CN206965838U - A kind of preparation facilities of nano particle - Google Patents
A kind of preparation facilities of nano particle Download PDFInfo
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- CN206965838U CN206965838U CN201720322502.5U CN201720322502U CN206965838U CN 206965838 U CN206965838 U CN 206965838U CN 201720322502 U CN201720322502 U CN 201720322502U CN 206965838 U CN206965838 U CN 206965838U
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Abstract
The utility model discloses a kind of preparation facilities of nano particle, belong to field of nano material preparation.Material is melted or gasified in local pole tiny area position for workpiece to be processed first in a condensed environment by this patent so that the product of fusing or gasification condenses rapidly, forms loose micron or nano particle, forms ablation product（Such as spark discharge processing）Ablation product feeding high-energy ball milling is handled again, the material formed by material caused by the fusing or gasification of local pole tiny area after rapid condensation has extremely loose structure, particularly suitable for ball milling, on the one hand rapidoprint can will be needed quickly to form micro-nano granules using such processing mode, on the other hand, the loose structure that microballoon has is ensure that, the speed that ball milling is processed is significantly improved.This processing mode can easily obtain the micro-nano granules of loose from particular volume material, greatly accelerate ball milling speed.
Description
Technical field
A kind of preparation facilities of nano particle is the utility model is related to, belongs to field of nanometer material technology technology.
Background technology
Due to nano particle have small-size effect, surface and interfacial effect, quantum effect, macro quanta tunnel effect and
Catalytic effect.Therefore, it is in catalytic performance, optical property, magnetic property, activeness and quietness performance, hydrogen storage property and greasy property etc.
Aspect has exceptional function, so as to obtain a wide range of applications.It is mainly used in：Catalyst, nano electron device, sensor,
Magnetic material, optics and stealth material and activeness and quietness material, biomedical material.There is nanometer in terms of activeness and quietness material
Particle activeness and quietness material, nano whisker, fibre reinforced materials, nano particle help agglomerated material, nano-weld technology.
Focus of the preparation of nano material as current research, numerous experts and scholars both domestic and external expand extensively to it
Research.At present, the preparation of nano particle has many methods, mainly there is sol-gal process, chemical vapour deposition technique, laser pyrolysis
Method, Plasma synthesis method etc..However, the existing method for preparing nano particle, process route is complicated, poor controllability and yields poorly
Etc. a series of deficiencies.
When carrying out preparing nano particle using ball-milling technology, the particle diameter that material is put into when in ball milling chamber in itself is that have strict limit
System, particle is thinner, and grinding efficiency is higher, and energy consumption is with regard to smaller.But the nanometer for thering are some to need to prepare some specific compositions
During particle（Such as some special alloys, semi-conducting material）, due to being the workpiece of monoblock when prepared by material material itself complete, it is
There can be a great processing difficulties from the body materials of these special compositions and then when nano particle is prepared.Generally, body material
Material can not directly carry out ball milling, it is necessary to Centimeter Level is first crushed to, then with big abrading-ball by its ball milling to millimeter
Level, then use smaller abrading-ball instead and continue to be milled to several microns, finally change smaller abrading-ball and continue to be refined to nanoscale, this is more
Level mechanical milling process is related to the abrading-ball and equipment of plurality of specifications, and energy consumption is huge and with high costs.
Utility model content
Existing difficulty during nano particle is obtained for above-mentioned processing lumpy body material, the utility model provides
A kind of novel combinational processing method.The method of this patent is in office first in a condensed environment for workpiece to be processed
Material is melted or gasified atomic zonule position in portion so that the product of fusing or gasification condenses rapidly, is formed loose
Micron or nano particle, formed ablation product, then by ablation product feeding high-energy ball milling handled, it is small by local pole
The material that material caused by the fusing or gasification in region is formed after rapid condensation has extremely loose structure, particularly suitable for
Ball milling, on the one hand rapidoprint can will be needed quickly to form micro-nano granules using such processing mode, on the other hand, protected
The loose structure that microballoon has has been demonstrate,proved, the speed that ball milling is processed is significantly improved.For fusing or the mistake of gasification materials
Journey, can use spark discharge processing mode, and this processing mode easily can obtain loose from particular volume material
Micro-nano granules, greatly accelerate ball milling speed.In addition, when being coupled with Process During High Energy Ball Milling, spark discharge technique
It is so harsh when need not be as preparing nano particle, using high current, big pulsewidth, coordinate numerical control feeding, it is possible to achieve quick erosion
Except body material efficiently prepares micron or submicron particles material, speed is that single spark discharge technique prepares nano particle speed
More than hundred times, what the pretreatment of such high speed can similarly greatly save that time-consuming during traditional grading ball milling lacks
Point, and such pretreatment mode can also solve the problems, such as high energy consumption existing for conventional multi-level ball milling bulky grain, overall energy
Consumption is also far smaller than the energy consumption needed for single ball-milling technology, the workpiece of certain material can be quickly prepared as into nano particle.
