CN1324159C - Method for preparing nanocystalline ingot casting by magnetic field and ultrasonic combined treatment of metal melt and dedicated apparatus therefor - Google Patents
Method for preparing nanocystalline ingot casting by magnetic field and ultrasonic combined treatment of metal melt and dedicated apparatus therefor Download PDFInfo
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- CN1324159C CN1324159C CNB200510046589XA CN200510046589A CN1324159C CN 1324159 C CN1324159 C CN 1324159C CN B200510046589X A CNB200510046589X A CN B200510046589XA CN 200510046589 A CN200510046589 A CN 200510046589A CN 1324159 C CN1324159 C CN 1324159C
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Abstract
The present invention relates to a method and the special equipment for preparing nanocrystalline cast ingots by a metal fused mass of the combined treatment of a magnetic field and ultrasonic waves, which solves problems of complex processing equipment, high cost, difficult acquisition of large-size nanometer materials, etc. exist in the prior art. In the method, the present invention comprises the following procedures: fusing and overheating prepared raw materials, carrying out deaeration treatment for the metal fused mass, and quickly casting deaerated metal fused mass into a preheating crucible; heating the metal fused mass so as to reach above liquidus, carrying out electromagnetic mixing and supersonic vibration for the metal fused mass, and then, cooling the crucible, and completely solidifying the metal fused mass so as to obtain the massive nanocrystalline cast ingots. The special equipment for enforcing the method for preparing nanocrystalline cast ingots by a metal fused mass of the combined treatment of a magnetic field and ultrasonic waves comprises a maintaining furnace, wherein the crucible is arranged in the maintaining furnace; the special equipment is characterized in that the outer side of themaintaining furnace is provided with a magnetic field generator, the upper surface of the crucible is provided with an ultrasonic transducer, and the bottom of the crucible is provided with a cooler.
Description
Technical field
The invention belongs to reguline metal nano material production field, particularly a kind of magnetic field and ultrasonic combined processing metal melt prepare the method and the specific equipment of nanocrystalline ingot casting.
Background technology
Nanometer is a unit of length, and nanometer science and technology is research by the science and technology of the technical problem in the characteristics of motion of the material compositional system between size 0.1～100nm and interaction and the possible practical application.At present, nano material can roughly be divided into six classes such as the nanometer powder, unidimensional nanofiber of zero dimension, the nanometer film of two dimension, three-dimensional nano block, nano composite material, nanostructure.Wherein, the metal nanocrystal material is because its crystal grain is tiny, usually less than 100nm, the interphase density height, thereby have small size quantum effect and a grain boundary effect, having shown a series of and common polycrystal and non-crystalline solids has performances such as the mechanics of essential distinction, magnetic, light, electricity, sound, has opened up new road for improving comprehensive mechanical performance, has a good application prospect.Thereby the technology of preparing of high-quality three-dimensional large size reguline metal nanocrystal has become one of key of nano materials research.
In the prior art, the technology of preparing of reguline metal nano material mainly contains inert gases agglomeration original position press molding method, mechanical alloy grinds in conjunction with the high undercooling direct crystallization method and the pulsed current direct crystallization method that add the piece method that is pressed into, amorphous crystallization method, high pressure, high temperature solid-state quench method and directly prepare the lumpy nanometer crystalline substance.
The preparation process of inert gases agglomeration original position press molding method is: make metal heated distillation under the protection of rare gas element and assemble, be condensed into the ultramicron of nano-scale in the high vacuum reaction chamber on liquid nitrogen Cold Mirrors wall; with scraper plate the nanoparticle on the collector is scraped again and enter funnel and import mould; under the 10-6Pa high vacuum, compression system makes nano powder original position pressurization (sintering) become piece with the pressure of 1～5GPa.Adopt this method successfully to make Pd, Cu, Fe, Ag, Mg, Sb, Ni
3Al, NiAl, TiAl, Fe
5Si
95Lumpy nanometer material Deng alloy.Though this method scope of application broad, the micro mist surface cleaning, help Theoretical Studies of Nano-Materials, but complex process equipment, output is extremely low, is difficult to satisfy the requirement of performance study and application, and particularly there is a large amount of microporositys in the nanocrystals samples of preparation in this way, fine and close sample rate only can reach 75%～97% of metal volume density, and this microporosity is very unfavorable to the raising of nano material's structure performance study and some performance.
