CN103785511A - Microwave and ultrasound combined assisted ball-milling device and process for preparing high-performance nanopowder - Google Patents
Microwave and ultrasound combined assisted ball-milling device and process for preparing high-performance nanopowder Download PDFInfo
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Abstract
The invention discloses a microwave and ultrasound combined assisted ball-milling device and process for preparing high-performance nanopowder. According to the device, a ball mill is placed in a microwave generator, and a bottomless ball-milling tank in the ball mill is connected with the top of an ultrasonic generator, so that the microwave and ultrasound combined assisted ball-milling device is formed. The process is characterized in that a medium solution and raw material powder in the ball-milling tank are subjected to cavatition of ultrasonic waves, the radiation effect of microwaves and the action of mechanical force of ball milling simultaneously, so that the speeds of reduction, oxidization, synthesis, decomposition and other reactions are greatly increased, and chemical reactions which cannot be realized by means of independent microwave-assisted ball milling or independent ultrasound-assisted ball milling in the prior art can happen. The device can be used for preparing multiple kinds of nanometer functional powder such as metallic oxide, ferrite, composite ferrite, wave-absorbing materials, luminescent materials and magnetic materials.
Description
Technical field
The invention belongs to the field of grinding, specifically a kind of microwave ultrasound associating auxiliary ball mill apparatus and technique of 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 who prepares at present the Magnaglos such as nanometer ferrite and other nanometer powders 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 people's daily productive life.Microwave has and selectively adds thermal property, thereby in separating substances, its excellent characteristic has also been brought into play in the aspects such as ore grinding.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 large-scale synthetic effective especially to controlling, because it can reduce the impact of thermal gradient to greatest extent.Secondly,, because the dielectric constant of solvent and reactant is different, 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 concentration and the shape of composition with control microwave irradiation time and nanostructured that can adjust the big or small of nano particle and pass through to change solvent by changing the concentration of presoma.
Ultrasonic wave is in certain Propagation process, and can interact between propagation medium, its result causing is exactly that the parameters such as hyperacoustic phase place and amplitude can change thereupon, and then causing the physical property of propagation medium and chemical property to change, 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 that affects 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, is mainly machinery and the chemical effect of utilizing ultrasonic wave to produce.Wherein mechanical effect main manifestations is the increase of heterogeneous reaction interface under ul-trasonic irradiation; Chemical effect is mainly the shattered to pieces TRANSIENT HIGH TEMPERATURE high pressure causing due to the bubble of cavitation effect hollow, 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 aspects such as wastewater treatment and plating.
Ball-milling method is at present in the world in the industrial main stream approach of preparing nanometer powder that is applied to.But ball-milling method mainly exists the ball action time long preparing in nanometer powder, product great efforts, the major defect such as granular size is inhomogeneous, poor repeatability, becomes restriction ball-milling method and is widely used in bottleneck prepared by nanometer powder industrial.
The SEPARATE APPLICATION of this team the patent of invention (ZL201110004753.6, ZL200910309641.4) such as the auxiliary ball milling of microwave and ultrasonic auxiliary 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 technique of preparing high-performance nano powder, the present invention combines the advantage of microwave, ultrasonic wave and ball milling, make, at low equipment requirement, under the conditions such as low environment pollution, can prepare efficiently various high performance nanometer powders.
For achieving the above object, the invention provides following technical scheme:
A kind of microwave ultrasound associating auxiliary ball mill apparatus of 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, under described ball grinder, be provided with supersonic generator, described supersonic generator comprises ultrasonic transducer, and the ultrasonic wave cylindrical shell of ultrasonic transducer outside, and ultrasonic wave cylindrical shell top and microwave generator bottom, 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 adopts polytetrafluoroethylene (PTFE) processing or pottery to make.
As the further scheme of the present invention: described abrading-ball is that diameter is Ceramic Balls or the Metal Ball of 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, guarantee that the liquid level of medium solution, 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 and 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) repeating step (2) and step (3), until obtain target product.
As the further scheme of the present invention: guarantee 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 per minute 235 to turn, 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, and 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, synthetic, decomposition is increased greatly, and some original chemical reactions of assisting ball milling or independent ultrasonic auxiliary ball milling to realize by microwave are separately 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;
Under it, be designated as: 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 Times;
Fig. 3 combines by microwave ultrasound the nanometer NiZnFe that auxiliary ball-milling method obtains
2o
4tEM figure;
Fig. 4 combines by microwave ultrasound the nanometer NiZnFe that auxiliary ball-milling method obtains
2o
4tEM figure;
Fig. 5 combines by microwave ultrasound the nanometer NiZnFe that auxiliary ball-milling method obtains
2o
4sAED picture;
Fig. 6 is the hysteresis curve figure that combines the nickel-zinc ferrite that auxiliary ball-milling method obtains after the different disposal time by microwave ultrasound;
Fig. 7 combines the XRD figure of the product obtaining after auxiliary ball milling through 10 hours microwave ultrasounds;
Fig. 8 is the TEM figure of the nano zine oxide for preparing of microwave ultrasound associating auxiliary ball mill apparatus.
The specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Based on the embodiment in the present invention, those of ordinary skills, not making the every other embodiment obtaining 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 of 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, described ball grinder 5 is arranged on microwave generator 6 inside, and cooling back installation 2, puddler 4 and liquid supply device 10 reach microwave generator 6 outsides, under described ball grinder 5, be provided with supersonic generator, described supersonic generator comprises ultrasonic transducer 8, and the ultrasonic wave cylindrical shell 9 of ultrasonic transducer 8 outsides, and ultrasonic wave cylindrical shell 9 tops and microwave generator 6 bottoms, 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; Described abrading-ball 11 is that diameter is Ceramic Balls or the Metal Ball of 0.5-2mm; Described Metal Ball comprises stainless steel ball, iron ball, titanium ball and copper ball; Between described ultrasonic wave cylindrical shell 9 tops and the flange in the bottom of bottomless ball grinder 5, be provided with sealing device 7.
A kind of technique that adopts 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, guarantee that the liquid level of medium solution, at the 1/2-3/4 place of ball grinder 5 total heights, is preferably 2/3; Cover ball milling cover 12; Then open motor 1, drive puddler 4, puddler 4 drives abrading-ball 11 to grind material powder; Or open motor 1 and microwave generator 6 simultaneously material powder is carried out to the auxiliary ball milling of microwave; Or open motor 1 and supersonic generator simultaneously, material powder is carried out to the auxiliary ball milling of ultrasonic wave; Or the motor 1 of simultaneously performing fighting, microwave generator 6 and supersonic generator carry out microwave ultrasound to material powder and combine auxiliary ball milling, there is various physics or chemistry or physical-chemical reaction in material powder, thereby 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, synthetic, decomposition is increased greatly, and some original chemical reactions of assisting ball milling or independent ultrasonic auxiliary ball milling to realize by microwave are separately 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 further to set forth the present invention, 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, then by reactant, the mass ratio take ratio of grinding media to material as 100:1 is put into the ball grinder of Ф 135 × 215mm, then adds 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 per minute 235 to turn, reactant is carried out to 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, follow again ultrasonic ball milling 15 minutes, so repeatedly; After the regular hour, sample, first the sample of taking-up is placed on filter filtration on paper, is then placed in drying box and is dried 12 hours at the temperature of 50 ℃; Again the sample taking out is ground, then by XRD, VSM, TEM, the detection means such as SAED characterize and detect.
As can be seen from Figure 2, after combining auxiliary ball milling, 6 hours microwave ultrasounds 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 that obtain are completely corresponding to spinel-type NiZnFe
2o
4.Prove microwave ultrasound combine auxiliary ball milling be under a kind of low temperature, prepare ferritic, the new method of energy-conserving and environment-protective.
Can find out from Fig. 3 and Fig. 4, the particle that the method obtains is more regular subsphaeroidal, and evenly, size is in 10-15 nm left and right, and crystal formation is more complete for size.Analysis by the SAED figure to Fig. 5 finds, each diffraction ring strict corresponding to NiZnFe
2o
4each crystal face (as shown as icons), this is consistent with XRD analysis result, thereby further proves that this nano particle is NiZnFe
2o
4.
The saturation magnetization of the product obtaining after the microwave ultrasound of 30 hours is combined auxiliary ball milling as can be seen from Figure 6, has reached 77.87emu/g.(60emu/g) sent out in this method that certainly spreads (63emu/g) co-precipitation than bibliographical information, and the corresponding ferritic saturation magnetization that the methods such as high-energy ball milling heat treated method prepare is all high.This proves that it is a kind of excellent process of preparing high-performance nano ferrite powder that microwave ultrasound is combined auxiliary ball milling.
In the time adopting the auxiliary ball milling of microwave or ultrasonic auxiliary ball to grind standby nickel-zinc ferrite, need respectively 80 hours consuming time and 70 hours, 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 is combined auxiliary ball milling product powder has improved nearly 30%.