In addition, the coupling by high-energy ball milling and spark discharge, it is possible to achieve reduce spark discharge technique present in micron or
The problem of particle diameter distribution of submicron particles is uneven, finally make it that nano particle diameter distribution is narrower.
A kind of method that spark discharge and high-energy ball milling group technology prepare nano particle, comprises the following steps：
1st step, in condensed environment, high temperature melting and/or gasification are carried out to the surface of workpiece to be processed, and make fusing
And/or the material of gasification condenses rapidly, ablation product is formed；
2nd step, ablation product is sent into high-energy ball milling device and carries out wet ball grinding, obtains nano-particle.
Comprising the concrete steps that in the 1st described step：Using material to be processed as piece pole, then by piece pole and instrument
Electrode is connected on the two poles of the earth of the pulse power respectively, makes to form continuous pulse feature between tool-electrode and piece pole in working solution and puts
Electricity, material is removed using high temperature caused by spark discharge, obtains ablation product.
In the 1st described step, material to be processed is preferably capable of carrying out any material of electro-discharge machining, as electric conductivity is good
Metal material（Such as：Copper, silver etc.）, the semi-conducting material of conductive energy（Such as silicon, germanium）, and insulating materials（Ceramics,
Jewel etc.）.
In the 1st described step, material to be processed can be pure substance（Such as metal, the intrinsic semiconductor material of single-element
Material etc.）Or mixture（E.g. metal alloy, doped semiconductor materials etc.）.
In the 1st described step, when workpieces processing is insulating materials, it is necessary to be that workpieces processing increases an auxiliary electrode,
Piece pole is integrally formed；The nanoparticle without any impurity can be obtained when tool-electrode and workpieces processing are same material
Son.
In the 1st described step, it is necessary to will cool down gas or coolant flow through at a high speed it is between tool-electrode and piece pole plus
Break gap, ablation product is taken out of at discharge channel, improve processing gap state, ensure being smoothed out for processing.
Described condensed environment refers to there is condition existing for cooling gas or coolant.
The iknsulating liquids such as the preferred deionized water of coolant, aviation kerosine.
The pulsewidth of electric pulse caused by the pulse power is preferably the μ s of 0.1 μ s~500.
High-speed punching hydraulic pressure is preferably 1MPa~20MPa by force.
In the 1st described step, the particle in working solution can be after filtering, then is sent into after being formulated as slurry at the 2nd step
Reason；Can also be that the working solution containing particle is directly sent into the processing of the 2nd step.
In the 2nd described step, the size preferable particle size of abrading-ball is 0.03~1mm, the preferred zirconium oxide of material of abrading-ball, oxidation
Aluminium, steel etc..
In the 2nd described step, the preferred deionized water of grinding aid, ethanol, ethylene glycol, polyethylene glycol, butyl acetate, propyl alcohol,
Isopropanol, butanol or other organic solvents, but can not be with treating that it is anti-that chemistry occurs for abrasive particle, abrading-ball and other materials contacted
Should.
The ratio that the quality of particle accounts for gross mass in slurry is preferably 0.1~30%.
The time of high-energy ball milling is preferably 1~80h.
Slurry is circulated by pump between material cylinder and ball milling chamber.
Grid in ball milling chamber separates slurry and abrading-ball, and slurry can be freed in and out, and abrading-ball is blocked in ball milling chamber,
Ensure being normally carried out for high-energy ball milling.
A kind of spark discharge and high-energy ball milling group technology prepare the device of nano particle, include：Spark discharge is processed
Device and high-energy ball milling device；
Include in described spark discharge processing unit (plant)：
Tool-electrode and piece pole, it is connected to the two poles of the earth of the pulse power；
Digital control system, for controlling the feeding of piece pole；
Work tank, inside are equipped with working solution, and tool-electrode and piece pole submergence are wherein；
Working solution circulating slot, interlinked for depositing working solution, and with work tank；
First delivery pump, for making working solution be circulated in working solution circulating slot；
Filter, for the particle of acquisition to be filtered out；
Include in described high-energy ball milling device：
Ball milling chamber, inside are equipped with dispersion impeller, dispersion impeller and motor connection, abrading-ball are housed in ball milling chamber.
Also include material cylinder, and the second delivery pump, for slurry to be circulated between material cylinder and ball milling chamber.
