CN103785511B - A kind of microwave ultrasound associating auxiliary ball mill apparatus and technique preparing high-performance nano powder - Google Patents
A kind of microwave ultrasound associating auxiliary ball mill apparatus and technique preparing high-performance nano powder Download PDFInfo
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Abstract
Applicant has invented a kind of microwave ultrasound associating auxiliary ball mill apparatus and technique preparing high-performance nano powder.This device is that ball mill is placed in microwave generator, and the bottomless ball grinder in ball mill is connected with supersonic generator top, composition microwave ultrasound associating auxiliary ball grinding machine.This process characteristic is that medium solution in ball grinder and material powder are subject to hyperacoustic cavitation simultaneously, the triple roles such as the radiation effects of microwave and the mechanical force of ball milling, the speed of the reactions such as reduction, oxidation, synthesis, decomposition is increased greatly, and some chemical reactions that originally cannot realize separately through microwave radiation technology ball milling or independent ultrasonic wave added ball milling are occurred; This device can be used for preparing the multiple nano functional powder such as metal oxide, ferrite, complex ferrite, absorbing material, luminescent material, magnetic material.
Description
Technical field
The invention belongs to the field of grinding, specifically a kind of microwave ultrasound associating auxiliary ball mill apparatus and technique preparing high-performance nano powder.
Background technology
Nanometer ferrite has good microwave absorption energy and desirable magnetic performance, is widely used in microwave absorbing coating, inhales ripple divider wall, high frequency magnetic recording, magnetic resonance device, and sensor field.The main preparation method preparing the Magnaglos such as nanometer ferrite and other nanometer powders at present has sol-gel process, hydro-thermal method, microwave-hydrothermal method, coprecipitation, citrate precursor process, high-energy ball milling method etc.But these methods or environmental pollution are serious, or energy consumption is large, or the shortcoming such as the production time is long.
Microwave is a kind of Novel heating energy of efficient and environmental protection, and it has been widely used in the daily productive life of people.Microwave has and selectively adds thermal property, thus in separating substances, the aspects such as ore grinding have also played the characteristic of its excellence.Microwave heating method has a lot of advantages: first it does not need high temperature and high pressure, and nano materials is simple and quick; In addition, microwave method is effective especially to the large-scale synthesis of control, because it can reduce the impact of thermal gradient to greatest extent.Secondly, because solvent is different with the dielectric constant of reactant, the selective heating of medium can significantly improve reaction rate; The most important advantage of the method is the Convective Heating of micro-wave dielectric, and reactant can be added under room temperature (or slightly high-temperature).And, the size of nano particle can be adjusted by the concentration changing presoma and pass through to change the concentration of solvent and form with the shape controlling microwave irradiation time and nanostructured.
Ultrasonic wave is in certain Propagation process, and can interact between propagation medium, its result caused is exactly that the parameter such as hyperacoustic phase place and amplitude can change thereupon, and then causing the physical property of propagation medium and chemical property to change, namely this phenomenon is called ultrasonic effect.Ultrasonic effect specifically can be divided into four classes, i.e. fuel factor, cavitation effect, mechanical effect and chemical effect.The concrete factor affecting ul-trasonic irradiation effect comprises surface tension and the coefficient of viscosity of hyperacoustic intensity, frequency and liquid.Ultrasonic cavitation acts on the application of chemical field, the machinery mainly utilizing ultrasonic wave to produce and chemical effect.Wherein mechanical effect main manifestations is the increase of heterogeneous reaction interface under ul-trasonic irradiation; Chemical effect is mainly due to the shattered to pieces TRANSIENT HIGH TEMPERATURE high pressure caused of cavitation effect hollow bubble, and under the effect of this larger power, the molecular structure of material is destroyed, and new bond structure is formed.Ultrasonic wave in practice, is mainly used in cleaning, catalysis, the aspect such as wastewater treatment and plating.
Ball-milling method is industrially applied to the main stream approach preparing nanometer powder in the world at present.But ball-milling method mainly to there is the ball action time long preparing in nanometer powder, product great efforts, the major defects such as granular size is uneven, poor repeatability, become restriction ball-milling method and are industrially widely used in bottleneck prepared by nanometer powder.
