nanometer silicon nitride polishing composition according to claim 1 is characterized in that: described base oil is the mineral oil of C4-C8 alkane.
5, the preparation method of any one described nanometer silicon nitride polishing composition of claim 1-4, it is characterized in that: it comprises the steps:
(1) be 1 by weight: the nano-silicon nitride of 10-15 and deionized water are put into the ball mill ball milling; Be that 1: 0.12～0.15 weight ratio adds polyoxyethylene, ball milling again by nano-silicon nitride and polyoxyethylene then; Will the nano-silicon nitride slurry behind ball milling emit and dewater, the nano-silicon nitride drying after will dewatering be again used the pulverizer high speed pulverization at last, promptly gets the nano-silicon nitride of surface modification;
(2) with total polishing composition weight percent meter, the base oil with 88%～98.7% is divided into three parts;
In first part's base oil, with total polishing composition weight percent meter, add 0.1～1.0% titanate coupling agent, allow it fully dissolve;
In the second section base oil, add additive,, wherein add 0.1%～2% pentaerythritol stearate, add 0.1%～1% glycerine list n-Hexadecane acid esters with total polishing composition weight percent meter;
(3) two kinds of solution with step (2) mix, and then, with total polishing composition weight percent meter, the nano silicon nitride silicon powder of the surface modification of adding 1%～8% is placed on the ultra-sonic dispersion machine again and is dispersed into slurry;
(4) third part base oil in the slurry of step (3) gained is mixed with mixed solution in container, stirs, promptly get nanometer silicon nitride polishing composition.
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| CNB2006100331279A CN100357381C (en) | 2006-01-24 | 2006-01-24 | Nanometer silicon nitride polishing composition and production thereof |
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| CNB2006100331279A CN100357381C (en) | 2006-01-24 | 2006-01-24 | Nanometer silicon nitride polishing composition and production thereof |
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| CN1817997A true CN1817997A (en) | 2006-08-16 |
| CN100357381C CN100357381C (en) | 2007-12-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250589A (en) * | 2011-05-18 | 2011-11-23 | 杨福河 | High performance silica-free heat conductive paste, and preparation method thereof |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3909217A (en) * | 1971-11-26 | 1975-09-30 | Winfield Brooks Company Inc | Abrasive composition containing a gel and a boron-dialkyl silicon-oxygen polymer |
| SU642357A1 (en) * | 1977-02-16 | 1979-01-15 | Институт Химии Высокомолекулярных Соединений Ан Украинской Сср | Composition for running-in |
| JPS60252698A (en) * | 1984-05-29 | 1985-12-13 | Ishikawajima Constr Material Co Ltd | Ceramic cutting and grinding oil |
| JPH0662919B2 (en) * | 1985-03-22 | 1994-08-17 | 昭和電工株式会社 | Polish |
| JP2513492B2 (en) * | 1987-09-17 | 1996-07-03 | 株式会社ジャパンエナジー | Crystal cutting fluid composition |
| US6121143A (en) * | 1997-09-19 | 2000-09-19 | 3M Innovative Properties Company | Abrasive articles comprising a fluorochemical agent for wafer surface modification |
| CN1384166A (en) * | 2002-05-16 | 2002-12-11 | 深圳市纳科实业有限公司 | Polishing composition for polishing surface of memory, hard disk and magnetic head and its polihsing method |
| JP2005246548A (en) * | 2004-03-04 | 2005-09-15 | Bando Chem Ind Ltd | Magnetic polishing fluid |
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- 2006-01-24 CN CNB2006100331279A patent/CN100357381C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250589A (en) * | 2011-05-18 | 2011-11-23 | 杨福河 | High performance silica-free heat conductive paste, and preparation method thereof |
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| CN100357381C (en) | 2007-12-26 |
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Granted publication date: 20071226 Termination date: 20110124 |