Mechanical alloy grinds that to be pressed into the piece method be the technology that American I NCO company developed the end of the sixties in conjunction with adding.It is at Ar
2Under the gas shiled; collision mutually between hardened steel ball by mechanical mill process high speed operation and the grinding element; powder particle is carried out clinkering, fracture repeatedly, makes the continuous refinement of crystal grain in the fritted process again; reach nano-scale; then, nano powder adopts technology pressurizations such as hot extrusion, hot isostatic pressing to make the lumpy nanometer material again.Studies show that amorphous, accurate brilliant, nanocrystalline, superconducting material, RE permanent magnetic alloy, superplastic alloy, intermetallic compound, the strong alloy of light metal height ratio all can synthesize by this method.The advantage of this method is: the alloy substrate composition is unrestricted, cost is low, output is big, technology is simple, particularly demonstrates stronger vigor at aspects such as the generation of the alloying of refractory metal, non-equilibrium phase and exploitation special purpose alloys.The problem that exists is: easily produce impurity, pollution, oxidation and stress in the process of lapping, be difficult to obtain clean nanocrystal interface, unfavorable to some basic research work, in addition, the stress influence of still needing and further overcoming in the ma process to be brought.
Amorphous crystallization method is that to make the product of crystallization be the crystal grain of nano-scale for crystallization kinetic process by the control non-crystalline solids.It is made up of acquisition and two processes of crystallization of non-crystalline solids usually.Non-crystalline solids can pass through technology preparations such as melt Quench, high speed d.c. sputtering, plasma jet atomizing, solid state reaction, and the most frequently used is that single roller or two roller revolve the method for quenching.Because above method can only obtain low-dimensional materials such as amorphous powder, silk and band, thus also need adopt the hot-die compacting, methods such as hot extrusion or High Temperature High Pressure sintering synthesize bulk sample.Crystallization adopts the isothermal annealing method usually, has also developed methods such as classification annealing, pulse annealing, SHOCK WAVE INDUCED in recent years.At present, utilize this method to prepare the nanocrystal of multiple alloy series such as Ni, Fe, Co, Pd base, also can prepare intermetallic compound and element semiconductor nanocrystal, this method is being most widely used aspect the preparation of Nano soft magnetic material.The characteristics of this method are: cost is low, output is big, interface cleanness is fine and close, pore-free crack in the sample, it is easy to control that grain fineness number changes, and help to study nanocrystalline formation mechanism and be used for checking classical nucleation grow up theoretical under the rapid solidification condition possibility of its application.Its limitation is: depend on the acquisition of non-crystalline solids, and, only being applicable to the alloy system that amorphous formation ability is stronger, its range of application is subjected to certain restriction.
High pressure, high temperature solid-state quench method are that the sample of vacuum arc furnace melting is inserted in the high-pressure chamber, heat up after being forced into several GPa, the long-range diffusion and the crystalline growth velocity that suppress atom by high pressure, thereby realize the nanometer of crystal grain, then, solid phase is quenched under the high temperature again, to keep high temperature, high pressure tissue.The characteristics of this method are: easy, the interface cleanness of technology can directly prepare the nanocrystalline of large block compact.Its limitation is: need very high pressure, chunk sizes obtains difficulty, in addition, does not also still have the report of applied research in other alloy system.
High undercooling direct crystallization method, well-known, rapid solidification has significant effect to grain refining, and therefore, chilling and high undercooling are effective two approach that realize the melt rapid solidification.The chilling flash set technology can only be produced such as low-dimensional materials such as strip, filament or powders owing to limited by heat transfer process, thereby is subjected to bigger restriction on using.The high undercooling flash set technology, realize rapid solidification under the big thermodynamics condensate depression by avoiding or remove heterogeneous nucleus, its melt growth is not controlled by extraneous radiating condition, its grain refining is arranged by the special physical mechanism of melt itself, is to realize that three-dimensional large volume liquid metal rapid solidification prepares an effective way of crystallite, amorphous and quasicrystal material.But this method in theory also is in conceptual phase at present, and production technique and production unit are also still immature.
