CN105131842B - Nano diamond aggregate pattern dressing method in polishing fluid - Google Patents
Nano diamond aggregate pattern dressing method in polishing fluid Download PDFInfo
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- CN105131842B CN105131842B CN201510655728.2A CN201510655728A CN105131842B CN 105131842 B CN105131842 B CN 105131842B CN 201510655728 A CN201510655728 A CN 201510655728A CN 105131842 B CN105131842 B CN 105131842B
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Abstract
The invention discloses Nano diamond aggregate pattern dressing method in a kind of polishing fluid, belong to Ultraprecise polished technical field.This method comprises the following steps：Nano diamond polishing liquid, diadust and Ceramic Balls are taken to mix, the mass ratio of Nano diamond and diadust, Ceramic Balls is 1 in polishing fluid:2~5:0.1~0.5, add grinding buffer, ball milling, you can.Ceramic Balls mainly assign diadust active force in mechanical milling process, diadust is set to collide, extrude with Nano diamond aggregate, aggregate surface is ground by a small margin, and the ledge (reunion pattern is irregular caused by reunion mode difference) on aggregate is removed, make its pattern closer to spherical, so as to reach pattern dressing purpose.Micron order diamond is separated with nano-diamond aggregate by way of centrifuging, filtering again after finishing, obtains can be directly used for the nano diamond polishing liquid of sapphire wafer polishing.
Description
Technical field
The present invention relates to a kind of nano-size abrasive materials pattern dressing method, and in particular to Nano diamond aggregate in polishing fluid
Pattern dressing method, belong to Ultraprecise polished technical field.
Background technology
Nano diamond has superhard, ultra-fine characteristic, in Ultraprecise polished field (such as sapphire wafer, silicon carbide whisker
Piece, hard disc of computer, computer magnetic head etc.) there is extensive use.The initial mean particle size of general commercially available Nano diamond 2~
Between 10nm, there is huge surface energy so that Nano diamond particle often exists with aggregating state, and agglomerate size reaches micro-
Rice even tens micron levels.In order to play premium properties of the Nano diamond in Ultraprecise polished, people are to diamond
Grain de-agglomerated technology has done numerous studies, also obtain the nano diamond polishing liquid of different aggregated particle sizes, to a certain extent
Realize the controllable processing of average grit diameter.As Zhu et al. (Yongwei Zhu, Xiangyang Xu, Baichun Wang,
etal.Surface modification and dispersion of nanodiamond in clean oil.China
Particuology,2004,2(3):Chemical modification 132-134.) is carried out to Nano diamond surface using hyper-dispersant, makes gold
Hard rock particle surface functional group is changed into hydrophobic group from hydrophilic group, so as to obtain particle diameter 53.2nm Nano diamond in oil medium
Suspension.Perhaps face south (de-agglomerated for the Nano diamonds that face south perhaps and stable dispersion research Hunan:Central South University's doctorate opinion
Text, 2007.) purification impurity elimination is carried out by adding dispersant in ball milling abrasive system, obtains size distribution in below 100nm
Dispersion, the average grain diameter of 83.5% abrasive grain is 25.7nm in the system.
During grinding and polishing, in addition to abrasive size has an impact to grinding and polishing quality, abrasive material particle shape also can be to grinding
Grinding and polishing light effect produces considerable influence.For micron order diamond micro mist, notification number CN101157200B patent of invention discloses
It is a kind of to realize efficient to diadust, rapid shaping method by adjusting steel ball matching in reshaping ball grinder, to reduce
Shaping number, shorten the shaping cycle, improve production efficiency.Notification number CN102250582B patent of invention also discloses that a kind of narrow
The preparation method of submicron-scale polycrystalline diamond abrasive is distributed, including：1) it is the polycrystalline diamond of 0.5~10 μm of granularity is micro-
Powder, grinding aid (monoethanolamine, ethylene glycol etc.) and/or dispersant (sodium hydroxide, potassium hydroxide etc.) are made into slurry (material water with pure water
Than 1:2~8)；2) slurry is mixed to (steel ball dosage is 0.3~12 times of polycrystalline diamond micro mist) with steel ball (0.2~16mm),
Agitation grinding shaping (100~1500rpm of speed of agitator)；3) in pure water, centrifugal classification produces ultrasonic disperse after pickling purification,
Regular by the diamond particles narrow particle size distribution of this method acquisition, shape, the precision available for sapphire, optical crystal etc. is thrown
Light.