Also include grid, for abrading-ball to be limited in ball milling chamber.
Mixer is additionally provided with described material cylinder.
Described ball milling chamber is arranged on ball-grinding machine pedestal.
Beneficial effect
The advantage that spark discharge and high-energy ball milling group technology prepare nano particle is that the preparation of energy high efficiency, low cost is received
Rice grain, controllability are strong.
The beneficial effects of the utility model include：
1st, after carrying out localized hyperthermia's fusing and gasification materials using the fine region to workpieces processing, loose knot can be obtained
The micro-nano granules of structure, nano particle can be easily crushed into, ball milling process velocity can be greatly enhanced；
2nd, employ spark discharge processing rapidly can obtain micro-nano granules from the workpiece for needing to process, then lead to
The uniform nano particle of particle diameter distribution can be obtained by crossing high-energy ball milling, and solving can not be quickly from certain material in conventional method
The problem of nano particle is obtained on bulk workpiece；
3rd, micro-nano granules can be quickly obtained by using spark discharge processing, solves traditional high-energy ball milling behaviour
The problem of ball milling step by step is needed in work to reduce more number of devices during particle diameter, complex operation.
4th, integrated by high-energy ball milling and electro-discharge machining, can solve that the particle diameter distribution in electro-discharge machining is uneven to ask
Topic.
Brief description of the drawings
Fig. 1 is the spark discharge processing unit (plant) structure chart in embodiment 1；
Fig. 2 is the high-energy ball milling structure drawing of device in embodiment 1；
Fig. 3 is spark discharge-high-energy ball milling process installation drawing in embodiment 2；
Fig. 4 is spark discharge-high-energy ball milling process installation drawing in embodiment 3.
Fig. 5 is to process the obtained electron microscope of micro-nano granules by spark discharge.
Fig. 6 is to process the obtained grain size distribution of micro-nano granules by spark discharge.
Fig. 7 is the grain size distribution for the nano particle that spark discharge and high-energy ball milling integrated approach obtain.
Wherein；1st, the pulse power；2nd, digital control system；3rd, work tank；4th, tool-electrode；5th, working solution；6th, piece pole；
7th, displacement platform；8th, working solution circulating slot；9th, filter；10th, the first delivery pump；11st, material cylinder；12nd, slurry；13rd, stir
Machine；14th, ball milling chamber；15th, grid；16th, abrading-ball；17th, dispersion impeller；18th, motor；19th, ball-grinding machine pedestal；20th, the second delivery pump；
21st, cyclone separator.
Embodiment
Embodiment 1
A kind of spark discharge processing provided by the utility model coupled with high-energy ball milling processing unit (plant) structure such as Fig. 1 and
Shown in Fig. 2.Spark discharge technique prepares the device of micron or submicron particles, and work tank 3 is fixed on displacement platform 7,
Piece pole 6 is fixed in work tank 3, realizes the feeding of piece pole 6 by digital control system 2, piece pole 6 is promoted blood circulation punching
The positive pole of power supply 1, the negative pole of the pulse current source 1 of tool-electrode 4, tool-electrode 4 is tubulose；Work is added in work tank 3
Liquid 5, the gap between dipped piece pole 6 and tool-electrode 4.Continuous pulse is formed between tool-electrode 4 and piece pole 6
Property spark discharge, make material surface that fusing and gasification occur using caused high temperature, then by working solution 5（Equivalent to coolant）
Condensation after, remove piece pole 6, obtain ablation product, this ablation product is to condense generation rapidly by gasification materials,
With loose internal structure；Working solution 5 forms high speed fliud flushing by the first delivery pump 10 and tool-electrode 4, by ablation product
Take out of at discharge channel, and flowed into working solution 5 in the working solution circulating slot 8 with filter 9, it is micro- by being filtrated to get
Rice or submicron particles；Working solution 5 recycles.
In fig. 2, high-energy ball milling uses wet ball grinding, first is dispersed in be formed micron or submicron particles in grinding aid and starches
Material 12, is placed in material cylinder 11, mixer 13, which rotates at a high speed, prevents particle from settling, and slurry 12 is delivered to by the second delivery pump 20
In ball milling chamber 14, dispersion impeller 17 is provided with ball milling chamber 14；Abrading-ball 16 is placed in ball milling chamber 14, and dispersion impeller 17 drives in motor 18
Lower high speed rotation, drives abrading-ball 16 and particle high-speed motion, particle is refined into nanoscale by collision repeatedly；Slurry 12 is logical
Cross the second delivery pump 20 constantly to circulate between material cylinder 11 and ball milling chamber 14, make all particles can be by ball milling, ball milling chamber 14
Side carry the device of grid 15, slurry 12 and abrading-ball 16 can be separated, slurry 12 can be returned in material cylinder 11 by grid 15,
And abrading-ball 16 is blocked in ball milling chamber 14；Finally slurry 12 is centrifuged, can obtain nano particle；The recyclable profit of grinding aid
With.