Pulsed current direct crystallization method starts from the 1980s, and India scholar A.K.Mistra is at first at Pb
68Sb
15Sn
7Eutectic and Pb
87Sb
10Sn
3Pass to 40mA/cm in the hypoeutectic alloy
2Direct current, organize obvious refinement after finding to solidify, people such as M.Nakada are at Sn
85Pb
15Promote blood circulation in the alloy graining process behind electric current, also find the solidified structure refinement and dendrite takes place to change to globular crystal, J.P.Barnak etc. have studied Pulse Electric Current with High Density to Sn
60Pb
40And Sn
63Pb
37The influence of alloy graining tissue.The result confirms that pulsed current can increase condensate depression, and can make the grain fineness number of eutectic reduce an order of magnitude, and grain fineness number reduces with the pulse current density increase.Domestic scientific research personnel has not only studied the influence of pulsed current to the alloy solidified structure experimentally, and done further investigation with the calculating theoretical and the crystallization grain-size of the crystallization nucleation of classical thermodynamics and electrodynamics of continuous media paired pulses galvanic action melt in theory, point out that pulse current density reaches 0.1GA/m
2The time, it is nanocrystalline to obtain bulk in theory.Because the critical pulse current density of some metal nanoizations that require can reach on engineering and meet substantially with experimental value in theory, the quick relaxation characteristics of pulsed current can limit growing up of nanocrystal in addition, therefore, along with pulsed current influences the further perfect of machine-processed further research and experimental installation to metal freezing, the pulse current processing might make melt directly be condensed into the bulk nanocrystalline material on some alloy when ultrashort, and becomes the direct crystallization legal system and be equipped with one of potential technology of nanocrystalline material.But this method only uses single outer field action in metal melt, action intensity to metal melt in the super-refinement process that realizes crystal grain is big not enough, and this method also is in theoretical research stage at present, is subjected to the restriction of experimental installation technically and does not obtain bigger progress.
Make a general survey of the researchdevelopment of nano material, be not difficult to find out, nano material apply the preparation that key is the lumpy nanometer material, the major objective of reguline metal nano material preparation technical development then is that development process is simple, the big scope of application of output is wide, can obtain the example interface cleaning, the macro nanometer material preparation technology in pore-free crack, its development trend then are the nanocrystalline technologies of preparing of direct crystallization method.
Summary of the invention
The technical problem to be solved in the present invention is, overcome complex process equipment, cost height, the macro nanometer material that above-mentioned prior art exists and obtain problems such as difficulty, provide that a kind of production technique and equipment are simple, cost is low, it is high-quality directly to prepare, the magnetic field of the brilliant ingot casting of large size lumpy nanometer and method and the specific equipment that ultrasonic combined processing metal melt prepares nanocrystalline ingot casting.
The method that magnetic field of the present invention and ultrasonic combined processing metal melt prepare nanocrystalline ingot casting realizes according to following step:
1, the composition according to the metallic nano crystal ingot casting requires to prepare burden, and the starting material that prepare are put into fusing with crucible, makes it fusing, and overheated 10～80 ℃;
2, metal melt is carried out degassing processing, the degasification time is 1～10 minute;
3, the metal melt after the degasification is poured in the crucible of preheating fast, the preheating temperature of crucible is 300～400 ℃;
4, with the metal melt that pours into heater heats to more than the liquidus line 10～100 ℃;
5, constant temperature under this temperature, and metal melt applied induction stirring, field voltage is 170～200V, conduction current density is 10
6～10
8A/m
2, magneticflux-density is 1～10T;
6, meanwhile, metal melt is applied ultrasonic vibration, ultrasonic power is 100～1000W, and ultrasonic frequency is 10～100kHz, and metal melt is applied magnetic field and hyperacoustic time is 4～30 minutes jointly;
7, metal melt is being applied induction stirring and ultrasonic vibration in the time of 2～10 minutes, begin crucible bottom is cooled off, make metal melt begin to solidify from the bottom, and before the metal melt surface solidification, withdraw from ultrasonic transducer, stop induction stirring, make it to solidify fully, can obtain the brilliant ingot casting of lumpy nanometer.
Above-mentioned said degassing processing is to add degassing refining agent or be blown into argon gas or nitrogen in metal melt.
A kind ofly implement the specific equipment that above-mentioned magnetic field and ultrasonic combined processing metal melt prepare the method for nanocrystalline ingot casting, it has a holding furnace, a crucible is arranged in holding furnace, its special character is, magnetic field generator is equipped with in the outside at holding furnace, a ultrasonic transducer is arranged on crucible, a water cooler is arranged in the bottom of crucible.
The present invention compared with prior art has following advantage:
1, at first is exactly the compound of outfield, because any single outfield all is difficult to grain refining to Nano grade, the present invention is exactly the nanocrystalline ingot casting of compound direct preparation by the outfield, and the present invention adopts the highest preceding two classes of intensity in the outfield, and promptly electromagnetic field combines with ultrasonic wave field, strong combination, acting in conjunction is in metal melt, thereby realized the super refinement of crystal grain, i.e. nanometer.