This team SEPARATE APPLICATION patent of invention (ZL201110004753.6, ZL200910309641.4) such as microwave radiation technology ball milling and ultrasonic wave added ball milling; These two patents all have certain progressive, but the part that also comes with some shortcomings, need to make improvements.
Summary of the invention
The object of the present invention is to provide a kind of microwave ultrasound associating auxiliary ball mill apparatus and the technique of preparing high-performance nano powder, present invention incorporates the advantage of microwave, ultrasonic wave and ball milling, make, at low equipment requirement, under the conditions such as low environment pollution, various high performance nanometer powder to be prepared efficiently.
For achieving the above object, the invention provides following technical scheme:
A kind of microwave ultrasound associating auxiliary ball mill apparatus preparing high-performance nano powder, described ball mill device comprises motor, puddler, ball grinder, abrading-ball, described motor drives puddler, described puddler extend in the abrading-ball of ball grinder, described ball grinder is provided with ball milling cover, described ball grinder covers and is provided with cooling back installation and liquid supply device, described ball grinder is placed on microwave generator inside, and cooling back installation, puddler and liquid supply device reach microwave generator outside, supersonic generator is provided with immediately below described ball grinder, described supersonic generator comprises ultrasonic transducer, and the ultrasonic wave cylindrical shell of ultrasonic transducer outside, and bottom ultrasonic wave cylindrical shell top and microwave generator, and the flange seal of the bottom of bottomless ball grinder connects.
As the further scheme of the present invention: described cooling back installation, puddler, ball grinder and liquid supply device all adopt polytetrafluoroethylene (PTFE) to process or pottery is made.
As the further scheme of the present invention: Ceramic Balls or the metal ball of described abrading-ball to be diameter be 0.5-2mm.
As the further scheme of the present invention: described metal ball comprises stainless steel ball, iron ball, copper ball and titanium ball.
As the further scheme of the present invention: be provided with sealing device between described ultrasonic wave cylindrical shell top and the flange in the bottom of bottomless ball grinder.
Adopt described microwave ultrasound associating auxiliary ball mill apparatus to prepare a technique for high-performance nano powder, concrete steps are:
(1) pour material powder and medium solution and abrading-ball into ball grinder, ensure that the liquid level of medium solution is at the 1/2-3/4 place of ball grinder total height, covers ball milling cover;
(2) open motor, open supersonic generator, motor rotary speed is that 100-1250 per minute turns, and motor drives puddler, and puddler drives abrading-ball to grind 10-20 minute to material powder;
(3) open microwave generator again to work together, the power of microwave generator is 0.8-1.2KW, and frequency is 2450MHz, the power of supersonic generator is 150-250W, and frequency is respectively 20KHz, 28KHz, and 40KHz, carry out radiation 10-20 minute, close microwave generator.
(4) step (2) and step (3) is repeated, until obtain target product.
As the further scheme of the present invention: ensure in step (1) that the liquid level of medium solution is at the 1/2-3/4 place of ball grinder total height.
As the further scheme of the present invention: motor rotary speed described in step (2) is 235 turns per minute, and the time of grinding is 15 minutes, and the power of supersonic generator is 200W, and frequency is respectively 20KHz, 28KHz, and 40KHz.
As the further scheme of the present invention: described in step (3), the power of microwave generator is 1KW, frequency is 2450MHz, carries out radiation 15 minutes.
Compared with prior art, the invention has the beneficial effects as follows:
Medium solution in ball grinder and material powder are subject to hyperacoustic cavitation simultaneously, the triple roles such as the radiation effects of microwave and the mechanical force of ball milling, the speed of the reactions such as reduction, oxidation, synthesis, decomposition is increased greatly, and some chemical reactions that originally cannot realize separately through microwave radiation technology ball milling or independent ultrasonic wave added ball milling are occurred; This device can be used for preparing the multiple nano functional powder such as metal oxide, ferrite, complex ferrite, absorbing material, luminescent material, magnetic material.
