CN105131842A - Shape dressing method for nanodiamond aggregate in polishing solution - Google Patents
Shape dressing method for nanodiamond aggregate in polishing solution Download PDFInfo
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- CN105131842A CN105131842A CN201510655728.2A CN201510655728A CN105131842A CN 105131842 A CN105131842 A CN 105131842A CN 201510655728 A CN201510655728 A CN 201510655728A CN 105131842 A CN105131842 A CN 105131842A
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Abstract
The invention discloses a shape dressing method for a nanodiamond aggregate in a polishing solution, and belongs to the technical field of super-precision polishing. The method includes the following steps that the nanodiamond polishing solution, diamond micro-powder and ceramic balls are collected to be mixed, and the mass ratio of nanodiamonds to the diamond micro-powder to the ceramic balls is 1:2-5:0.1-0.5 in the polishing solution; then a grinding buffer agent is added for ball milling. In the ball milling process, the ceramic balls mainly give acting force to the diamond micro-powder, the diamond micro-powder and the nanodiamond aggregate are collided and squeezed, small-amplitude grinding is conducted on the surface of the aggregate, protruding parts (the aggregation shape is irregular due to different aggregation modes) on the aggregate are removed, the shape is made to be closer to a sphere, and thus the shape dressing purpose is achieved. A micron-grade diamond aggregate is separated from the nanoscale diamond aggregate in centrifuging and filtering modes after dressing, and the nanodiamond polishing solution capable of being directly used for polishing sapphire wafers is obtained.
Description
Technical field
The present invention relates to a kind of nano-size abrasive materials pattern method for trimming, be specifically related to Nano diamond coacervate pattern method for trimming in polishing fluid, belong to Ultraprecise polished technical field.
Background technology
Nano diamond has superhard, ultra-fine characteristic, and in Ultraprecise polished field, (as sapphire wafer, silicon carbide wafer, hard disc of computer, computer magnetic head etc.) have widespread use.The initial mean particle size of general commercially available Nano diamond, between 2 ~ 10nm, has huge surface energy, and Nano diamond particle is often existed with aggregating state, and agglomerate size reaches micron even tens micron levels.In order to play the premium properties of Nano diamond in Ultraprecise polished, people have done large quantity research to diamond particles solution agglomeration techniques, also obtain the nano diamond polishing liquid of different aggregated particle size, achieve the controlled processing of average grit diameter to a certain extent.As the people such as Zhu (YongweiZhu, XiangyangXu, BaichunWang, etal.Surfacemodificationanddispersionofnanodiamondinclea noil.ChinaParticuology, 2004,2 (3): 132-134.) adopt hyper-dispersant to carry out chemical modification to Nano diamond surface, make diamond particle surfaces functional group become hydrophobic group from hydrophilic group, thus obtain the nanodiamond suspension of particle diameter 53.2nm in oily medium.Perhaps on the sunny side (to be permitted on the sunny side. the solution of Nano diamond is reunited and stable dispersion research. Hunan: Central South University Ph.D. Dissertation, 2007.) purification impurity elimination is carried out by adding dispersion agent in ball milling abrasive system, obtain the dispersion system of size-grade distribution at below 100nm, in this system, the median size of abrasive grain of 83.5% is 25.7nm.
In grinding and polishing process, except abrasive size has an impact to grinding and polishing quality, abrasive material particle shape also can produce considerable influence to grinding polishing effect.For micron order diamond micro mist, the patent of invention of notification number CN101157200B discloses a kind of by regulating steel ball matching in reshaping ball grinder to realize method that is efficient to diadust, rapid shaping, to reduce shaping number of times, shorten the shaping cycle, enhance productivity.The patent of invention of notification number CN102250582B also discloses a kind of preparation method of narrow ditribution submicron-scale polycrystalline diamond abrasive, comprising: 1) the polycrystalline diamond micro mist of granularity 0.5 ~ 10 μm, grinding aid (thanomin, ethylene glycol etc.) and/or dispersion agent (sodium hydroxide, potassium hydroxide etc.) and pure water are made into slurry (material-water ratio 1:2 ~ 8); 2) slurry is mixed with steel ball (0.2 ~ 16mm) (steel ball consumption is 0.3 ~ 12 times of polycrystalline diamond micro mist), agitation grinding shaping (mixing speed 100 ~ 1500rpm); 3) pickling purify after ultrasonic disperse in pure water, centrifugal classification and get final product, the diamond particles narrow particle size distribution obtained by the method, shape are regular, can be used for the precise polished of sapphire, optical crystal etc.
