CN102658529A - Method for preparing nano particles by nano grinding through superfine abrasive particles - Google Patents
Method for preparing nano particles by nano grinding through superfine abrasive particles Download PDFInfo
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- CN102658529A CN102658529A CN2012101410146A CN201210141014A CN102658529A CN 102658529 A CN102658529 A CN 102658529A CN 2012101410146 A CN2012101410146 A CN 2012101410146A CN 201210141014 A CN201210141014 A CN 201210141014A CN 102658529 A CN102658529 A CN 102658529A
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Abstract
The invention provides a method for preparing nano particles by nano grinding through superfine abrasive particles, belongs to the technical field of preparation of the nano particles by carrying out nano grinding on a hard-crisp and softly-crisp semiconductor, and particularly relates to a super-precise processing method of the hard-crisp and softly-crisp semiconductor. The method is characterized in that the hard-crisp and softly-crisp semiconductor with the nano hardness less than or equal to 15 GPa is used as a workpiece and the nano particles are obtained by super-precise process without chemical liquid. The method adopts No.10000-No.300000 superfine diamond abrasive particles as grinding materials and the concentration of diamonds is more than or equal to 200; and a superfine diamond sand wheel is prepared by a ceramic bonding agent. The feeding amount of a main shaft in the nano grinding is 1-100 microns/minute; and de-ionized water is used as grinding liquid to finish the super-precise processing method of ductility region grinding. According to the invention, a purely-mechanical super-precise processing method and a green physical method without chemical reaction and environmental pollution are adopted to prepare the nano particles. The method has the effect and the benefit of realizing the effect of the super-precise process without the chemical liquid of the hard-crisp and softly-crisp semiconductor with the nano hardness less than or equal to 15 GPa so as to obtain the nano particles.
Description
Technical field
The invention belongs to hard crisp and soft crisp semiconductor nano grinding and prepare the nano particle technical field, particularly hard crisp and soft crisp semi-conductive ultraprecise processing method.
Background technology
Nano particle occupies important position in nanosecond science and technology, like fields such as optics, semiconductor, machinery, photoelectrons.And the method for preparing nano particle that adopts at present is mainly chemical synthesis, physics synthetic method etc.These methods relate generally to the use of chemical liquids and physics high temperature, and chemical liquids is often brought appearance danger easily in potential injury and the building-up process to environment and operator.As in the chemical liquids during synthesis of nano particle, normally under higher temperature, several chemical reactions carry out simultaneously, and the difficult control of the speed of this chemical reaction and course of reaction.In case gas in reaction, occurs, it is improper to control, and the possibility of blast is just arranged.And reaction intermediate and product are also generally harmful to operator and environment.For physical method synthesis of nano particle, then often use high temperature, and this high temperature is unallowed for some semiconductors.Like soft crisp semiconductor mercury cadmium telluride; Its boiling temperature is merely 250 °, and melt temperature is merely 150 °, and this solid matter just decomposes near in a single day reaching boiling temperature easily; Thereby produce hypertoxic gas mercury vapour, all will bring great threat operator and environment.And other generally can not bear the high temperature that surpasses 200 degree attached to polymer on semiconductor and the photoelectric crystal and organic matter.Therefore, chemical synthesis and physics synthetic method all have limitation separately, for the present age fast-developing science and technology and the demand of industry to nano particle, can not adapt to gradually.Yet adopt the method for ultraprecise processing and preparing nano particle to rarely have report again, therefore, hindered the preparation method of nano particle under green and normal temperature condition development, and to current science and technology and development of modern industry.
Summary of the invention
The objective of the invention is to adopt the ultra-fine diamond abrasive material, preparation nanometer abrasive particle under the face abrasive machine mode of ductility territory, grinding fluid is a deionized water, realizes the purpose of preparation nano particle.
Technical scheme of the present invention is that the hard crisp and soft crisp semiconductor of employing nano hardness≤15 GPa is a workpiece, and no chemical liquids ultraprecise processing obtains the nano particle method.The ultra-fine diamond abrasive particle that adopts #10000-#300000 is as abrasive material, and adamantine concentration >=200 are prepared into the ultra-fine diamond emery wheel with vitrified bond.The axis feeding amount is 1-100 μ m/min in the nanometer grinding, adopts deionized water as grinding fluid, accomplishes ductility territory face grinding ultraprecise processing method.The present invention adopts pure mechanical ultraprecise processing method, and the green physical method of no chemical reaction and environmental pollution prepares nano particle.Effect of the present invention and benefit are to have realized that the hard crisp and soft crisp semi-conductive no chemical liquids ultraprecise processing of nano hardness≤15 GPa obtains the effect of nano particle.