For above-mentioned displacement platform 7 using the three coordinate sub-micron control platforms commonly used in electrical discharge machining, it is fixed to repeat
Position precision<5 μm, feed resolution ratio<5μm.
The technical solution of the utility model is further described with reference to preparation process：
Doped silicon is selected first（Resistivity is 0.01 Ω cm）（Size 125mm*125mm*10mm）As piece pole 6
It is fixed in work tank 3, the tool-electrode 4 of use is copper pipe（Dimension D 3mm*150mm）, it is working solution from deionized water
5。
The positioning and feeding of piece pole 6 are controlled by digital control system 2, utilizes discharge pulse caused by the pulse power 1
Pulsewidth is 100 μ s, dutycycle 1:4, open-circuit voltage 160V square-wave voltage is applied between piece pole and tool-electrode,
Ionization, breakdown insulated working medium form plasma discharge passage, after caused high temperature melting, gasification piece pole are condensed
To micron or sub-micron silicon grain.
At the same time, high speed fliud flushing takes ablation product out of at discharge channel, and ablation product is flowed into working solution 5 and carried
In the working solution circulating slot 8 of filter 9, micron or sub-micron silicon grain are obtained after filtering, its electron microscope is as shown in figure 5, grain
Footpath distribution map is as shown in fig. 6, its median particle diameter about 1560nm.
By the micron being collected into or sub-micron silicon grain and grinding aid（From deionized water）In mass ratio 1：19 mixing are equal
It is even to obtain slurry 12（Silicon grain 200g, deionized water 3800g）, after being poured into material cylinder 11, mixer 13 is stirred continuously.
A diameter of 0.1mm zirconium oxide balls 16 are housed in ball milling chamber 14, first start motor 18, drive dispersion impeller 17 at a high speed
Rotation, its edge linear velocity reaches 13.5m/s, and then drives the high-speed motion of abrading-ball 16.Restart the second delivery pump 20, make slurry 12
Constantly circulated between material cylinder 11 and ball milling chamber 14, high-energy ball milling 10 hours, ensure that all silicon grains can be by abundant ball milling.
After silicon grain manufactured in the present embodiment is purified, analyzed by X-ray fluorescence spectra（XRF）Analysis measures its purity
97%；Its particle diameter D50=80nm is analyzed using laser particle analyzer.
In the present embodiment, spark discharge prepares micron or sub-micron silicon grain yield is 200g/h, and high-energy ball milling is prepared and received
Rice silicon grain yield is 20g/h.
Reference examples 1
Difference with embodiment 1 is：It is micro- that doped silicon is first ground into about 5 μm of median particle diameter using the method for machining
Powder, it is re-fed into high-energy ball milling device, carries out ball-milling treatment using identical parameters, after ball milling 15h, analyzed using laser particle analyzer
Its particle diameter D50=210nm, compared embodiment 1 with reference examples 1 as can be seen that being obtained by way of by spark discharge micro-
Nano particle can greatly speed up the process velocity of high-energy ball milling.
Embodiment 2
As shown in Figure 1 and Figure 2, spark discharge technique prepares the device of micron or submicron particles and high-energy-milling will
Micron or submicron particles are prepared into the device of nano particle, and the difference with embodiment 1 is that workpiece material is nonconducting
Silicon is levied, working solution is the Na that concentration is 10%2CO3Solution, working solution is conductive, serves as auxiliary electrode.
Nano silicon particles manufactured in the present embodiment, are analyzed by X-ray fluorescence spectra（XRF）Analysis measures its purity and existed
91%；Its particle diameter D50=80nm is analyzed using laser particle analyzer.
Embodiment 3
As shown in Figure 1 and Figure 2, spark discharge technique prepares the device of micron or submicron particles and high-energy-milling will
Micron or submicron particles are prepared into the device of nano particle, and the difference with embodiment 1 is that the grinding aid of ball milling is anhydrous second
Alcohol, Ball-milling Time 20h.
Nano silicon particles manufactured in the present embodiment, are analyzed by X-ray fluorescence spectra（XRF）Analysis measures its purity and existed
97%；Its particle diameter D50=60nm is analyzed using laser particle analyzer.