In nano diamond polishing liquid, abrasive material is the Nano diamond coacervate of single particle, due to aggregation procedure disordering, the coacervate pole of figure is irregular, easily work piece being had a negative impact in polishing processing, as brought small cut, reducing the surface quality etc. of workpiece to be machined.Want to overcome because of the irregular defect causing quality of finish to decline of Nano diamond coacervate pattern, just need to control Nano diamond coacervate pattern.But in nano diamond polishing liquid, agglomerate particle size is everlasting between tens nanometers to hundreds of nanometer, and particle is superfine, and pattern difficulty of processing is large.Also rarely have at present and pattern processing, the research of finishing and report are carried out to Nano diamond coacervate in polishing fluid.
Summary of the invention
The object of this invention is to provide Nano diamond coacervate pattern method for trimming in a kind of polishing fluid.
In order to realize above object, the technical solution adopted in the present invention is:
Nano diamond coacervate pattern method for trimming in polishing fluid, comprise the following steps: get the mixing of nano diamond polishing liquid, diadust and Ceramic Balls, in polishing fluid, the mass ratio of Nano diamond and diadust, Ceramic Balls is 1:2 ~ 5:0.1 ~ 0.5, add grinding buffer reagent, ball milling.
In described polishing fluid, the mass percent of Nano diamond is 0.2% ~ 2%, median size 30 ~ 300nm.
Described diadust can adopt in granularity M5/10, M6/12, M8/16, M10/20, M15/25 etc. one or more.Diadust has superhard, ultra-fine characteristic, can collide with Nano diamond coacervate in polishing fluid under certain External Force Acting, directly touch coacervate surface, through multiple impacts friction, the irregular profile of Nano diamond coacervate is polished rounding, and pattern is subglobular gradually.
Described Ceramic Balls can adopt in zirconium oxide bead, oxidation silica bead, nitrogenize silica bead, alumina bead etc. one or more.The particle diameter of Ceramic Balls is 0.5 ~ 5mm.The object adding Ceramic Balls gives diadust reactive force, makes Nano diamond coacervate in diadust and polishing fluid collide, extrude.
Described grinding buffer reagent adopt in turbine oil, transformer oil, glycerine, oleic acid, white oil, Macrogol 200, Polyethylene Glycol-600 etc. one or more, in intergrinding process, play buffering grinding, avoid over-mastication.The dosage of grinding buffer reagent is 2% ~ 8% of nano diamond polishing liquid, diadust and Ceramic Balls three total mass.
Described ball milling can adopt U.S. SPEX8000D model high energy ball mill, ball milling 10 ~ 100min.
Described ball milling is complete takes out Ceramic Balls (as adopted the strainer filtering of aperture 0.4mm) from ball-milled mixtures, and remainder centrifuging and taking upper liquid, filters, and filtrate is the nano diamond polishing liquid after particle shape finishing.
Described centrifugal be centrifugal 5 ~ 10min under rotating speed 5000 ~ 10000r/min.
The aperture of filter screen that described filtration (after centrifugal) adopts is 0.3 ~ 1 μm.
Beneficial effect of the present invention:
The present invention adopts and the mode of diadust (5 ~ 25 μm), Ceramic Balls and nano diamond polishing liquid mix grinding is carried out pattern finishing to Nano diamond coacervate in polishing fluid, by mode that is centrifugal, that filter, micron order diamond is separated with nano-diamond coacervate after finishing, the pattern subglobular of Nano diamond coacervate in gained polishing fluid, surfaceness reduces greatly compared with before finishing, can be directly used in the polishing of sapphire wafer.
In intergrinding process, Ceramic Balls mainly gives diadust reactive force, diadust and Nano diamond coacervate is made to collide, extrude, coacervate surface is ground by a small margin, and the protuberance (because reunion mode difference causes reunion pattern irregularity) on coacervate is removed, make its pattern more mellow and fuller, thus reach pattern dressing purpose.
Accompanying drawing explanation
Fig. 1 is the SEM figure of Nano diamond coacervate before pattern finishing in the embodiment of the present invention 6;
Fig. 2 is the SEM figure of Nano diamond coacervate after pattern finishing in embodiment 6.
Embodiment
Following embodiment is only described in further detail the present invention, but does not form any limitation of the invention.