The nanometer grinding method is the face grinding of ductility territory.Removing material is removed and is mainly contained dual mode, and a kind of is that brittle fracture is removed, and a kind of is that remove in the ductility territory.Brittle fracture is removed and is mainly used in macroscopical grinding or rough, and the removal of ductility territory is mainly used in fine ginding and superfine grinding.The nanometer grinding method that the present invention adopts is a kind of of ultraprecise processing method, therefore will under the grinding condition of ductility territory, carry out, so that obtain nano particle, guarantees the uniformity of nano particle simultaneously.The face method for grinding is different from traditional vertical method for grinding, and traditional vertical method for grinding is open method for grinding at intermittence, and the face method for grinding is the continuous grinding method of sealing.When workpiece when being circular, the edge of face abrasive grinding wheel is through the center of round piece, thereby guarantees that the contact area in grinding process equates that when feed rate was constant, grinding force was constant, thereby avoids the intermittently impact process at intermittence of grinding.During the face grinding, abrasive dust is that nano particle is to be stored in the hole of ultra-fine diamond emery wheel, so abrasive dust is the physics hole that the size of nano particle depends on ultra-fine emery wheel.The physical arrangement of ultra-fine emery wheel is much bigger to the more vertical grinding of the influence of nano particle during the face grinding.Why called after nanometer grinding, be because the hole during ultra-fine abrasive particle face grinding generally in nanometer scale, and the clearance that the emery wheel list changes is usually also in nanometer scale.When being 1 μ m/min like the feed speed of main shaft, rotating speed of table is 200 rpm, and the clearance that changes of workpiece list is 5 nm so.Therefore, be different from traditional method for grinding, be called the nanometer grinding method.
Axis feeding speed is 1-100 μ m/min, and the speed of mainshaft is 1500-10000 rpm, and rotating speed of table is 40-500 rpm.For the diameter range of controlling nano particle below 100 nm, and guarantee that the grinding method of different materials is the grinding of ductility territory, therefore limiting the speed of mainshaft is 1-100 μ m/min.Axis feeding speed has the greatest impact to nano particle and workpiece surface roughness in three kinds of machined parameters, is the speed of mainshaft secondly, is rotating speed of table at last.Too high rigidity and the required precision to lathe of the speed of mainshaft increases, and can improve processing cost, and according to our processing experience, the speed of mainshaft is proper at 1500-10000 rpm.Rotating speed of table is minimum to the influence of nano particle diameter.Therefore adopt suitable low speed, like 40-500 rpm, all of great advantage for the vibration aspect that obtains uniform nano particle and reduction lathe.
Wear particle size is #10000-#300000, and corresponding abrasive material diameter is below 1 μ m.Its diameter of ultra-fine abrasive particle is generally below 1 μ m, so its corresponding wear particle size is usually greater than #10000.Wear particle size also is not suitable for excessive, excessive words vitrified bond and is difficult to the hold that provides enough, and the hole of ultra-fine emery wheel also can become more and more littler, is unfavorable for obtaining high-quality finished surface, the also difficult control of the size of nano particle.On the other hand, when the granularity of diamond abrasive was excessive, adamantine ledge will be very little, possibly be that vitrified bond is carrying out ablation to a certain extent, and abrasive material and vitrified bond all come off easily, and therefore selected wear particle size is #10000-#300000.
Abrasive material is a diamond, volumn concentration >=50%, corresponding diamond concentration >=200.In grinding, grinding force is born by outstanding diamond abrasive, so the quantity of abrasive material is extremely important for the grinding force that reduces single abrasive particle.If the concentration of abrasive particle is lower, the grinding force that so single abrasive particle is born will be bigger, and abrasive particle grinds bald easily, and under bigger grinding force effect, come off easily.For ultra-fine abrasive particle; It is much little that the abrasive particle of the more traditional coarse plain emery wheel of contact area of vitrified bond is wanted, and therefore in order to prevent that ultra-fine abrasive particle from coming off, must reduce the suffered grinding force of single abrasive particle; So adamantine concentration >=200, corresponding volumn concentration is generally >=50%.