Embodiment 4
As shown in Figure 1 and Figure 2, spark discharge technique prepares the device of micron or submicron particles and high-energy-milling will
Micron or submicron particles are prepared into the device of nano particle, and the difference with embodiment is that the piece pole 6 of use is copper, ball
The grinding aid of mill is absolute ethyl alcohol.
Copper nano particles manufactured in the present embodiment, are analyzed by X-ray fluorescence spectra（XRF）Analysis measures its purity and existed
99.9%；Its particle diameter D50=75nm is analyzed using laser particle analyzer.
Embodiment 5
The processing of another spark discharge couples processing unit (plant) with high-energy ball milling, as shown in figure 3, in order to prevent electric spark
Reunion can be produced after by filtering and concentrating by processing obtained micro-and nano-particles, can also by working solution circulating slot 8 directly with
High-energy ball milling device is coupled, and the working solution 5 in working solution circulating slot 8 is fed directly in ball milling chamber 14 by the second delivery pump 20,
Because micro-and nano-particles are directly scattered in working solution, the agglomeration traits easily occurred after filtering is taken out are avoided, here
Working solution can use water, can also add a certain amount of ball-milling additive in working solution.Furthermore it is also possible to using another electricity fire
Flower electro-discharge machining couples processing unit (plant) with high-energy ball milling, as shown in figure 4, being connected with cyclonic separation in the outlet of the second delivery pump 20
Device 21, is acted on by cyclonic separation, micro-nano can obtain initial gross separation, cyclone separator 21 by what is obtained in electrical discharge machining
Heavy material outlet and light material outlet be all delivered to ball milling chamber, the tie point of light material outlet is closer to grid 15, therefore gently
Range ability of the small size particle in ball milling chamber 14 in material is relatively short, avoids prolonged ball milling so that ball milling
The particle diameter distribution that process finally gives is more uniform.
Claims (5)
1. a kind of preparation facilities of nano particle, it is characterised in that include：Spark discharge processing unit (plant) and high-energy ball milling dress
Put；
Include in described spark discharge processing unit (plant)：
Tool-electrode（4）And piece pole（6）, it is connected to the pulse power（1）The two poles of the earth；
Digital control system（2）, for controlling piece pole（6）Feeding；
Work tank（3）, inside is equipped with working solution（5）, tool-electrode（4）And piece pole（6）Submergence is wherein；
Working solution circulating slot（8）, for depositing working solution（5）, and and work tank（3）Interlink；
First delivery pump（10）, for making working solution（5）In working solution circulating slot（8）In circulate；
Filter（9）, for the particle of acquisition to be filtered out；
Include in described high-energy ball milling device：
Ball milling chamber（14）, inside is equipped with dispersion impeller（17）, dispersion impeller（17）With motor（18）Connection, in ball milling chamber（14）In be equipped with
Abrading-ball（16）.
2. the preparation facilities of nano particle according to claim 1, it is characterised in that also include material cylinder（11）, with
And second delivery pump（20）, for by slurry（12）In material cylinder（11）With ball milling chamber（14）Between circulate.
3. the preparation facilities of nano particle according to claim 1, it is characterised in that also including grid（15）, for inciting somebody to action
In abrading-ball（16）It is limited to ball milling chamber（14）In.
4. the preparation facilities of nano particle according to claim 2, it is characterised in that described material cylinder（11）In also set
It is equipped with mixer（13）.
5. the preparation facilities of nano particle according to claim 1, it is characterised in that described ball milling chamber（14）It is arranged at
Ball-grinding machine pedestal（19）On.
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| CN201720322502.5U CN206965838U (en) | 2017-03-30 | 2017-03-30 | A kind of preparation facilities of nano particle |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106881174A (en) * | 2017-03-30 | 2017-06-23 | 南京航空航天大学 | The preparation method and device of a kind of nano particle |
| CN108514928A (en) * | 2018-04-03 | 2018-09-11 | 中国矿业大学 | A kind of dispersion mill preparing nano-material modified cement |
-
2017
- 2017-03-30 CN CN201720322502.5U patent/CN206965838U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106881174A (en) * | 2017-03-30 | 2017-06-23 | 南京航空航天大学 | The preparation method and device of a kind of nano particle |
| CN106881174B (en) * | 2017-03-30 | 2018-10-12 | 南京航空航天大学 | A kind of preparation method and device of nano particle |
| CN108514928A (en) * | 2018-04-03 | 2018-09-11 | 中国矿业大学 | A kind of dispersion mill preparing nano-material modified cement |
| CN108514928B (en) * | 2018-04-03 | 2020-05-08 | 中国矿业大学 | Dispersion mill for preparing nano material modified cement |
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