Accompanying drawing explanation
Fig. 1 is the structural representation of microwave ultrasound associating auxiliary ball mill apparatus;
Be designated as under it: 1-motor, 2-cooling back installation, 3-screw, 4-puddler, 5-ball grinder, 6-microwave generator, 7-sealing device, 8-ultrasonic transducer, 9-ultrasonic wave cylindrical shell, 10-liquid supply device, 11-abrading-ball, 12-ball milling cover;
Fig. 2 is for adopting iron powder and nickel oxide, and Zinc oxide powder is raw material, the XRD figure of the product after different Ball-milling Time;
Fig. 3 combines by microwave ultrasound the Ni nanoparticle ZnFe that auxiliary ball-milling method obtains
2o
4tEM figure;
Fig. 4 combines by microwave ultrasound the Ni nanoparticle ZnFe that auxiliary ball-milling method obtains
2o
4tEM figure;
Fig. 5 combines by microwave ultrasound the Ni nanoparticle ZnFe that auxiliary ball-milling method obtains
2o
4sAED picture;
Fig. 6 is the hysteresis curve figure being combined the nickel-zinc ferrite that auxiliary ball-milling method obtains after the different disposal time by microwave ultrasound;
Fig. 7 is the XRD figure of the product obtained after 10 hours microwave ultrasounds combine auxiliary ball milling;
Fig. 8 is the TEM figure of the nano zine oxide that microwave ultrasound associating auxiliary ball mill apparatus prepares.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Refer to Fig. 1, a kind of microwave ultrasound associating auxiliary ball mill apparatus preparing high-performance nano powder, described ball mill device comprises motor 1, puddler 4, ball grinder 5, abrading-ball 11 and ball milling cover 12, described motor 1 drives puddler 4, described puddler 4 extend in the abrading-ball 11 of ball grinder 5, described ball grinder 5 connects ball milling cover 12 by screw 3, described ball milling cover 12 is provided with cooling back installation 2 and liquid supply device 10, it is inner that described ball grinder 5 is arranged on microwave generator 6, and cooling back installation 2, it is outside that puddler 4 and liquid supply device 10 reach microwave generator 6, supersonic generator is provided with immediately below described ball grinder 5, described supersonic generator comprises ultrasonic transducer 8, and the ultrasonic wave cylindrical shell 9 of ultrasonic transducer 8 outside, and bottom ultrasonic wave cylindrical shell 9 top and microwave generator 6, and the flange in the bottom of bottomless ball grinder 5 is tightly connected.
As the further scheme of the present invention: the power of described motor 1 is 1200W, and rotating speed is 235 revs/min; The power of described microwave generator 6 is 1000W, and micro-wave frequency is 2450MHz; The power of described ultrasonic transducer 8 is 200W, and frequency is 20KHz, 28KHz and 40KHz.
As the further scheme of the present invention: described cooling back installation 2, puddler 4, ball grinder 5 and liquid supply device 10 all adopt polytetrafluoroethylene (PTFE) to be processed into; Ceramic Balls or the metal ball of described abrading-ball 11 to be diameters be 0.5-2mm; Described metal ball comprises stainless steel ball, iron ball, titanium ball and copper ball; Sealing device 7 is provided with between the flange in the bottom of described ultrasonic wave cylindrical shell 9 top and bottomless ball grinder 5.
A kind of technique adopting described microwave ultrasound associating auxiliary ball mill apparatus to prepare high-performance nano powder, concrete steps are: pour material powder and medium solution (water or other organic solvents) and abrading-ball 11 into ball grinder 5, ensure that the liquid level of medium solution is at the 1/2-3/4 place of ball grinder 5 total height, is preferably 2/3; Cover ball milling cover 12; Then open motor 1, drive puddler 4, puddler 4 drives abrading-ball 11 pairs of material powders to grind; Or open motor 1 and microwave generator 6 pairs of material powders carry out microwave radiation technology ball milling simultaneously; Or open motor 1 and supersonic generator simultaneously, ultrasonic assistant ball milling is carried out to material powder; Or motor 1 of performing fighting, microwave generator 6 and supersonic generator carry out microwave ultrasound to material powder and combine auxiliary ball milling simultaneously, there is various physics or chemical or physical-chemical reaction in material powder, thus obtain high-performance nano powder under the effect of the combination of ball milling, microwave and ultrasound.