Bond is the 2-4 kind in carborundum, aluminium oxide, silica, cerium oxide, lanthana, sodium chloride, the sodium acid carbonate.Vitrified bond can provide bigger hold with respect to resinoid bond, and the heat conduction efficiency of vitrified bond is much higher than the conventional resins bond.Because the conventional resins bond is lower to the hold of abrasive particle, the granularity of abrasive particle generally is lower than #5000, and the diameter of corresponding abrasive particle generally is higher than 2 μ m.For ultra-fine abrasive particle, vitrified bond can provide higher hold, also can obtain enough porositys simultaneously, and realize the self-sharpening of emery wheel easily, and this has important effect for the finished surface that obtains uniform nano particle and ultra-smooth.Though metallic bond can provide higher hold and better heat conduction efficiency, also lost simultaneously emery wheel from sharp ability.Metallic bond is oxidation easily in grinding, and instability when ultra-fine abrasive wear, is not easy to come off, and it is very unfavorable for the size of control nano particle to grind bald diamond abrasive grain.And metallic bond also is not easy to obtain uniform porosity.In addition, metallic bond is in processing during same material, and it is cutting force big than vitrified bond longitudinally, makes that easily soft crisp semiconductor is broken.Therefore, the present invention selects vitrified bond for use.In order to reduce the cost of emery wheel, select the remarkable vitrified bond of performance commonly used, like carborundum, aluminium oxide, silica.Lanthana and cerium oxide are as lubricated and sintering aid.Sodium chloride and sodium acid carbonate are respectively applied for the particle that suppresses in the sintering and grow up and produce hole.Because the cubical contraction of different potteries when sintering is different, helps obtaining higher porosity.Too much ceramic species is not utilized the stability of control sintering temperature, therefore selects the 2-4 kind to be advisable.
The diameter of the nano particle that can prepare is 0.5-100 nm.Because science and technology and contemporary industry are that the demand of 0.5-100 nm is bigger for yardstick, machined parameters of therefore selecting for use and ultra-fine abrasive particle are mainly used in the particle of this yardstick of processing.
The nano hardness of workpiece≤15 GPa.Because the carborundum of selecting for use and the nano hardness of aluminium oxide are about 25 and 11.5 GPa, so the hardness of workpiece should not be too high, otherwise can make ultra-fine abrasive particle come off easily, therefore limit nano hardness≤15 GPa of workpiece.This hardness all is suitable for for most hard crisp and soft crisp semiconductor and photoelectric crystal.Hardness like traditional silicon, germanium, GaAs is respectively 12,10.5,6 GPa; The hardness of novel soft crisp semiconductor tellurium zinc cadmium and mercury cadmium telluride is respectively 1.2 GPa and 0.5 GPa; For nonlinear optical crystal lithium niobate and lithium tantalate; Nano hardness is respectively 6.3 and 5.5 GPa, and this restriction for workpiece hardness is enough to process most hard crisp and soft crisp semiconductor and photoelectric crystal.
Grinding fluid is a deionized water.Adopting deionized water as grinding fluid, mainly is cooling effect.Deionized water is a Green Grinding liquid, can not work the mischief to environment and operator, and also cheap, can cut down finished cost and the subsequent treatment expense, perhaps need not subsequent treatment.Make cooling fluid with deionized water, can obtain nano particle at normal temperatures, need not chemical reaction and hot conditions.
Effect of the present invention and benefit are to have realized that the hard crisp and soft crisp semi-conductive no chemical liquids ultraprecise processing of nano hardness≤15 GPa obtains the effect of nano particle.
The specific embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with technical scheme.
The workpiece of selecting for use is the silicon single crystal wafer of (100) six inches of Si, and grinding machine is the Japanese Okamoto product VG401 MKII of company ultraprecise grinding machine.Workpiece is fixed on the workbench with the vacuum ceramic sucker automatically.Ultra-fine abrasive material is a diamond, and granularity is #15000, and corresponding particle diameter is 700 nm, and adamantine concentration is 200, and promptly volumn concentration is 50%.The main component of vitrified bond is a carborundum, is mixed with a spot of aluminium oxide, and sodium chloride.Ultra-fine emery wheel sinters 56 teeth into, and each tooth is of a size of that 18 mm are long, 3 mm are wide, 5 mm are thick, be distributed in 350 mm diameters the groove at al alloy disk edge in, fix with high strength glue, pass through dynamic balancing after, be installed on the ultraprecise grinding machine.Grinding fluid is a deionized water.