In nano diamond polishing liquid, abrasive material is the Nano diamond aggregate of individual particle, because aggregation procedure is unordered
Change, aggregate shape irregular, easily have a negative impact in polishing processing to work piece, such as bring small draw
Trace, reduce surface quality of workpiece to be machined etc..Want to overcome because Nano diamond aggregate pattern irregularly caused by polish matter
The defects of amount declines, it is necessary to be controlled to Nano diamond aggregate pattern.But in nano diamond polishing liquid, group
For aggressiveness granularity often between tens nanometers to hundreds of nanometers, particle is superfine, and pattern difficulty of processing is big.Also rarely have to polishing fluid at present
Middle Nano diamond aggregate carries out pattern processing, the research of finishing and report.
The content of the invention
It is an object of the invention to provide Nano diamond aggregate pattern dressing method in a kind of polishing fluid.
In order to realize the above object the technical solution adopted in the present invention is：
Nano diamond aggregate pattern dressing method, comprises the following steps in polishing fluid：Take nano diamond polishing liquid,
Diadust and Ceramic Balls mix, and the mass ratio of Nano diamond and diadust, Ceramic Balls is 1 in polishing fluid:2~5:
0.1~0.5, add grinding buffer, ball milling, you can.
The mass percent of Nano diamond is 0.2%~2% in the polishing fluid, 30~300nm of average grain diameter.
The diadust can use one kind or more in granularity M5/10, M6/12, M8/16, M10/20, M15/25 etc.
Kind.Diadust has superhard, ultra-fine characteristic, can be with Nano diamond aggregate in polishing fluid under the effect of certain external force
Collide, directly touch aggregate surface, through multiple impacts friction, the irregular contour of Nano diamond aggregate is smoothed
Rounding, pattern subglobular gradually.
The Ceramic Balls can use the one or more in zirconium oxide bead, oxidation silica bead, nitridation silica bead, alumina bead etc..
The particle diameter of Ceramic Balls is 0.5~5mm.Add Ceramic Balls purpose be to confer to diadust active force, make diadust with
Nano diamond aggregate is collided, extruded in polishing fluid.
The grinding buffer is using turbine oil, transformer oil, glycerine, oleic acid, white oil, polyethylene glycol 200, polyethylene glycol
One or more in 600 grades, buffering abrasive action is played in intergrinding process, avoids overmastication.Grind the dosage of buffer
For the 2%~8% of nano diamond polishing liquid, diadust and Ceramic Balls three's gross mass.
The ball milling can use U.S.'s SPEX 8000D model high energy ball mills, 10~100min of ball milling.
The ball milling finishes and Ceramic Balls (strainer filtering as used aperture 0.4mm) is taken out from ball-milled mixtures, remaining
Part centrifugal takes upper liquid, filtering, and filtrate is the nano diamond polishing liquid after particle shape finishing.
The centrifugation is that 5~10min is centrifuged under 5000~10000r/min of rotating speed.
The aperture of filter screen used (after centrifugation) that filters is 0.3~1 μm.
Beneficial effects of the present invention：
The present invention is by the way of by diadust (5~25 μm), Ceramic Balls and nano diamond polishing liquid mix grinding pair
Nano diamond aggregate carries out pattern finishing in polishing fluid, by micron order diamond by way of centrifuging, filtering after finishing
Separated with nano-diamond aggregate, the pattern subglobular of Nano diamond aggregate in gained polishing fluid, before finishing
Substantially reduced compared to surface roughness, can be directly used for the polishing of sapphire wafer.
In intergrinding process, Ceramic Balls mainly assign diadust active force, make diadust and Nano diamond
Aggregate is collided, extruded, and aggregate surface is ground by a small margin, and by the ledge on aggregate (because reuniting
Mode difference causes the reunion pattern irregular) remove, make its pattern more mellow and fuller, so as to reach pattern dressing purpose.
Brief description of the drawings
Fig. 1 is the SEM figures of Nano diamond aggregate before pattern finishing in the embodiment of the present invention 6；
Fig. 2 is the SEM figures of Nano diamond aggregate after pattern finishing in embodiment 6.