The mechanism of action of the present invention is: the medium solution in ball grinder and material powder are subject to hyperacoustic cavitation simultaneously, the triple roles such as the radiation effects of microwave and the mechanical force of ball milling, the speed of the reactions such as reduction, oxidation, synthesis, decomposition is increased greatly, and some chemical reactions that originally cannot realize separately through microwave radiation technology ball milling or independent ultrasonic wave added ball milling are occurred; This device can be used for preparing the multiple nano functional powder such as metal oxide, ferrite, complex ferrite, absorbing material, luminescent material, magnetic material.
In order to set forth the present invention further, refer to following embodiment.
Embodiment 1: microwave ultrasound associating auxiliary ball grinds standby high-performance nano nickel zinc complex ferrite
Reactant is analytically pure nickel oxide, zinc oxide and iron powder, first prepare according to certain chemical ratios, mix, be then the ball grinder that the mass ratio of 100:1 puts into Ф 135 × 215mm with ratio of grinding media to material by reactant, then add 2/3 place of deionized water to jar.Open motor 1 and supersonic generator, the power of supersonic generator is 200W, and frequency is 20KHz, starts stirring ball-milling, speed of agitator is 235 turns per minute, reactant is carried out aqueous solution ball milling 15 minutes, and then open microwave generator and work together, the power of microwave generator is 1KW, frequency is 2450MHz, carry out radiation 15 minutes, then ultrasonic ball milling 15 minutes again, so repeatedly; Sample after the regular hour, first the sample of taking-up is placed on filter filtration on paper, to be then placed in drying box at the temperature of 50 DEG C dry 12 hours; Again the sample taken out is ground, then undertaken characterizing and detecting by detection means such as XRD, VSM, TEM, SAED.
As can be seen from Figure 2, after 6 hours microwave ultrasounds combine auxiliary ball milling, there is a small amount of NiZnFe
2o
4, after 18 hours, iron powder and nickel oxide, oxide powder and zinc reacts completely, and all diffraction maximums obtained correspond to spinel-type NiZnFe completely
2o
4.Prove microwave ultrasound combine auxiliary ball milling be prepare under a kind of low temperature ferritic, the new method of energy-conserving and environment-protective.
As can be seen from Fig. 3 and Fig. 4, the particle that the method obtains is more regular subsphaeroidal, and size is even, and size is at about 10-15nm, and crystal formation is more complete.Found by the analysis of the SAED figure to Fig. 5, what each diffraction ring was strict corresponds to NiZnFe
2o
4each crystal face (as shown as icons), this is consistent with XRD analysis result, thus proves that further this nano particle is NiZnFe
2o
4.
As can be seen from Figure 6, the saturation magnetization of the product obtained after the microwave ultrasound of 30 hours combines auxiliary ball milling reaches 77.87emu/g.This sends out (60emu/g) than self-propagating method (63emu/g) co-precipitation of bibliographical information, and the corresponding ferritic saturation magnetization that the methods such as high-energy ball milling heating method prepare is all high.This proves that microwave ultrasound combines auxiliary ball milling is a kind of excellent process preparing high-performance nano ferrite powder.
When adopting microwave radiation technology ball milling or ultrasonic wave added ball milling to prepare nickel-zinc ferrite, need 80 hours consuming time and 70 hours respectively, and its dispersion effect obviously not have microwave ultrasound to combine the dispersion effect of the standby powder of auxiliary ball milling legal system good, and the saturation magnetization that microwave ultrasound combines auxiliary ball milling powder product improves nearly 30%.
Embodiment 2: microwave ultrasound associating auxiliary ball grinds standby nano zine oxide
We are raw material with basic zinc carbonate, with ethylene glycol be organic solvent as ball-milling medium, by the method identical with embodiment 1, also prepared zinc-oxide nano oxide.