Employing has the cast iron plate of texture and the silicon carbide abrasive particles of #600 is carried out shaping to novel ultra-fine emery wheel, adopts manual shaping methods, promptly gently rotates emery wheel with have gentle hands, rubs with the cast iron plate that is covered with silicon carbide abrasive particles, realizes shaping.After shaping is accomplished, adopts six inches silicon chip to try grinding so that obtain the nanometer grinding parameter comparatively optimized, and the completion emery wheel from sharp operation.The machined parameters of the final nanometer grinding of confirming is 8 μ m/min for axis feeding speed, and the speed of mainshaft is 1800 rpm, and rotating speed of table is 100 rpm.After manual tool setting is accomplished, remember its coordinate, carry out automated setting then.Apart from workpiece 20 μ m the time, begin to carry out above-mentioned nanometer grinding parameter.With top, carry out the fast feed of workpiece at 20 μ m.With the feeding distance after workpiece contacts is 80 μ m, i.e. lathe contact workpiece continued feeding 8 min, and feed-disabling continues tarry matter 0.5 min then, and with abundant release strain, this is very beneficial for improving the accuracy of form and position.Move back emery wheel then, accomplish the nanometer grinding.
After the nanometer grinding is accomplished, open the protective cover of ultraprecise grinding machine, collect grinding fluid with the clean beaker after the acetone sonicated.After grinding fluid shaken up, drip one with pipette and drop on the transmission electron microscope carbon film of standard of 3 mm diameters.Carbon film is 240 orders, and carbon film is placed on the filter paper, absorbs liquid, in dry environment, places after 1 day, deposits in the sample box of special transmission electron microscope, waits to do the transmission electron microscope experiment.The transmission electron microscope of selecting for use is FEI Tecnai G2 F30 S-twin, and directly will drip has the copper ring of abrasive dust or nano particle to be installed in the transmission electron microscope.Operating voltage is 300 kV.Under high-resolution-ration transmission electric-lens, the diameter of the nano particle that discovery obtains is at 30-60 nm.Thereby realized that the grinding of ultra-fine abrasive particle nanometer prepares the nano particle method, this method uses green deionized water as grinding fluid and cooling fluid, at room temperature adopts ultraprecise processing method to obtain the Si crystalline nanoparticles.
Claims (1)
1. ultra-fine abrasive particle nanometer grinding prepares the nano particle method, adopts the ultra-fine diamond abrasive material, preparation nanometer abrasive particle under the face abrasive machine mode of ductility territory, and grinding fluid is a deionized water, realizes the purpose of preparation nano particle, it is characterized in that:
(1) the nanometer grinding method is the face grinding of ductility territory;
(2) axis feeding speed is 1-100 μ m/min, and the speed of mainshaft is 1500-10000 rpm, and rotating speed of table is 40-500 rpm;
(3) wear particle size is #10000-#300000, and corresponding abrasive material diameter is below 1 μ m;
(4) abrasive material is a diamond, volumn concentration >=50%, corresponding diamond concentration >=200;
(5) bond is the 2-4 kind in carborundum, aluminium oxide, silica, cerium oxide, lanthana, sodium chloride, the sodium acid carbonate;
The diameter of the nano particle that (6) can prepare is 0.5-100 nm;
(7) nano hardness of workpiece≤15 GPa;
(8) grinding fluid is a deionized water.
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Cited By (5)
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| CN104385065A (en) * | 2014-12-05 | 2015-03-04 | 山东大学 | Quartz glass ductile-regime grinding method based on laser crack pre-repairing |
| CN104551871A (en) * | 2014-12-31 | 2015-04-29 | 浙江工业大学 | Lithium tantalate wafer grinding method |
| CN104802043A (en) * | 2015-04-23 | 2015-07-29 | 山东大学 | Self-heating assisted efficient ductile-mode ultra-precision quartz glass grinding method |
| CN106737247A (en) * | 2017-01-03 | 2017-05-31 | 山东理工大学 | A kind of grinding tool of tangential grinding force high and low normal grinding force |
| CN107042467A (en) * | 2017-04-07 | 2017-08-15 | 大连理工大学 | Nm deep damages layer mechanochemistry method for grinding |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104385065A (en) * | 2014-12-05 | 2015-03-04 | 山东大学 | Quartz glass ductile-regime grinding method based on laser crack pre-repairing |
| CN104551871A (en) * | 2014-12-31 | 2015-04-29 | 浙江工业大学 | Lithium tantalate wafer grinding method |
| CN104802043A (en) * | 2015-04-23 | 2015-07-29 | 山东大学 | Self-heating assisted efficient ductile-mode ultra-precision quartz glass grinding method |
| CN106737247A (en) * | 2017-01-03 | 2017-05-31 | 山东理工大学 | A kind of grinding tool of tangential grinding force high and low normal grinding force |
| CN107042467A (en) * | 2017-04-07 | 2017-08-15 | 大连理工大学 | Nm deep damages layer mechanochemistry method for grinding |
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Application publication date: 20120912 |