Embodiment 2: microwave ultrasound associating auxiliary ball grinds standby nano zine oxide
We using ethylene glycol as organic solvent is as ball-milling medium, by the method identical with embodiment 1, have also prepared zinc-oxide nano oxide take basic zinc carbonate as raw material.
7 can find out from the graph, combine after auxiliary ball milling through 10 hours microwave ultrasounds, and all basic zinc carbonates have all transferred zinc oxide to.This proves that it is a kind of effective means that basic zinc carbonate effectively can be decomposed into zinc oxide that microwave ultrasound is combined auxiliary ball milling.And in this technique, product is not carried out to the heat treatment such as calcining and so on, and in whole process, all reactions are all to carry out in organic solvent, reaction temperature does not exceed 100 ℃, prove that this equipment is that one can be used for realizing fast salt decomposition, prepares the industrialized new equipment of class of the low energy environmental protection of nanometer powder.
The powder particle of can the method preparing from Fig. 8 has good dispersiveness, and particle is tiny, and average grain diameter is in 30nm left and right.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 respectively the auxiliary ball milling of microwave and ultrasonic auxiliary ball milling test with identical raw material, find by test, and compared with ultrasonic auxiliary ball milling or the auxiliary ball milling of microwave, the speed of this installation method has improved 30%-50%.
Embodiment 3: microwave ultrasound associating auxiliary ball grinds standby nano oxidized tin powder
We are take 100 object glass puttys as raw material, using organic solvents such as acetic acid as ball-milling medium, and by the method identical with embodiment 1, the tin oxide nano powder that also to have prepared granularity in 10 hours be 10-20nm.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 respectively the auxiliary ball milling of microwave and ultrasonic auxiliary ball milling test with identical raw material, find by test, and the auxiliary ball milling of ultrasonic auxiliary ball milling or microwave 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 in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other concrete form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, is therefore intended to all changes that drop in the implication and the scope that are equal to important document of claim to include in the present invention.Any Reference numeral in claim should be considered as limiting related claim.
In addition, be to be understood that, although this description is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should make description as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (8)
1. prepare the microwave ultrasound associating auxiliary ball mill apparatus of high-performance nano powder for one kind, 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, it is characterized in that: 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, under described ball grinder, be provided with supersonic generator, described supersonic generator comprises ultrasonic transducer, and the ultrasonic wave cylindrical shell of ultrasonic transducer outside, and ultrasonic wave cylindrical shell top and microwave generator bottom, and the flange in the bottom of ball grinder is tightly connected.
2. the microwave ultrasound associating auxiliary ball mill apparatus of preparing high-performance nano powder according to claim 1, is characterized in that, described cooling back installation, puddler, ball grinder and liquid supply device all adopts polytetrafluoroethylene (PTFE) or pottery to be processed into.
3. the microwave ultrasound associating auxiliary ball mill apparatus of preparing high-performance nano powder according to claim 1, is characterized in that, described abrading-ball is that diameter is Ceramic Balls or the Metal Ball of 0.5-2mm.
4. the microwave ultrasound associating auxiliary ball mill apparatus of preparing high-performance nano powder according to claim 3, is characterized in that, described Metal Ball comprises stainless steel ball, iron ball, copper ball and titanium ball.
5. the microwave ultrasound associating auxiliary ball mill apparatus of preparing high-performance nano powder according to claim 1, is characterized in that, between described ultrasonic wave cylindrical shell top and the flange in the bottom of bottomless ball grinder, is provided with sealing device.
6. employing microwave ultrasound associating auxiliary ball mill apparatus as described in one of you 1-5 of claim is prepared a technique for high-performance nano powder, and concrete steps are:
Pour material powder and medium solution and abrading-ball into ball grinder, guarantee that the liquid level of medium solution, at the 1/2-3/4 place of ball grinder total height, covers ball milling cover;
Open motor, open supersonic generator, motor rotary speed is that 100-1250 per minute turns, motor drives puddler, and puddler drives abrading-ball to grind 10-20 minute to material powder, and the power of supersonic generator is 150-250W, frequency is respectively 20KHz, 28KHz, 40KHz;
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;
Repeating step (2) and step (3), until obtain target product.
7. the technique of preparing high-performance nano powder according to claim 1, is characterized in that, guarantees that the liquid level of medium solution is at the 1/2-3/4 place of ball grinder total height in step (1).
8. the technique of preparing high-performance nano powder according to claim 1, is characterized in that, described in step (3), the power of microwave generator is 1KW, frequency is 2450MHz, and the power of supersonic generator is 200W, and frequency is divided into 20KHz, 28KHz and 40KHz, carry out radiation 15 minutes.
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