7 can find out from the graph, and after 10 hours microwave ultrasounds combine auxiliary ball milling, all basic zinc carbonates have all transferred zinc oxide to.This proves that microwave ultrasound combines auxiliary ball milling is a kind of effective means that basic zinc carbonate effectively can be decomposed into zinc oxide.And in this technique, not to the heat treatment that product is such as calcined and so on, and in whole process, all reactions are all carry out in organic solvent, reaction temperature is not more than 100 DEG C, prove that this equipment is that one can be used for realizing salt decomposition fast, prepare the industrialized new equipment of class of the low-energy environment-friendly of nanometer powder.
The powder particle can prepared in this way from Fig. 8 has good dispersiveness, and particle is tiny, and average grain diameter is at about 30nm.We have also successfully prepared cupric oxide by this microwave ultrasound associating auxiliary ball mill apparatus in addition, nickel oxide, barium monoxide, titanium oxide, the multiple nano-oxide such as manganese oxide, this prove this device be prepare nano-oxide easily realize industrialized ideal equipment.
We have also carried out microwave radiation technology ball milling and the test of ultrasonic wave added ball milling respectively with identical raw material, and found by test, compared with ultrasonic wave added ball milling or microwave radiation technology ball milling, the speed of this installation method improves 30%-50%.
Embodiment 3: microwave ultrasound associating auxiliary ball grinds standby nano oxidized tin powder
We for raw material, using organic solvents such as acetic acid as ball-milling medium, by the method identical with embodiment 1, have also prepared the tin oxide nano powder that granularity is 10-20nm with 100 object glass puttys in 10 hours.This method has efficient feature, is ideal device and the process of the nano oxidized tin powder of a kind of suitability for industrialized production.
We have also carried out microwave radiation technology ball milling and the test of ultrasonic wave added ball milling respectively with identical raw material, are found by test, and ultrasonic wave added ball milling or microwave radiation technology ball milling all cannot prepare nano oxidized tin powder in long-time.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.Any Reference numeral in claim should be considered as the claim involved by limiting.
In addition, be to be understood that, although this description is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should by description integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (2)
1. the technique adopting microwave ultrasound associating auxiliary ball mill apparatus to prepare high-performance nano powder, described ball mill device comprises motor, puddler, ball grinder, abrading-ball, described motor drives puddler, described puddler extend in the abrading-ball of ball grinder, described ball grinder is provided with ball milling cover, described ball grinder covers and is provided with cooling back installation and liquid supply device, described ball grinder is placed on microwave generator inside, and cooling back installation, puddler and liquid supply device reach microwave generator outside, supersonic generator is provided with immediately below described ball grinder, described supersonic generator comprises ultrasonic transducer, and the ultrasonic wave cylindrical shell of ultrasonic transducer outside, and bottom ultrasonic wave cylindrical shell top and microwave generator, and the flange in the bottom of ball grinder is tightly connected, described technique concrete steps are:
Step (1): pour material powder and medium solution and abrading-ball into ball grinder, ensures that the liquid level of medium solution is at the 1/2-3/4 place of ball grinder total height, covers ball milling cover;
Step (2): open motor, open supersonic generator, motor rotary speed is that 100-1250 per minute turns, motor drives puddler, puddler drives abrading-ball to grind 10-20 minute to material powder, and the power of supersonic generator is 150-250W, and frequency is respectively 20KHz, 28KHz, 40KHz;
Step (3): open microwave generator again and work together, the power of microwave generator is 0.8-1.2KW, and frequency is 2450MHz, carries out radiation 10-20 minute, closes microwave generator;
Step (4): repeat step (2) and step (3), until obtain target product.
2. employing microwave ultrasound associating auxiliary ball mill apparatus according to claim 1 prepares the technique of high-performance nano powder, it is characterized in that, in step (2), motor rotary speed is 235 turns per minute, grind 15 minutes, the power of supersonic generator is 200W, and frequency is divided into 20KHz, 28KHz and 40KHz; Described in step (3), the power of microwave generator is 1KW, and frequency is 2450MHz, carries out radiation 15 minutes.
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