Embodiment
Following embodiments are only described in further detail to the present invention, but do not form any limitation of the invention.
Embodiment 1
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, zirconium oxide bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M5/10 and M6/12 (mass ratioes 1:1), the particle diameter of zirconium oxide bead is 0.5mm, the mass percent of Nano diamond in polishing fluid
For 1%, average grain diameter 30nm, the mass ratio of Nano diamond and diadust, zirconium oxide bead is 1 in polishing fluid:2:0.1,
Polyethylene glycol 200 is added in the mixture, and dosage is the 2% of mixture gross mass, using U.S.'s SPEX 8000D model high energy
Ball mill ball milling 5min；
2) ball milling finishes, and zirconium oxide bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 5min is centrifuged under rotating speed 10000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 300nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 2
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, oxidation silica bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M5/10, the particle diameter for aoxidizing silica bead are 0.6mm, and the mass percent of Nano diamond is 0.2% in polishing fluid, average grain diameter
50nm, Nano diamond and diadust in polishing fluid, the mass ratio for aoxidizing silica bead are 1:2:0.3, add in the mixture
Macrogol 600, dosage are the 4% of mixture gross mass, ball milling 10min (high energy ball mill is with embodiment 1)；
2) ball milling finishes, and oxidation silica bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 10min is centrifuged under rotating speed 8000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 300nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 3
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, nitridation silica bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M6/12, the particle diameter for nitrogenizing silica bead are 0.8mm, and the mass percent of Nano diamond is 2%, average grain diameter 60nm in polishing fluid,
The mass ratio of Nano diamond and diadust, nitridation silica bead is 1 in polishing fluid:5:0.5, turbine oil is added in the mixture
With glycerine (mass ratio 1:1), dosage is the 8% of mixture gross mass, ball milling 30min (high energy ball mill is with embodiment 1)；
2) ball milling finishes, and nitridation silica bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 8min is centrifuged under rotating speed 8000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 300nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 4
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, nitridation silica bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M6/12, the particle diameter for nitrogenizing silica bead are 0.8mm, and the mass percent of Nano diamond is 2%, average grain diameter 60nm in polishing fluid,
The mass ratio of Nano diamond and diadust, nitridation silica bead is 1 in polishing fluid:5:0.5, transformer is added in the mixture
Oil, dosage are the 4% of mixture gross mass, ball milling 30min (high energy ball mill is with embodiment 1)；
2) ball milling finishes, and nitridation silica bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 10min is centrifuged under rotating speed 8000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 300nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 5
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, alumina bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M6/12 and M8/16 (mass ratioes 1:1), the particle diameter of alumina bead is 0.8mm, the mass percent of Nano diamond in polishing fluid
For 1%, average grain diameter 80nm, the mass ratio of Nano diamond and diadust, alumina bead is 1 in polishing fluid:3:0.2,
Transformer oil is added in the mixture, and dosage is the 6% of mixture gross mass, ball milling 30min (the same embodiments of high energy ball mill
1)；
2) ball milling finishes, and alumina bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 7min is centrifuged under rotating speed 9000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 400nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 6
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, alumina bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M8/16, the particle diameter of alumina bead are 1mm, and the mass percent of Nano diamond is 0.2% in polishing fluid, average grain diameter 100nm
(see Fig. 1), the mass ratio of Nano diamond and diadust, alumina bead is 1 in polishing fluid:2:0.1, add in the mixture
Enter white oil and oleic acid (mass ratio 1:1), dosage is the 8% of mixture gross mass, ball milling 15min (the same embodiments of high energy ball mill
1)；
2) ball milling finishes, and alumina bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 5min is centrifuged under rotating speed 7000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 400nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape (see Fig. 2).