Embodiment 1
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, zirconium oxide bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M5/10 and M6/12 (mass ratio 1:1), the particle diameter of zirconium oxide bead is 0.5mm, in polishing fluid, the mass percent of Nano diamond is 1%, median size 30nm, in polishing fluid, the mass ratio of Nano diamond and diadust, zirconium oxide bead is 1:2:0.1, add Macrogol 200 in the mixture, dosage is 2% of mixture total mass, adopts U.S. SPEX8000D model high energy ball mill ball milling 5min;
2) ball milling is complete, zirconium oxide bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 5min under rotating speed 10000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 300nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 2
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, oxidation silica bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M5/10, the particle diameter of oxidation silica bead is 0.6mm, in polishing fluid, the mass percent of Nano diamond is 0.2%, median size 50nm, Nano diamond and diadust in polishing fluid, the mass ratio being oxidized silica bead are 1:2:0.3, add Polyethylene Glycol-600 in the mixture, dosage is 4% of mixture total mass, ball milling 10min (high energy ball mill is with embodiment 1);
2) ball milling is complete, oxidation silica bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 10min under rotating speed 8000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 300nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 3
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, nitrogenize silica bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M6/12, the particle diameter of nitrogenize silica bead is 0.8mm, in polishing fluid, the mass percent of Nano diamond is 2%, median size 60nm, in polishing fluid, the mass ratio of Nano diamond and diadust, nitrogenize silica bead is 1:5:0.5, add turbine oil and glycerine (mass ratio 1:1) in the mixture, dosage is 8% of mixture total mass, ball milling 30min (high energy ball mill is with embodiment 1);
2) ball milling is complete, nitrogenize silica bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 8min under rotating speed 8000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 300nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 4
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, nitrogenize silica bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M6/12, the particle diameter of nitrogenize silica bead is 0.8mm, in polishing fluid, the mass percent of Nano diamond is 2%, median size 60nm, in polishing fluid, the mass ratio of Nano diamond and diadust, nitrogenize silica bead is 1:5:0.5, adds transformer oil in the mixture, dosage is 4% of mixture total mass, ball milling 30min (high energy ball mill is with embodiment 1);
2) ball milling is complete, nitrogenize silica bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 10min under rotating speed 8000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 300nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 5
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, alumina bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M6/12 and M8/16 (mass ratio 1:1), the particle diameter of alumina bead is 0.8mm, in polishing fluid, the mass percent of Nano diamond is 1%, median size 80nm, in polishing fluid, the mass ratio of Nano diamond and diadust, alumina bead is 1:3:0.2, add transformer oil in the mixture, dosage is 6% of mixture total mass, ball milling 30min (high energy ball mill is with embodiment 1);
2) ball milling is complete, alumina bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 7min under rotating speed 9000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 400nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 6
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, alumina bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M8/16, the particle diameter of alumina bead is 1mm, in polishing fluid, the mass percent of Nano diamond is 0.2%, median size 100nm (see Fig. 1), in polishing fluid, the mass ratio of Nano diamond and diadust, alumina bead is 1:2:0.1, add white oil and oleic acid (mass ratio 1:1) in the mixture, dosage is 8% of mixture total mass, ball milling 15min (high energy ball mill is with embodiment 1);
2) ball milling is complete, alumina bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 5min under rotating speed 7000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 400nm, filtrate is the nano diamond polishing liquid (see Fig. 2) after particle shape finishing.
Embodiment 7
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, zirconium oxide bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M8/16, the particle diameter of zirconium oxide bead is 2mm, in polishing fluid, the mass percent of Nano diamond is 2%, median size 120nm, in polishing fluid, the mass ratio of Nano diamond and diadust, zirconium oxide bead is 1:3:0.3, adds white oil in the mixture, dosage is 2% of mixture total mass, ball milling 20min (high energy ball mill is with embodiment 1);
2) ball milling is complete, zirconium oxide bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 6min under rotating speed 6000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 500nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 8
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, zirconium oxide bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M10/20, the particle diameter of zirconium oxide bead is 3mm, in polishing fluid, the mass percent of Nano diamond is 2%, median size 150nm, in polishing fluid, the mass ratio of Nano diamond and diadust, zirconium oxide bead is 1:2:0.1, adds white oil in the mixture, dosage is 4% of mixture total mass, ball milling 15min (high energy ball mill is with embodiment 1);
2) ball milling is complete, zirconium oxide bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 9min under rotating speed 6000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 600nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 9
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, nitrogenize silica bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M15/25, the particle diameter of nitrogenize silica bead is 4mm, in polishing fluid, the mass percent of Nano diamond is 0.8%, median size 200nm, in polishing fluid, the mass ratio of Nano diamond and diadust, nitrogenize silica bead is 1:3:0.2, adds turbine oil in the mixture, dosage is 3% of mixture total mass, ball milling 30min (high energy ball mill is with embodiment 1);
2) ball milling is complete, nitrogenize silica bead (aperture 0.4mm strainer filtering) is taken out from ball-milled mixtures, remainder is placed in whizzer, centrifugal 10min under rotating speed 5000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 800nm, filtrate is the nano diamond polishing liquid after particle shape finishing.