2, secondly, be exactly directly to prepare large-sized ingot casting, at present, nano material is meant nano-powder material mostly, and preparation lumpy nanometer material is subjected to the qualification of technology of preparing, very difficult, the compound outfield that the present invention utilizes magnetic field and high-energy ultrasonic to produce cooperates with metal melt, has directly prepared large-sized ingot casting, is directly hewing out a new road on the preparation three-dimensional manometer crystal technique.
3, induction stirring combines with ultrasonic wave, and metal melt is produced the intensive mixing effect, and electromagnetic field also has the effect of eliminating macrosegregation, and ultrasonic wave also has degassing effect, thereby has obtained cleaning, imporosity, large-sized nanocrystalline ingot casting.
4, simple, the less investment of preparation method of the present invention and production unit, realized production nanocrystalline material high-quality, low-cost, many kinds, being a kind of multidisciplinary synthesis and the nano material preparation technology of intersecting, also is one of nanocrystalline Development of Preparation Technology direction.
5, the present invention studies the Changing Pattern of compound melt after the match to the refining effect mechanism in research outfield, understands the technology of preparing that nanocrystalline material forms mechanism and development and improves nano material, and important scientific meaning is all arranged.
Description of drawings
Fig. 1 is the structural representation of specific equipment of the present invention.
Embodiment
Embodiment 1:
The concrete steps that magnetic field of the present invention and ultrasonic combined processing metal melt prepare nanocrystalline ingot casting are:
1, the composition according to the metallic nano crystal ingot casting requires to prepare burden, and is example with low melting point alloy Al-1.0%Cu, and the starting material that prepare are put into fusing with crucible, makes it fusing, and overheated 10 ℃;
2, metal melt is carried out degassing processing, add degassing refining agent in metal melt, the add-on of degassing refining agent is 0.8% of a metal melt weight, and the degasification time is 1 minute;
3, the metal melt after the degasification is poured in the crucible of preheating fast, the preheating temperature of crucible is 300 ℃;
4, with the metal melt that pours into heater heats to more than the liquidus line 100 ℃;
5, constant temperature under this temperature, and metal melt applied induction stirring, field voltage is 170V, conduction current density is 10
6A/m
2, magneticflux-density is 1T;
6, meanwhile, metal melt is applied ultrasonic vibration, ultrasonic power is 1000W, and ultrasonic frequency is 10kHz, and metal melt is applied magnetic field and hyperacoustic time is 4 minutes jointly;
7, metal melt is being applied induction stirring and ultrasonic vibration in the time of 2 minutes, begin crucible bottom is cooled off, in water cooler, feed water coolant, make metal melt begin to solidify from the bottom, and before the metal melt surface solidification, withdraw from ultrasonic transducer, stop induction stirring, make it to solidify fully, can obtain the brilliant ingot casting of lumpy nanometer.
Embodiment 2:
1, the composition according to the metallic nano crystal ingot casting requires to prepare burden, and is example with low melting point alloy Pb-Sn, and the starting material that prepare are put into fusing with crucible, makes it fusing, and overheated 50 ℃;
2, metal melt is carried out degassing processing, be blown into nitrogen in metal melt, the degasification time is 8 minutes;
3, the metal melt after the degasification is poured in the plumbago crucible of preheating fast, the preheating temperature of crucible is 350 ℃;
4, with the metal melt that pours into heater heats to more than the liquidus line 70 ℃;
5, constant temperature under this temperature, and metal melt applied induction stirring, field voltage is 200V, conduction current density is 10
8A/m
2, magneticflux-density is 10T;
6, meanwhile, metal melt is applied ultrasonic vibration, ultrasonic power is 500W, and ultrasonic frequency is 100kHz, and metal melt is applied magnetic field and hyperacoustic time is 20 minutes jointly;
7, metal melt is being applied induction stirring and ultrasonic vibration in the time of 5 minutes, begin crucible bottom is cooled off, in the water cooler of crucible bottom, feed water coolant, make metal melt begin to solidify from the bottom, and before the metal melt surface solidification, withdraw from ultrasonic transducer, stop induction stirring, make it to solidify fully, can obtain the brilliant ingot casting of lumpy nanometer.