Embodiment 7
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, zirconium oxide bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M8/16, the particle diameter of zirconium oxide bead are 2mm, and the mass percent of Nano diamond is 2%, average grain diameter 120nm in polishing fluid,
The mass ratio of Nano diamond and diadust, zirconium oxide bead is 1 in polishing fluid:3:0.3, white oil is added in the mixture,
Dosage is the 2% of mixture gross mass, ball milling 20min (high energy ball mill is with embodiment 1)；
2) ball milling finishes, and zirconium oxide bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 6min is centrifuged under rotating speed 6000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 500nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 8
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, zirconium oxide bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M10/20, the particle diameter of zirconium oxide bead are 3mm, and the mass percent of Nano diamond is 2%, average grain diameter 150nm in polishing fluid,
The mass ratio of Nano diamond and diadust, zirconium oxide bead is 1 in polishing fluid:2:0.1, white oil is added in the mixture,
Dosage is the 4% of mixture gross mass, ball milling 15min (high energy ball mill is with embodiment 1)；
2) ball milling finishes, and zirconium oxide bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 9min is centrifuged under rotating speed 6000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 600nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 9
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, nitridation silica bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M15/25, the particle diameter for nitrogenizing silica bead are 4mm, and the mass percent of Nano diamond is 0.8% in polishing fluid, average grain diameter
200nm, Nano diamond and diadust in polishing fluid, the mass ratio for nitrogenizing silica bead are 1:3:0.2, add in the mixture
Turbine oil, dosage are the 3% of mixture gross mass, ball milling 30min (high energy ball mill is with embodiment 1)；
2) ball milling finishes, and nitridation silica bead (aperture 0.4mm strainer filterings) is taken out from ball-milled mixtures, remainder is placed in
In centrifuge, 10min is centrifuged under rotating speed 5000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 800nm, and filtrate is
Nano diamond polishing liquid after being repaired for particle shape.
Embodiment 10
Nano diamond aggregate pattern dressing method, step are as follows in polishing fluid：
1) diadust, nitridation silica bead are added in nano diamond polishing liquid and mixed, the granularity of diadust is
M15/25, the particle diameter for nitrogenizing silica bead are 5mm, and the mass percent of Nano diamond is 2%, average grain diameter 300nm in polishing fluid,
The mass ratio of Nano diamond and diadust, nitridation silica bead is 1 in polishing fluid:2:0.1, turbine is added in the mixture
Oil, dosage are the 4% of mixture gross mass, ball milling 10min (high energy ball mill is with embodiment 1)；
2) ball milling finishes, and nitridation silica bead is taken out from ball-milled mixtures, remainder is placed in a centrifuge, in rotating speed
5min is centrifuged under 5000r/min, centrifugation end takes upper liquid to filter, aperture of filter screen 1000nm, and filtrate is after particle shape is repaired
Nano diamond polishing liquid.
Claims (6)
1. Nano diamond aggregate pattern dressing method in polishing fluid, it is characterised in that：Comprise the following steps：Take a nanometer Buddha's warrior attendant
Stone polishing fluid, diadust and Ceramic Balls mix, Nano diamond and diadust, the mass ratio of Ceramic Balls in polishing fluid
For 1:2-5:0.1-0.5, add grinding buffer, ball milling, you can；
The mass percent of Nano diamond is 0.2%-2%, average grain diameter 30-300nm in the polishing fluid；
The diadust uses the one or more in granularity M5/10, M6/12, M8/16, M10/20, M15/25；
The Ceramic Balls are using the one or more in zirconium oxide bead, oxidation silica bead, nitridation silica bead, alumina bead, particle diameter 0.5-
5mm。
2. pattern dressing method according to claim 1, it is characterised in that：The grinding buffer is using turbine oil, change
One or more in depressor oil, glycerine, oleic acid, white oil, polyethylene glycol 200, Macrogol 600, grind the dosage of buffer
For the 2%-8% of nano diamond polishing liquid, diadust and Ceramic Balls three's gross mass.
3. pattern dressing method according to claim 1, it is characterised in that：The Ball-milling Time is 10-100min.
4. pattern dressing method according to claim 1, it is characterised in that：The ball milling finishes to be taken from ball-milled mixtures
Go out Ceramic Balls, remainder centrifuging and taking upper liquid, filtering, obtain filtrate.
5. pattern dressing method according to claim 4, it is characterised in that：The centrifugation is in rotating speed
5-10min is centrifuged under 5000-10000r/min.
6. pattern dressing method according to claim 4, it is characterised in that：The aperture of filter screen used that filters is 0.3-
1μm。
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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 |
-
2015
- 2015-10-13 CN CN201510655728.2A patent/CN105131842B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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