Embodiment 10
Nano diamond coacervate pattern method for trimming in polishing fluid, step is as follows:
1) diadust, nitrogenize silica bead are added in nano diamond polishing liquid and mix, the granularity of diadust is M15/25, the particle diameter of nitrogenize silica bead is 5mm, in polishing fluid, the mass percent of Nano diamond is 2%, median size 300nm, in polishing fluid, the mass ratio of Nano diamond and diadust, nitrogenize silica bead is 1:2:0.1, adds turbine oil in the mixture, dosage is 4% of mixture total mass, ball milling 10min (high energy ball mill is with embodiment 1);
2) ball milling is complete, and from ball-milled mixtures, take out nitrogenize silica bead, remainder is placed in whizzer, centrifugal 5min under rotating speed 5000r/min, centrifugal end is got upper liquid and is filtered, aperture of filter screen 1000nm, and filtrate is the nano diamond polishing liquid after particle shape finishing.
Claims (9)
1. Nano diamond coacervate pattern method for trimming in polishing fluid, it is characterized in that: comprise the following steps: get the mixing of nano diamond polishing liquid, diadust and Ceramic Balls, in polishing fluid, the mass ratio of Nano diamond and diadust, Ceramic Balls is 1:2 ~ 5:0.1 ~ 0.5, add grinding buffer reagent, ball milling.
2. pattern method for trimming according to claim 1, is characterized in that: in described polishing fluid, the mass percent of Nano diamond is 0.2% ~ 2%, median size 30 ~ 300nm.
3. pattern method for trimming according to claim 1, is characterized in that: described diadust adopt in granularity M5/10, M6/12, M8/16, M10/20, M15/25 one or more.
4. pattern method for trimming according to claim 1, is characterized in that: described Ceramic Balls adopt in zirconium oxide bead, oxidation silica bead, nitrogenize silica bead, alumina bead one or more, particle diameter 0.5 ~ 5mm.
5. pattern method for trimming according to claim 1, it is characterized in that: described grinding buffer reagent adopt in turbine oil, transformer oil, glycerine, oleic acid, white oil, Macrogol 200, Polyethylene Glycol-600 one or more, the dosage of grinding buffer reagent is 2% ~ 8% of nano diamond polishing liquid, diadust and Ceramic Balls three total mass.
6. pattern method for trimming according to claim 1, is characterized in that: described Ball-milling Time is 10 ~ 100min.
7. pattern method for trimming according to claim 1, is characterized in that: described ball milling is complete takes out Ceramic Balls from ball-milled mixtures, remainder centrifuging and taking upper liquid, filters, obtains filtrate.
8. pattern method for trimming according to claim 7, is characterized in that: described centrifugal under rotating speed 5000 ~ 10000r/min centrifugal 5 ~ 10min.
9. pattern method for trimming according to claim 7, is characterized in that: the described aperture of filter screen filtering employing is 0.3 ~ 1 μm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110936284A (en) * | 2018-09-21 | 2020-03-31 | 邵丙璜 | Grinding method of semiconductor wafer |
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| CN1962964A (en) * | 2006-11-08 | 2007-05-16 | 北京国瑞升科技有限公司 | Nano monocrystalline diamond and method for making same |
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| CN202343280U (en) * | 2011-12-08 | 2012-07-25 | 河南省惠丰金刚石有限公司 | Inner circulating type diamond micro mist reshaping device |
| CN104395234A (en) * | 2012-04-27 | 2015-03-04 | 泰恩河畔纽卡斯尔大学 | Method for separation of diamond particle clusters |
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- 2015-10-13 CN CN201510655728.2A patent/CN105131842B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1827301A (en) * | 2006-04-07 | 2006-09-06 | 清华大学 | Particle shaping method and device thereof |
| CN1962964A (en) * | 2006-11-08 | 2007-05-16 | 北京国瑞升科技有限公司 | Nano monocrystalline diamond and method for making same |
| CN101045829A (en) * | 2007-03-08 | 2007-10-03 | 武汉理工大学 | Diamond powder modification method and equipment |
| CN202343280U (en) * | 2011-12-08 | 2012-07-25 | 河南省惠丰金刚石有限公司 | Inner circulating type diamond micro mist reshaping device |
| CN104395234A (en) * | 2012-04-27 | 2015-03-04 | 泰恩河畔纽卡斯尔大学 | Method for separation of diamond particle clusters |
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| CN110936284A (en) * | 2018-09-21 | 2020-03-31 | 邵丙璜 | Grinding method of semiconductor wafer |
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