Embodiment 3:
1, the composition according to the metallic nano crystal ingot casting requires to prepare burden, and is example with soft steel Fe-0.1%C, and the starting material that prepare are put into fusing with crucible, makes it fusing, and overheated 80 ℃;
2, metal melt is carried out degassing processing, be blown into argon gas in metal melt, the degasification time is 10 minutes;
3, the metal melt after the degasification is poured in the plumbago crucible of preheating fast, the preheating temperature of crucible is 400 ℃;
4, with the metal melt that pours into heater heats to more than the liquidus line 10 ℃;
5, constant temperature under this temperature, and metal melt applied induction stirring, field voltage is 180V, conduction current density is 10
7A/m
2, magneticflux-density is 8T;
6, meanwhile, metal melt is applied ultrasonic vibration, ultrasonic power is 100W, and ultrasonic frequency is 60kHz, and metal melt is applied magnetic field and hyperacoustic time is 30 minutes jointly;
7, metal melt is being applied induction stirring and ultrasonic vibration in the time of 10 minutes, begin crucible bottom is cooled off, in the water cooler of crucible bottom, feed water coolant, make metal melt begin to solidify from the bottom, and before the metal melt surface solidification, withdraw from ultrasonic transducer, stop induction stirring, make it to solidify fully, can obtain the brilliant ingot casting of lumpy nanometer.
Be elaborated to implementing the specific equipment that above-mentioned magnetic field and ultrasonic combined processing metal melt prepare the method for nanocrystalline ingot casting below:
As shown in Figure 1, it has a holding furnace 5, and holding furnace 5 is made of aluminium sesquioxide flue and resistance heating body, and resistance heating body is wrapped in the flue; A crucible 4 is arranged in holding furnace 5, and crucible 4 adopts graphite to make, and also can make of other materials; In the outside of holding furnace 5 magnetic field generator 6 is housed, magnetic field generator 6 is a spiral coil; A ultrasonic transducer 1 is arranged on crucible 4, and described ultrasonic transducer 1 is an existing structure, and it mainly is made of shell, coil, transducing head etc., the water-in and water-out joint is arranged, so that transducing head is cooled off on shell; In the bottom of transducing head horn 2 is housed, in the bottom of horn 2 ultrasonic vibration bar 3 is housed, the top of ultrasonic vibration bar 3 is the steel pole, and the bottom is a ceramic rod; Described ultrasonic transducer 1 is installed on the column 9 by sliding support 10, and sliding support 10 can move up and down thereby drive ultrasonic transducer 1 along moving up and down at column 9, and column 9 is fixed on the worktable 8; A water cooler 7 is arranged in the bottom of crucible 4, water cooler 7 is placed on the worktable 8, described water cooler 7 is made of cooling plate and water tank, the water-in and water-out joint is arranged on water tank, cooling plate is in the same place with tank weld, constitutes watercooling jacket, and cooling plate is done with copper, and be positioned at water tank above, to improve cooling performance to crucible 4.
Claims (3)
1, a kind of magnetic field and ultrasonic combined processing metal melt prepare the method for nanocrystalline ingot casting, it is characterized in that it is realized according to following step:
(1), require to prepare burden, the starting material that prepare are put into fusing with crucible, make it fusing according to the composition of metallic nano crystal ingot casting, and overheated 10～80 ℃;
(2), metal melt is carried out degassing processing, the degasification time is 1～10 minute;
(3), the metal melt after the degasification is poured in the crucible of preheating fast, the preheating temperature of crucible is 300～400 ℃;
(4), with the metal melt that pours into heater heats to more than the liquidus line 10～100 ℃;
(5), under this temperature constant temperature, and metal melt applied induction stirring, field voltage is 170～200V, conduction current density is 10
6～10
8A/m
2, magneticflux-density is 1～10T;
(6), meanwhile, metal melt is applied ultrasonic vibration, ultrasonic power is 100～1000W, and ultrasonic frequency is 10～100kHz, and metal melt is applied magnetic field and hyperacoustic time is 4～30 minutes jointly;
(7), metal melt is being applied induction stirring and ultrasonic vibration in the time of 2～10 minutes, begin crucible bottom is cooled off, make metal melt begin to solidify from the bottom, and before the metal melt surface solidification, withdraw from ultrasonic transducer, stop induction stirring, make it to solidify fully, can obtain the brilliant ingot casting of lumpy nanometer.
2, magnetic field according to claim 1 and ultrasonic combined processing metal melt prepare the method for nanocrystalline ingot casting, it is characterized in that, above-mentioned said degassing processing is to add degassing refining agent or be blown into argon gas or nitrogen in metal melt.
3, a kind of magnetic field of claim 1 and specific equipment that ultrasonic combined processing metal melt prepares the method for nanocrystalline ingot casting implemented, it has a holding furnace, a crucible is arranged in holding furnace, it is characterized in that, magnetic field generator is equipped with in the outside at holding furnace, a ultrasonic transducer is arranged on crucible, a water cooler is arranged in the bottom of crucible.
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